Sample records for zirconium oxide bazro3

  1. Reactions of calcium orthosilicate and barium zirconate with oxides and sulfates of various elements

    NASA Technical Reports Server (NTRS)

    Zaplatynsky, I.

    1979-01-01

    Calcium orthosilicate and barium zirconate were evaluated as the insulation layer of thermal barrier coatings for air cooled gas turbine components. Their reactions with various oxides and sulfates were studied at 1100 C and 1300 C for times ranging up to 400 and 200 hours, respectively. These oxides and sulfates represent potential impurities or additives in gas turbine fuels and in turbine combustion air, as well as elements of potential bond coat alloys. The phase compositions of the reaction products were determined by X-ray diffraction analysis. BaZrO3 and 2CaO-SiO2 both reacted with P2O5, V2O5, Cr2O3, Al2O3, and SiO2. In addition, 2CaO-SiO2 reacted with Na2O, BaO, MgO, and CoO and BaZrO3 reacted with Fe2O3.

  2. Density functional calculations of carbon substituting for Zr in barium zirconate

    NASA Astrophysics Data System (ADS)

    Al-Hadidi, Meaad; Goss, J. P.; Al-Ani, Oras A.; Briddon, P. R.; Rayson, M. J.

    2017-06-01

    Oxide perovskites such as BaZrO3 possess many significant properties which render them useful in many technological and scientific applications such as sensors, optoelectronics, laser frequency doubling and high capacity memory cells. Several methods are used to grow BaZrO3 crystal, and organic species that may be present during growth lead to carbon contamination. We have investigated, using density-functional theory, the role of carbon impurities on the structural, electrical and electronic properties of carbon substituting of Zr in cubic barium zirconate. The local vibrational modes of the defect centre has been calculated and we suggest it is a feasible route to experimental identification

  3. Reactivity and oxygen diffusion property of resistive barriers for Bi-2223/Ag tapes

    NASA Astrophysics Data System (ADS)

    Kováč, P.; Hušek, I.

    2002-12-01

    Reactivity of several oxide materials (OM) with BSCCO powder and oxygen diffusion through OM layer has been tested at temperature ≈840 °C in air. The OM (e.g.: BaZrO 3, SrCO 3, MgO and ZrO 2) showing the low or no reactivity with BSCCO have been mixed (10 wt.%) with precursor powder and used for single-core tapes. Bi-2223/Ag/OM/Ag single-core tapes with oxide barriers made of BaZrO 3, SrCO 3, ZrO 2 and Al 2O 3 have been also prepared by a standard powder-in-tube technique. The used OM in the direct contact with BSCCO influences the electrical properties of Bi-2223 phase differently. These is because the oxides react with BSCCO during the heat treatment and simultaneously affect the 2212→2223 phase transformation, the Bi-2223 grain growth and so also grain connectivity. SrCO 3 powder has been evaluated as the best material from the point of no destructive effect on 2223 phase transport current property. The oxide barrier controls the oxygen diffusion during the tape heat treatment and simultaneously the HTS phase formation kinetics, its purity and content within the superconducting core. For single-core Bi-2223/Ag/OM/Ag tapes, the highest current density was measured for Al 2O 3 due to only slightly reduced oxygen diffusion through the barrier.

  4. No difference in in vivo polyethylene wear particles between oxidized zirconium and cobalt-chromium femoral component in total knee arthroplasty.

    PubMed

    Minoda, Yukihide; Hata, Kanako; Iwaki, Hiroyoshi; Ikebuchi, Mitsuhiko; Hashimoto, Yusuke; Inori, Fumiaki; Nakamura, Hiroaki

    2014-03-01

    Polyethylene wear particle generation is one of the most important factors affecting mid- to long-term results of total knee arthroplasties. Oxidized zirconium was introduced as a material for femoral components to reduce polyethylene wear generation. However, an in vivo advantage of oxidized zirconium on polyethylene wear particle generation is still controversial. The purpose of this study was to compare in vivo polyethylene wear particles between oxidized zirconium total knee prosthesis and conventional cobalt-chromium (Co-Cr) total knee prosthesis. Synovial fluid was obtained from the knees of 6 patients with oxidized zirconium total knee prosthesis and from 6 patients with conventional cobalt-chromium (Co-Cr) total knee prosthesis 12 months after the operation. Polyethylene particles were isolated and examined using a scanning electron microscope and image analyser. Total number of particles in each knee was 3.3 ± 1.3 × 10(7) in the case of oxidized zirconium (mean ± SD) and 3.4 ± 1.2 × 10(7) in that of Co-Cr (n.s.). The particle size (equivalent circle diameter) was 0.8 ± 0.3 μm in the case of oxidized zirconium and 0.6 ± 0.1 μm in that of Co-Cr (n.s.). The particle shape (aspect ratio) was 1.4 ± 0.0 in the case of oxidized zirconium and 1.4 ± 0.0 in that of metal Co-Cr (n.s). Although newly introduced oxidized zirconium femoral component did not reduce the in vivo polyethylene wear particles in early clinical stage, there was no adverse effect of newly introduced material. At this moment, there is no need to abandon oxidized zirconium femoral component. However, further follow-up of polyethylene wear particle generation should be performed to confirm the advantage of the oxidized zirconium femoral component. Therapeutic study, Level III.

  5. A-Site Cation Substitutions in Strained Y-Doped BaZrO 3 Multilayer Films Leading to Fast Proton Transport Pathways

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

    Aruta, Carmela; Han, Chu; Zhou, Si

    Proton-conducting perovskite oxides form a class of solid electrolytes for novel electrochemical devices operating at moderate temperatures. Here, we use hard X-ray photoelectron spectroscopy, scanning transmission electron microscopy, and density functional theory calculations to investigate the structure and elucidate the origin of the fast proton transport properties of strained ultrathin films of Y-doped BaZrO 3 grown by pulsed lased deposition on NdGaO 3. Our study shows that our BaZr 0.8Y 0.2O 3 films incorporate a significant amount of Y dopants, and to a lesser extent also Zr ions, substituting for Ba 2+, and that these substitutional defects agglomerate forming columnarmore » regions crossing vertically from the surface to the interface the entire film. In conclusion, our calculations also show that, in regions rich in Y substitutions for both Zr and Ba, the proton transfer process involves nearly zero-energy barriers, indicating that A-site cation substitutions by Y lead to fast transport pathways and hence are responsible for the previously observed enhanced values of the proton conductivity of these perovskite oxide films.« less

  6. Fretting wear behavior of zirconium alloy in B-Li water at 300 °C

    NASA Astrophysics Data System (ADS)

    Zhang, Lefu; Lai, Ping; Liu, Qingdong; Zeng, Qifeng; Lu, Junqiang; Guo, Xianglong

    2018-02-01

    The tangential fretting wear of three kinds of zirconium alloys tube mated with 304 stainless steel (SS) plate was investigated. The tests were conducted in an autoclave containing 300 °C pressurized B-Li water for tube-on-plate contact configuration. The worn surfaces were examined with scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and 3D microscopy. The cross-section of wear scar was examined with transmission electron microscope (TEM). The results indicated that the dominant wear mechanism of zirconium alloys in this test condition was delamination and oxidation. The oxide layer on the fretted area consists of outer oxide layer composed of iron oxide and zirconium oxide and inner oxide layer composed of zirconium oxide.

  7. 40 CFR 721.10602 - Lead niobium titanium zirconium oxide.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... as specified in § 721.90 (a)(4), (b)(4), and (c)(4) (Where N=8, and 8 is an aggregate of releases for the following substances: Lead strontium titanium zirconium oxide (PMN P-11-270; CAS No. 61461-40-3... strontium titanium tungsten oxide (PMN P-11-272; CAS No. 1262279-30-0); Lanthanum lead titanium zirconium...

  8. 40 CFR 721.10602 - Lead niobium titanium zirconium oxide.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... as specified in § 721.90 (a)(4), (b)(4), and (c)(4) (Where N=8, and 8 is an aggregate of releases for the following substances: Lead strontium titanium zirconium oxide (PMN P-11-270; CAS No. 61461-40-3... strontium titanium tungsten oxide (PMN P-11-272; CAS No. 1262279-30-0); Lanthanum lead titanium zirconium...

  9. Method for preparing hydrous zirconium oxide gels and spherules

    DOEpatents

    Collins, Jack L.

    2003-08-05

    Methods for preparing hydrous zirconium oxide spherules, hydrous zirconium oxide gels such as gel slabs, films, capillary and electrophoresis gels, zirconium monohydrogen phosphate spherules, hydrous zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite sorbent, zirconium monohydrogen phosphate spherules having suspendable particles of at least one different sorbent homogeneously embedded within to form a composite sorbent having a desired crystallinity, zirconium oxide spherules having suspendable particles homogeneously embedded within to form a composite, hydrous zirconium oxide fiber materials, zirconium oxide fiber materials, hydrous zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite, zirconium oxide fiber materials having suspendable particles homogeneously embedded within to form a composite and spherules of barium zirconate. The hydrous zirconium oxide spherules and gel forms prepared by the gel-sphere, internal gelation process are useful as inorganic ion exchangers, catalysts, getters and ceramics.

  10. Refractory Materials of Zirconate. Part 2: Synthesis and some properties of strontium, zirconate, calcium zirconate and barium zirconate

    NASA Technical Reports Server (NTRS)

    Okubo, Tsutomo; Yonemochi, Osamu; Nakamura, Kazuo; Maeda, Minoru

    1988-01-01

    Chemical compounds SrZrO3, CaZrO3, and BaZrO3 were synthesized by solid reaction and arc fusion, and their properties examined. Results were as follows: (1) in the synthesis of CaZrO3 by solid reaction, ZrO2 solid solution with cubic form was produced, which then changed into CaZrO3; (2) the BaZrO3 was a cubic form and did not show any transformation, while SrZrO3 and CaZrO3 with an orthorhombic form transformed to a cubic form at high temperature; and (3) the solubility of BaZrO3 in acid and its vaporization rate at a high temperature were greater than those of zirconates.

  11. Dielectric and modulus studies of polycrystalline BaZrO3 ceramic

    NASA Astrophysics Data System (ADS)

    Saini, Deepash S.; Singh, Sunder; Kumar, Anil; Bhattacharya, D.

    2018-05-01

    In the present work, dielectric and modulus studies of polycrystalline BaZrO3 ceramic, prepared by modified combustion method followed by conventional sintering, are investigated over the frequency range of 100 Hz to 106 Hz at different temperatures from 250 to 500 °C in air. The high value of dielectric constant (ɛ' ˜ 103) of BaZrO3 at high temperature and low frequency can be attributed to the Maxwell-Wagner polarization mechanism as well as to the thermally activated mechanism of charge carriers. Electric modulus reveal two type relaxations in the 250 °C to 800 °C temperature region as studied at different frequencies over 100 Hz to 106 Hz in air.

  12. Hydration characteristics of zirconium oxide replaced Portland cement for use as a root-end filling material.

    PubMed

    Camilleri, J; Cutajar, A; Mallia, B

    2011-08-01

    Zirconium oxide can be added to dental materials rendering them sufficiently radiopaque. It can thus be used to replace the bismuth oxide in mineral trioxide aggregate (MTA). Replacement of Portland cement with 30% zirconium oxide mixed at a water/cement ratio of 0.3 resulted in a material with adequate physical properties. This study aimed at investigating the microstructure, pH and leaching in physiological solution of Portland cement replaced zirconium oxide at either water-powder or water-cement ratios of 0.3 for use as a root-end filling material. The hydration characteristics of the materials which exhibited optimal behavior were evaluated. Portland cement replaced by zirconium oxide in varying amounts ranging from 0 to 50% in increments of 10 was prepared and divided into two sets. One set was prepared at a constant water/cement ratio while the other set at a constant water/powder ratio of 0.3. Portland cement and MTA were used as controls. The materials were analyzed under the scanning electron microscope (SEM) and the hydration products were determined. X-ray energy dispersive analysis (EDX) was used to analyze the elemental composition of the hydration products. The pH and the amount of leachate in Hank's balanced salt solution (HBSS) were evaluated. A material that had optimal properties that satisfied set criteria and could replace MTA was selected. The microstructure of the prototype material and Portland cement used as a control was assessed after 30 days using SEM and atomic ratio diagrams of Al/Ca versus Si/Ca and S/Ca versus Al/Ca were plotted. The hydration products of Portland cement replaced with 30% zirconium oxide mixed at water/cement ratio of 0.3 were calcium silicate hydrate, calcium hydroxide and minimal amounts of ettringite and monosulphate. The calcium hydroxide leached in HBSS solution resulted in an increase in the pH value. The zirconium oxide acted as inert filler and exhibited no reaction with the hydration by-products of Portland cement. A prototype dental material composed of Portland cement replaced with 30% zirconium oxide as radiopacifier leached calcium ions on hydration which reacted with phosphates present in simulated tissue fluids. This resulted in bioactive cement that could prospectively be used as a root-end filling material. The zirconium oxide acted as inert filler and did not participate in the hydration reaction of the Portland cement. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

  13. The Effect of Luting Cement and Titanium Base on the Final Color of Zirconium Oxide Core Material.

    PubMed

    Capa, Nuray; Tuncel, Ilkin; Tak, Onjen; Usumez, Aslihan

    2017-02-01

    To evaluate the effects of different types of luting cements and different colors of zirconium cores on the final color of the restoration that simulates implant-supported fixed partial dentures (FPDs) by using a titanium base on the bottom. One hundred and twenty zirconium oxide core plates (Zr-Zahn; 10 mm in width, 5 mm in length, 0.5 mm in height) were prepared in different shades (n = 20; noncolored, A2, A3, B1, C2, D2). The specimens were subdivided into two subgroups for the two types of luting cements (n = 10). The initial color measurements were made on zirconium oxide core plates using a spectrometer. To create the cement thicknesses, stretch strips with holes in the middle (5 mm in diameter, 70 μm in height) were used. The second measurement was done on the zirconium oxide core plates after the application of the resin cement (U-200, A2 Shade) or polycarboxylate cement (Lumicon). The final measurement was done after placing the titanium discs (5 mm in diameter, 3 mm in height) in the bottom. The data were analyzed with two-way ANOVA and Tukey's honestly significant differences (HSD) tests (α = 0.05). The ∆E* ab value was higher in the resin cement-applied group than in the polycarboxylate cement-applied group (p < 0.001). The highest ∆E* ab value was recorded for the zirconium oxide core-resin cement-titanium base, and the lowest was recorded for the polycarboxylate cement-zirconium oxide core (p < 0.001). The luting cement, the presence of titanium, and the color of zirconium are all important factors that determine the final shade of zirconia cores in implant-supported FPDs. © 2015 by the American College of Prosthodontists.

  14. Layer Protecting the Surface of Zirconium Used in Nuclear Reactors.

    PubMed

    Ashcheulov, Petr; Skoda, Radek; Skarohlíd, Jan; Taylor, Andrew; Fendrych, Frantisek; Kratochvílová, Irena

    2016-01-01

    Zirconium alloys have very useful properties for nuclear facilities applications having low absorption cross-section of thermal electrons, high ductility, hardness and corrosion resistance. However, there is also a significant disadvantage: it reacts with water steam and during this (oxidative) reaction it releases hydrogen gas, which partly diffuses into the alloy forming zirconium hydrides. A new strategy for surface protection of zirconium alloys against undesirable oxidation in nuclear reactors by polycrystalline diamond film has been patented- Czech patent 305059: Layer protecting the surface of zirconium alloys used in nuclear reactors and PCT patent: Layer for protecting surface of zirconium alloys (Patent Number: WO2015039636-A1). The zirconium alloy surface was covered by polycrystalline diamond layer grown in plasma enhanced chemical vapor deposition apparatus with linear antenna delivery system. Substantial progress in the description and understanding of the polycrystalline diamond/ zirconium alloys interface and material properties under standard and nuclear reactors conditions (irradiation, hot steam oxidation experiments and heating-quenching cycles) was made. In addition, process technology for the deposition of protective polycrystalline diamond films onto the surface of zirconium alloys was optimized. Zircaloy2 nuclear fuel pins were covered by 300 nm thick protective polycrystalline diamond layer (PCD) using plasma enhanced chemical vapor deposition apparatus with linear antenna delivery system. The polycrystalline diamond layer protects the zirconium alloy surface against undesirable oxidation and consolidates its chemical stability while preserving its functionality. PCD covered Zircaloy2 and standard Zircaloy2 pins were for 30 min. oxidized in 1100°C hot steam. Under these conditions α phase of zirconium changes to β phase (more opened for oxygen/hydrogen diffusion). PCD anticorrosion protection of Zircaloy nuclear fuel assemblies can significantly prolong lifetime of Zirconium alloy in nuclear reactors even above Zirconium phase transition temperatures. Even after ion beam irradiation (10 dpa, 3 MeV Fe(2+)) the diamond film still shows satisfactory structural integrity with both sp(3) and sp(2) carbon phases. Zircaloy2 under the carbon-based protective layer after hot steam oxidation test differed from the original Zircaloy2 material composition only very slightly, proving that the diamond coating increases the material resistance to high temperature oxidation. Zirconium alloys nuclear fuel pins' surfaces were covered by compact and homogeneous polycrystalline diamond layers consisting of sp(3) and sp(2) carbon phases with a high crystalline diamond content and low roughness. Diamond withstands very high temperatures, has excellent thermal conductivity and low chemical reactivity, it does not degrade over time and (important for the nuclear fuel cladding) being pure carbon, it has perfect neutron cross-section properties. Moreover, polycrystalline diamond layers consisting of crystalline (sp(3)) and amorphous (sp(2)) carbon phases could have suitable thermal expansion. Zirconium alloys coated with polycrystalline diamond film are protected against undesirable changes and processes. Further, the polycrystalline diamond layer prevents the reaction between the alloy surface and water vapor. During such reaction, water molecules dissociate and initiate formation of zirconium dioxide and hydrogen, accompanied by the release of large amount of heat. Thus the protective layer prevents the formation of hydrogen and the release of reaction heat. Few relevant patents to the topic have been reviewed and cited.

  15. Comparison of Zirconium Phosphonate-Modified Surfaces for Immobilizing Phosphopeptides and Phosphate-Tagged Proteins.

    PubMed

    Forato, Florian; Liu, Hao; Benoit, Roland; Fayon, Franck; Charlier, Cathy; Fateh, Amina; Defontaine, Alain; Tellier, Charles; Talham, Daniel R; Queffélec, Clémence; Bujoli, Bruno

    2016-06-07

    Different routes for preparing zirconium phosphonate-modified surfaces for immobilizing biomolecular probes are compared. Two chemical-modification approaches were explored to form self-assembled monolayers on commercially available primary amine-functionalized slides, and the resulting surfaces were compared to well-characterized zirconium phosphonate monolayer-modified supports prepared using Langmuir-Blodgett methods. When using POCl3 as the amine phosphorylating agent followed by treatment with zirconyl chloride, the result was not a zirconium-phosphonate monolayer, as commonly assumed in the literature, but rather the process gives adsorbed zirconium oxide/hydroxide species and to a lower extent adsorbed zirconium phosphate and/or phosphonate. Reactions giving rise to these products were modeled in homogeneous-phase studies. Nevertheless, each of the three modified surfaces effectively immobilized phosphopeptides and phosphopeptide tags fused to an affinity protein. Unexpectedly, the zirconium oxide/hydroxide modified surface, formed by treating the amine-coated slides with POCl3/Zr(4+), afforded better immobilization of the peptides and proteins and efficient capture of their targets.

  16. TEM study on the initial oxidation of Zircaloy-4 thin foil specimens heated in a low vacuum air condition at 280-300 °C

    NASA Astrophysics Data System (ADS)

    Wang, Zhen; Zhou, Bang-xin; Zhu, Wei; Wen, Bang; Yao, Mei-yi; Li, Qiang; Wu, Lu; Zhang, Jin-long; Fang, Zhong-qiang

    2017-04-01

    As one of the important structural materials in nuclear industry, the corrosion resistance of zirconium alloy limits their in-pile application. Therefore, it is necessary to investigate the corrosion mechanism of zirconium alloys. The zirconium-oxygen reaction at the O/M interface is one of the factors that affect the oxidation process. There are few reports in this regard. Ideally, the reaction process at the O/M interface has certain relevance with the initiation oxidation of zirconium, which provided a new way to investigate the reaction process by observing the initiation oxidation behaviours. To investigate the oxidation behaviours of zirconium alloy at the initial stage, in this paper, zircaloy-4 TEM thin foil specimens in 3 mm diameter were studied by TEM observation after heating in air condition with a vacuum of 3 Pa at 280 °C, 290 °C and 300 °C for 30 min exposures. The results show that, ZrO2 begin to nucleate at a size of 3-5 nm at a high Zr/O ratio of 10.4 and oxide layer formed while Zr/O was 4.6. As a result of stress caused by the P.B ratio of Zr, slip bands formed and a bcc structure sub-oxide b-ZrOx (a = 0.51 nm) grew up along with the slip bands was observed. At both sides of b-ZrOx, two hcp structure sub-oxides having the same a-axis lattice parameter and different c-axis lattice parameter were detected.

  17. In vitro tensile bond strength of adhesive cements to new post materials.

    PubMed

    O'Keefe, K L; Miller, B H; Powers, J M

    2000-01-01

    The purpose of this study was to measure the in vitro tensile bond strength of 3 types of adhesive resin cements to stainless steel, titanium, carbon fiber-reinforced resin, and zirconium oxide post materials. Disks of post materials were polished to 600 grit, air abraded, and ultrasonically cleaned. Zirconium oxide bonding surfaces were pretreated with hydrofluoric acid and silanated. Bis-Core, C&B Metabond, and Panavia cements were bonded to the post specimens and placed in a humidor for 24 hours. Post specimens were debonded in tension. Means and standard deviations (n = 5) were analyzed by 2-way analysis of variance. Tukey-Kramer intervals at the 0.05 significance level were calculated. Failure modes were observed. Panavia 21 provided the highest bond strengths for all types of post materials, ranging from 22 MPa (zirconium oxide) to 37 MPa (titanium). C&B Metabond bonded significantly more strongly to stainless steel (27 MPa) and titanium (22 MPa) than to zirconium oxide (7 MPa). Bis-Core results were the lowest, ranging from 16 MPa (stainless steel) to 8 MPa (zirconium oxide). In most cases, bonds to carbon fiber post materials were weaker than to stainless steel and titanium, but stronger than to zirconium oxide. In general, higher bond strengths resulted in a higher percentage of cohesive failures within the cement. Panavia 21 provided the highest bond strengths to all post materials, followed by C&B Metabond. In most cases, adhesive resins had higher bond strengths to stainless steel, titanium, and carbon fiber than to zirconium oxide.

  18. Fabrication of oxide layer on zirconium by micro-arc oxidation: Structural and antimicrobial characteristics.

    PubMed

    Fidan, S; Muhaffel, F; Riool, M; Cempura, G; de Boer, L; Zaat, S A J; Filemonowicz, A Czyrska-; Cimenoglu, H

    2017-02-01

    The aim of this study was to cover the surfaces of zirconium (Zr) with an antimicrobial layer for biomedical applications. For this purpose, the micro-arc oxidation (MAO) process was employed in a sodium silicate and sodium hydroxide containing base electrolyte with and without addition of silver acetate (AgC 2 H 3 O 2 ). In general, synthesized MAO layers were composed of zirconium oxide (ZrO 2 ) and zircon (ZrSiO 4 ). Addition of AgC 2 H 3 O 2 into the base electrolyte caused homogenous precipitation of silver-containing particles in the MAO layer, which exhibited excellent antibacterial efficiency against methicillin-resistant Staphylococcus aureus (MRSA) as compared to the untreated and MAO-treated Zr. Copyright © 2016 Elsevier B.V. All rights reserved.

  19. Thermoluminescence (TL) of europium-doped ZrO2 obtained by sol-gel method

    NASA Astrophysics Data System (ADS)

    Rivera, T.; Furetta, C.; Azorín, J.; Barrera, M.; Soto, A. M.

    This article reports the preparation and characterization of europium-doped zirconium oxide (ZrO2:Eu3+) formed by homogeneous precipitation from propoxyde of zirconium [Zr(OC3H7)4]. The alkoxide sol gel process is an efficient method to prepare the zirconium oxide matrix by the hydrolysis of alkoxide precursors followed by condensation to yield a polymeric oxo-bridged ZrO2 network. All compounds were characterized by thermal analysis and the X-ray diffractometry method. The thermoluminescence (TL) emission properties of ZrO2:Eu3+ under beta radiation effects are studied. The europium-doped sintered zirconia powder presents a TL glow curve with two peaks (Tmax) centered at around 204 and around 292 °C, respectively. TL response of ZrO2:Eu3+ as a function of beta-absorbed dose was linear from 2 Gy up to 90 Gy. The europium ion (Eu3+)-doped ZrO2 was found to be more sensitive to beta radiation than undoped ZrO2 obtained by the same method and presented a little fading of the TL signal compared with undoped zirconium oxide.

  20. Electroless deposition process for zirconium and zirconium alloys

    DOEpatents

    Donaghy, R. E.; Sherman, A. H.

    1981-08-18

    A method is disclosed for preventing stress corrosion cracking or metal embrittlement of a zirconium or zirconium alloy container that is to be coated on the inside surface with a layer of a metal such as copper, a copper alloy, nickel, or iron and used for holding nuclear fuel material as a nuclear fuel element. The zirconium material is etched in an etchant solution, desmutted mechanically or ultrasonically, oxidized to form an oxide coating on the zirconium, cleaned in an aqueous alkaline cleaning solution, activated for electroless deposition of a metal layer and contacted with an electroless metal plating solution. This method provides a boundary layer of zirconium oxide between the zirconium container and the metal layer. 1 fig.

  1. Electroless deposition process for zirconium and zirconium alloys

    DOEpatents

    Donaghy, Robert E.; Sherman, Anna H.

    1981-01-01

    A method is disclosed for preventing stress corrosion cracking or metal embrittlement of a zirconium or zirconium alloy container that is to be coated on the inside surface with a layer of a metal such as copper, a copper alloy, nickel, or iron and used for holding nuclear fuel material as a nuclear fuel element. The zirconium material is etched in an etchant solution, desmutted mechanically or ultrasonically, oxidized to form an oxide coating on the zirconium, cleaned in an aqueous alkaline cleaning solution, activated for electroless deposition of a metal layer and contacted with an electroless metal plating solution. This method provides a boundary layer of zirconium oxide between the zirconium container and the metal layer.

  2. Efficient One-Pot Synthesis of Colloidal Zirconium Oxide Nanoparticles for High-Refractive-Index Nanocomposites.

    PubMed

    Liu, Chao; Hajagos, Tibor Jacob; Chen, Dustin; Chen, Yi; Kishpaugh, David; Pei, Qibing

    2016-02-01

    Zirconium oxide nanoparticles are promising candidates for optical engineering, photocatalysis, and high-κ dielectrics. However, reported synthetic methods for the colloidal zirconium oxide nanoparticles use unstable alkoxide precursors and have various other drawbacks, limiting their wide application. Here, we report a facile one-pot method for the synthesis of colloidally stable zirconium oxide nanoparticles. Using a simple solution of zirconium trifluoroacetate in oleylamine, highly stable zirconium oxide nanoparticles have been synthesized with high yield, following a proposed amidization-assisted sol-gel mechanism. The nanoparticles can be readily dispersed in nonpolar solvents, forming a long-term stable transparent solution, which can be further used to fabricate high-refractive-index nanocomposites in both monolith and thin-film forms. In addition, the same method has also been extended to the synthesis of titanium oxide nanoparticles, demonstrating its general applicability to all group IVB metal oxide nanoparticles.

  3. THE ANALYSIS OF URANIUM-ZIRCONIUM ALLOYS

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

    Milner, G.W.C.; Skewies, A.F.

    1953-03-01

    A satisfactory procedure is described for the analysis of uranium-zirconium alloys containing up to 25% zirconium. It is based on the separation of the zirconium from the uranium by dissolving the cupferron complex of the former element into chloroform. After the evaporation of the solvent from the combined organic extracts, the residue is ignited to zirconium oxide. The latter is then re-dissolved and zirconium is separated from other elements co-extracted in the solvent extraction procedure by precipitation with mandelic acid. The zirconium mandelate is finally ignited to oxide at 960 deg C. The uranium is separated from the aqueous solutionmore » remaining from the cupferron extraction by precipitating with tannin at a pH of 8; the precipitate being removed by filtration and then ignited a t 800 deg C. The residue is dissolved in nitric acid and the uranium is finally determined by precipitating as ammonium diuranate and then igniting to U{sub 3}O{sub 8}. (auth)« less

  4. Oxide film on metal substrate reduced to form metal-oxide-metal layer structure

    NASA Technical Reports Server (NTRS)

    Youngdahl, C. A.

    1967-01-01

    Electrically conductive layer of zirconium on a zirconium-oxide film residing on a zirconium substrate is formed by reducing the oxide in a sodium-calcium solution. The reduced metal remains on the oxide surface as an adherent layer and seems to form a barrier that inhibits further reaction.

  5. About structural phase state of coating based on zirconium oxide formed by microplasma oxidation method

    NASA Astrophysics Data System (ADS)

    Gubaidulina, Tatiana A.; Sergeev, Viktor P.; Kuzmin, Oleg S.; Fedorischeva, Marina V.; Kalashnikov, Mark P.

    2017-12-01

    The oxide-ceramic coating based of zirconium oxide is formed by the method of microplasma oxidation. The producing modes of the oxide layers on E110 zirconium alloy are under testing. It was found that using microplasma treatment of E110 zirconium in aluminosilicate electrolyte makes possible the formation of porous oxide-ceramic coatings based on zirconium alloyed by aluminum and niobium. The study is focused on the modes how to form heat-shielding coatings with controlled porosity and minimal amount of microcracks. The structural-phase state of the coating is studied by X-ray diffraction analysis and scanning electron microscopy (SEM). It was found that the ratio of the monoclinic and tetragonal phases changes with the change occurring in the coating formation modes.

  6. Color variation induced by abutments in the superior anterior maxilla: an in vitro study in the pig gingiva.

    PubMed

    Atash, Ramin; Boularbah, Mohamed-Reda; Sibel, Cetik

    2016-12-01

    The aim of this work is to evaluate different types of materials used for making implant abutments, by means of an in vitro study and a review of the literature, in order to identify the indications for a better choice of an implant-supported restoration in the anterior section. 5 implant abutments were tested in a random order in the superior anterior maxilla of pig gingiva (n = 8): titanium dioxide (Nobel Biocare); zirconium dioxide, Standard BO shade (Nobel Biocare, Kloten, Switzerland); zirconium dioxide, Light BI shade (Nobel Biocare); zirconium dioxide, Intense A 3.5 shade (Nobel Biocare); and aluminium oxide. Each abutment was tested for 2 mm and 3 mm thickness. To determine color variation, VITA Easyshade Advance spectrophotometer (Vita Zahnfabrik, Bad Sackingen, Germany) was used. Results showed that the color variation induced by the abutment would be affected by the abutment material and gingival thickness, when the gingival thickness is 2 mm. All materials except zirconium dioxide (Standard shade) caused a visible change of color. Then, as the thickness of the gingiva increased to 3 mm, the color variation was attenuated in a significant manner and became invisible for all types of abutments, except those made of aluminium oxide. Zirconium dioxide is the material causing the lowest color variation at 2 mm and at 3 mm, whereas aluminium oxide causes the highest color variation no matter the thickness.

  7. Zirconium doped nano-dispersed oxides of Fe, Al and Zn for destruction of warfare agents

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

    Stengl, Vaclav, E-mail: stengl@uach.cz; Houskova, Vendula; Bakardjieva, Snejana

    2010-11-15

    Zirconium doped nano dispersive oxides of Fe, Al and Zn were prepared by a homogeneous hydrolysis of the respective sulfate salts with urea in aqueous solutions. Synthesized metal oxide hydroxides were characterized using Brunauer-Emmett-Teller (BET) surface area and Barrett-Joiner-Halenda porosity (BJH), X-ray diffraction (XRD), infrared spectroscopy (IR), scanning electron microscopy (SEM) and energy-dispersive X-ray microanalysis (EDX). These oxides were taken for an experimental evaluation of their reactivity with sulfur mustard (HD or bis(2-chloroethyl)sulfide), soman (GD or (3,3'-Dimethylbutan-2-yl)-methylphosphonofluoridate) and VX agent (S-[2-(diisopropylamino)ethyl]-O-ethyl-methylphosphonothionate). The presence of Zr{sup 4+} dopant can increase both the surface area and the surface hydroxylation of the resultingmore » doped oxides, decreases their crystallites' sizes thereby it may contribute in enabling the substrate adsorption at the oxide surface thus it can accelerate the rate of degradation of warfare agents. Addition of Zr{sup 4+} converts the product of the reaction of ferric sulphate with urea from ferrihydrite to goethite. We found out that doped oxo-hydroxides Zr-FeO(OH) - being prepared by a homogeneous hydrolysis of ferric and zirconium oxo-sulfates mixture in aqueous solutions - exhibit a comparatively higher degradation activity towards chemical warfare agents (CWAs). Degradation of soman or VX agent on Zr-doped FeO(OH) containing ca. 8.3 wt.% of zirconium proceeded to completion within 30 min.« less

  8. Methods of repairing a substrate

    NASA Technical Reports Server (NTRS)

    Riedell, James A. (Inventor); Easler, Timothy E. (Inventor)

    2011-01-01

    A precursor of a ceramic adhesive suitable for use in a vacuum, thermal, and microgravity environment. The precursor of the ceramic adhesive includes a silicon-based, preceramic polymer and at least one ceramic powder selected from the group consisting of aluminum oxide, aluminum nitride, boron carbide, boron oxide, boron nitride, hafnium boride, hafnium carbide, hafnium oxide, lithium aluminate, molybdenum silicide, niobium carbide, niobium nitride, silicon boride, silicon carbide, silicon oxide, silicon nitride, tin oxide, tantalum boride, tantalum carbide, tantalum oxide, tantalum nitride, titanium boride, titanium carbide, titanium oxide, titanium nitride, yttrium oxide, zirconium boride, zirconium carbide, zirconium oxide, and zirconium silicate. Methods of forming the ceramic adhesive and of repairing a substrate in a vacuum and microgravity environment are also disclosed, as is a substrate repaired with the ceramic adhesive.

  9. Self-assembled Co-BaZrO 3 nanocomposite thin films with ultra-fine vertically aligned Co nanopillars

    DOE PAGES

    Huang, Jijie; Li, Leigang; Lu, Ping; ...

    2017-05-11

    A simple one-step pulsed laser deposition (PLD) method has been applied to grow self-assembled metal-oxide nanocomposite thin films. The as-deposited Co-BaZrO 3 films show high epitaxial quality with ultra-fine vertically aligned Co nanopillars (diameter <5 nm) embeded in BZO matrix. The diameter of the nanopillars can be further tuned by varying the deposition frequency. The metal and oxide phases grow separately without inter-diffusion or mixing. Taking advantage of this unique structure, a high saturation magnetization of ~1375 emu/cm 3 in the Co- BaZrO 3 nanocomposites has been achieved and further confirmed by Lorentz microscopy imaging in TEM. Furthermore, the coercivitymore » values of this nanocomposite thin films range from 600 Oe (20 Hz) to 1020 Oe (2 Hz), which makes the nanocomposite an ideal candidate for high-density perpendicular recording media.« less

  10. Effect of surface treatment and type of cement on push-out bond strength of zirconium oxide posts.

    PubMed

    Almufleh, Balqees S; Aleisa, Khalil I; Morgano, Steven M

    2014-10-01

    The effect of the surface treatment of zirconium oxide posts on their push-out bond strength is controversial. The purpose of this study was to compare the effects of 2 surface treatments on the bond strength of zirconium oxide posts cemented with different cements and to assess the failure mode. Seventy extracted human teeth were divided into 7 groups (n=10). Custom zirconium oxide posts (Cercon; Degudent) were fabricated for 6 groups. Posts in 3 groups were airborne-particle abraded (A). Posts in the other 3 groups were tribochemical silica coated (T). Three cements were used. Zinc phosphate cement was used to cement the zirconium oxide posts in groups AZ and TZ, RelyX ARC cement was used in groups ARA and TRA, and RelyX Unicem cement was used in groups ARU and TRU. Group C contained custom metal posts cemented with zinc phosphate cement. Specimens were horizontally sectioned into 3 sections and subjected to a push-out test. A mixed model analysis of variance, 1-way ANOVA, and the Tukey multiple comparison tests were used for statistical analysis. The highest push-out bond strength was recorded for Group ARU (21.03 MPa), and the lowest was recorded for Group ARA (7.57 MPa). No significant difference in push-out bond strength was found among the different surface treatments and root regions (P>.05). The type of cement had a significant effect on the push-out bond strength of zirconium oxide posts (P=.049). RelyX Unicem cement recorded (19.57 ±8.83 MPa) significantly higher push-out bond strength compared with zinc phosphate (9.95 ±6.31 MPa) and RelyX ARC cements (9.39 ±5.45 MPa). Adhesive failure at the post-cement interface was recorded for 75% of the posts cemented with zinc phosphate and RelyX ARC cements, while mixed failure was recorded for 75% of the posts cemented with RelyX Unicem cement. The type of cement used resulted in a statistically significant difference in the push-out bond strength of zirconium oxide posts, while both the surface treatment and root region resulted in no statistically significant effect after artificial aging. RelyX Unicem cement had significantly higher push-out bond strength than did zinc phosphate and RelyX ARC cements. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  11. Development of Self-Healing Zirconium-Silicide Coatings for Improved Performance Zirconium-Alloy Fuel Cladding

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

    Sridharan, Kumar; Mariani, Robert; Bai, Xianming

    Zirconium-alloy fuel claddings have been used successfully in Light Water Reactors (LWR) for over four decades. However, under high temperature accident conditions, zirconium-alloys fuel claddings exhibit profuse exothermic oxidation accompanied by release of hydrogen gas due to the reaction with water/steam. Additionally, the ZrO 2 layer can undergo monoclinic to tetragonal to cubic phase transformations at high temperatures which can induce stresses and cracking. These events were unfortunately borne out in the Fukushima-Daiichi accident in in Japan in 2011. In reaction to such accident, protective oxidation-resistant coatings for zirconium-alloy fuel claddings has been extensively investigated to enhance safety margins inmore » accidents as well as fuel performance under normal operation conditions. Such surface modification could also beneficially affect fuel rod heat transfer characteristics. Zirconium-silicide, a candidate coating material, is particularly attractive because zirconium-silicide coating is expected to bond strongly to zirconium-alloy substrate. Intermetallic compound phases of zirconium-silicide have high melting points and oxidation of zirconium silicide produces highly corrosion resistant glassy zircon (ZrSiO 4) and silica (SiO 2) which possessing self-healing qualities. Given the long-term goal of developing such coatings for use with nuclear reactor fuel cladding, this work describes results of oxidation and corrosion behavior of bulk zirconium-silicide and fabrication of zirconium-silicide coatings on zirconium-alloy test flats, tube configurations, and SiC test flats. In addition, boiling heat transfer of these modified surfaces (including ZrSi 2 coating) during clad quenching experiments is discussed in detail.« less

  12. Oxidized zirconium on ceramic; Catastrophic coupling.

    PubMed

    Ozden, V E; Saglam, N; Dikmen, G; Tozun, I R

    2017-02-01

    Oxidized zirconium (Oxinium™; Smith & Nephew, Memphis, TN, USA) articulated with polyethylene in total hip arthroplasty (THA) appeared to have the potential to reduce wear dramatically. The thermally oxidized metal zirconium surface is transformed into ceramic-like hard surface that is resistant to abrasion. The exposure of soft zirconium metal under hard coverage surface after the damage of oxidized zirconium femoral head has been described. It occurred following joint dislocation or in situ succeeding disengagement of polyethylene liner. We reported three cases of misuse of Oxinium™ (Smith & Nephew, Memphis, TN, USA) heads. These three cases resulted in catastrophic in situ wear and inevitable failure although there was no advice, indication or recommendation for this use from the manufacturer. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

  13. Effect of zirconium oxide nanofiller and dibutyl phthalate plasticizer on ionic conductivity and optical properties of solid polymer electrolyte.

    PubMed

    Yasin, Siti Mariah Mohd; Ibrahim, Suriani; Johan, Mohd Rafie

    2014-01-01

    New solid polymer electrolytes (SPE) based on poly(ethylene oxide) (PEO) doped with lithium trifluoromethanesulfonate (LiCF3SO3), dibutyl phthalate (DBP) plasticizer, and zirconium oxide (ZrO2) nanoparticles were prepared by solution-casting technique. The conductivity was enhanced by addition of dibutyl phthalate (DBP) plasticizer and ZrO2 nanofiller with maximum conductivity (1.38 × 10(-4) Scm(-1)). The absorption edge and band gap values showed decreases upon addition of LiSO3CF3, DBP, and ZrO2 due to the formation of localized states in the SPE and the degree of disorder in the films increased.

  14. Effect of Zirconium Oxide Nanofiller and Dibutyl Phthalate Plasticizer on Ionic Conductivity and Optical Properties of Solid Polymer Electrolyte

    PubMed Central

    Yasin, Siti Mariah Mohd; Ibrahim, Suriani

    2014-01-01

    New solid polymer electrolytes (SPE) based on poly(ethylene oxide) (PEO) doped with lithium trifluoromethanesulfonate (LiCF3SO3), dibutyl phthalate (DBP) plasticizer, and zirconium oxide (ZrO2) nanoparticles were prepared by solution-casting technique. The conductivity was enhanced by addition of dibutyl phthalate (DBP) plasticizer and ZrO2 nanofiller with maximum conductivity (1.38 × 10−4 Scm−1). The absorption edge and band gap values showed decreases upon addition of LiSO3CF3, DBP, and ZrO2 due to the formation of localized states in the SPE and the degree of disorder in the films increased. PMID:25133244

  15. Thermochemistry of amorphous and crystalline zirconium and hafnium silicates.

    NASA Astrophysics Data System (ADS)

    Ushakov, S.; Brown, C. E.; Navrotsky, Alexandra; Boatner, L. A.; Demkov, A. A.; Wang, C.; Nguyen, B.-Y.

    2003-03-01

    Calorimetric investigation of amorphous and crystalline zirconium and hafnium silicates was performed as part of a research program on thermochemistry of alternative gate dielectrics. Amorphous hafnium and zirconium silicates with varying SiO2 content were synthesized by a sol-gel process. Crystalline zirconium and hafnium silicates (zircon and hafnon) were synthesized by solid state reaction at 1450 °C from amorphous gels and grown as single crystals from flux. High temperature oxide melt solution calorimetry in lead borate (2PbO.B2O3) solvent at 800 oC was used to measure drop solution enthalpies for amorphous and crystalline zirconium and hafnium silicates and corresponding oxides. Applying appropriate thermochemical cycles, formation enthalpy of crystalline ZrSiO4 (zircon) from binary oxides (baddeleite and quartz) at 298 K was calculated as -23 +/-2 kJ/mol and enthalpy difference between amorphous and crystalline zirconium silicate (vitrification enthalpy) was found to be 61 +/-3 kJ/mol. Crystallization onset temperatures of amorphous zirconium and hafnium silicates, as measured by differential scanning calorimetry (DSC), increased with silica content. The resulting crystalline phases, as characterized by X-ray diffraction (XRD), were tetragonal HfO2 and ZrO2. Critical crystallite size for tetragonal to monoclinic transformation of HfO2 in the gel was estimated as 6 +/-2 nm from XRD data Crystallization enthalpies per mole of hafnia and zirconia in gels decrease slightly together with crystallite size with increasing silica content, for example from -22 to -15 +/-1 kJ per mol of HfO2 crystallized at 740 and 1006 °C from silicates with 10 and 70 mol Applications of thermal analyses and solution calorimetry techniques together with first-principles density functional calculations to estimate interface and surface energies are discussed.

  16. Functionally gradient material for membrane reactors to convert methane gas into value-added products

    DOEpatents

    Balachandran, U.; Dusek, J.T.; Kleefisch, M.S.; Kobylinski, T.P.

    1996-11-12

    A functionally gradient material for a membrane reactor for converting methane gas into value-added-products includes an outer tube of perovskite, which contacts air; an inner tube which contacts methane gas, of zirconium oxide, and a bonding layer between the perovskite and zirconium oxide layers. The bonding layer has one or more layers of a mixture of perovskite and zirconium oxide, with the layers transitioning from an excess of perovskite to an excess of zirconium oxide. The transition layers match thermal expansion coefficients and other physical properties between the two different materials. 7 figs.

  17. Functionally gradient material for membrane reactors to convert methane gas into value-added products

    DOEpatents

    Balachandran, Uthamalingam; Dusek, Joseph T.; Kleefisch, Mark S.; Kobylinski, Thadeus P.

    1996-01-01

    A functionally gradient material for a membrane reactor for converting methane gas into value-added-products includes an outer tube of perovskite, which contacts air; an inner tube which contacts methane gas, of zirconium oxide, and a bonding layer between the perovskite and zirconium oxide layers. The bonding layer has one or more layers of a mixture of perovskite and zirconium oxide, with the layers transitioning from an excess of perovskite to an excess of zirconium oxide. The transition layers match thermal expansion coefficients and other physical properties between the two different materials.

  18. CHARACTERISTICS OF ANODIC AND CORROSION FILMS ON ZIRCONIUM

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

    Misch, R.D.

    1960-05-01

    Zirconium anodizes similarly to tungsten in respect to the change of interference colors with applied voltage. However, the oxide layer on tungsten cannot reach as great a thickness. Hafnium does not anodize in the same way as zirconium but is similar to tantalum. By measuring the interference color and capacitative thicknesses on zirconium (Grades I and III) and a 2.5 wt.% tin ailoy, the film was found to grow less rapidly in terms of capacitance than in terms of iaterference colors. This was interpreted to mean that cracks develop in the oxide as it thickens. The effect was most pronouncedmore » on Grade III zirconium and least pronounced on the tin alloy. The reduction in capacitative thickness was especially noticeable when white oxide appeared. Comparative measurements on Grade I zirconium and 2.5 wt.% tin alloy indicated that the thickness of the oxide film on the tin alloy (after 16 hours in water) increased more rapidly with temperature than the film on zirconium. Tin is believed to act in ways to counteract the tendency of the oxide to form cracks, and to produce vacancies which promote ionic diffusion. (auth)« less

  19. Upward shift of the vortex solid phase in high-temperature-superconducting wires through high density nanoparticle addition

    DOE PAGES

    Miura, Masashi; Maiorov, Boris; Balakirev, Fedor F.; ...

    2016-02-08

    Here, we show a simple and effective way to improve the vortex irreversibility line up to very high magnetic fields (60T) by increasing the density of second phase BaZrO 3 nanoparticles. (Y 0.77,Gd 0.23)Ba 2Cu 3O y films were grown on metal substrates with different concentration of BaZrO 3 nanoparticles by the metal organic deposition method. We find that upon increase of the BaZrO 3 concentration, the nanoparticle size remains constant but the twin-boundary density increases. Up to the highest nanoparticle concentration (n ~ 1.3 × 10 22/m 3), the irreversibility field (H irr) continues to increase with no signmore » of saturation up to 60 T, although the vortices vastly outnumber pinning centers. We find extremely high H irr, namely H irr = 30 T (H||45°) and 24 T (H||c) at 65 K and 58 T (H||45°) and 45 T (H||c) at 50K. The difference in pinning landscape shifts the vortex solid-liquid transition upwards, increasing the vortex region useful for power applications, while keeping the upper critical field, critical temperature and electronic mass anisotropy unchanged.« less

  20. Surface characterization of anodized zirconium for biomedical applications

    NASA Astrophysics Data System (ADS)

    Sanchez, A. Gomez; Schreiner, W.; Duffó, G.; Ceré, S.

    2011-05-01

    Mechanical properties and corrosion resistance of zirconium make this material suitable for biomedical implants. Its good in vivo performance is mainly due to the presence of a protective oxide layer that minimizes corrosion rate, diminishes the amount of metallic ions released to the biological media and facilitates the osseointegration process. Since the implant surface is the region in contact with living tissues, the characteristics of the surface film are of great interest. Surface modification is a route to enhance both biocompatibility and corrosion resistance of permanent implant materials. Anodizing is presented as an interesting process to modify metal surfaces with good reproducibility and independence of the geometry. In this work the surface of zirconium before and after anodizing in 1 mol/L phosphoric acid solution at a fixed potential between 3 and 30 V, was characterized by means of several surface techniques. It was found that during anodization the surface oxide grows with an inhomogeneous coverage on zirconium surface, modifying the topography. The incorporation of P from the electrolyte to the surface oxide during the anodizing process changes the surface chemistry. After 30 days of immersion in Simulated Body Fluid (SBF) solution, Ca-P rich compounds were present on anodized zirconium.

  1. Ceramic material suitable for repair of a space vehicle component in a microgravity and vacuum environment, method of making same, and method of repairing a space vehicle component

    NASA Technical Reports Server (NTRS)

    Riedell, James A. (Inventor); Easler, Timothy E. (Inventor)

    2009-01-01

    A precursor of a ceramic adhesive suitable for use in a vacuum, thermal, and microgravity environment. The precursor of the ceramic adhesive includes a silicon-based, preceramic polymer and at least one ceramic powder selected from the group consisting of aluminum oxide, aluminum nitride, boron carbide, boron oxide, boron nitride, hafnium boride, hafnium carbide, hafnium oxide, lithium aluminate, molybdenum silicide, niobium carbide, niobium nitride, silicon boride, silicon carbide, silicon oxide, silicon nitride, tin oxide, tantalum boride, tantalum carbide, tantalum oxide, tantalum nitride, titanium boride, titanium carbide, titanium oxide, titanium nitride, yttrium oxide, zirconium diboride, zirconium carbide, zirconium oxide, and zirconium silicate. Methods of forming the ceramic adhesive and of repairing a substrate in a vacuum and microgravity environment are also disclosed, as is a substrate repaired with the ceramic adhesive.

  2. Aqueous sodium borohydride induced thermally stable porous zirconium oxide for quick removal of lead ions

    PubMed Central

    Nayak, Nadiya B.; Nayak, Bibhuti B.

    2016-01-01

    Aqueous sodium borohydride (NaBH4) is well known for its reducing property and well-established for the development of metal nanoparticles through reduction method. In contrary, this research paper discloses the importance of aqueous NaBH4 as a precipitating agent towards development of porous zirconium oxide. The boron species present in aqueous NaBH4 play an active role during gelation as well as phase separated out in the form of boron complex during precipitation, which helps to form boron free zirconium hydroxide [Zr(OH)4] in the as-synthesized condition. Evolved in-situ hydrogen (H2) gas-bubbles also play an important role to develop as-synthesized loose zirconium hydroxide and the presence of intra-particle voids in the loose zirconium hydroxide help to develop porous zirconium oxide during calcination process. Without any surface modification, this porous zirconium oxide quickly adsorbs almost hundred percentages of toxic lead ions from water solution within 15 minutes at normal pH condition. Adsorption kinetic models suggest that the adsorption process was surface reaction controlled chemisorption. Quick adsorption was governed by surface diffusion process and the adsorption kinetic was limited by pore diffusion. Five cycles of adsorption-desorption result suggests that the porous zirconium oxide can be reused efficiently for removal of Pb (II) ions from aqueous solution. PMID:26980545

  3. Zirconium-based conversion film formation on zinc, aluminium and magnesium oxides and their interactions with functionalized molecules

    NASA Astrophysics Data System (ADS)

    Fockaert, L. I.; Taheri, P.; Abrahami, S. T.; Boelen, B.; Terryn, H.; Mol, J. M. C.

    2017-11-01

    Zirconium-based conversion treatment of zinc, aluminium and magnesium oxides have been studied in-situ using ATR-FTIR in a Kretschmann geometry. This set-up was coupled to an electrochemical cell, which allowed to obtain chemical and electrochemical information simultaneously as a function of conversion time. This elucidated the strong relation between physico-chemical surface properties and zirconium-based conversion kinetics. Whereas the surface hydroxyl density of zinc and aluminium increased during conversion, magnesium (hydr)oxide was shown to dissolve in the acid solution. Due to this dissolution, strong surface alkalization can be expected, explaining the rapid conversion kinetics. AES depth profiling was used to determine the final oxide thickness and elemental composition. This confirmed that magnesium is most active and forms a zirconium oxide layer approximately 10 times thicker than zinc. On the other hand, the presence of zirconium oxide on aluminium is very low and can be considered as not fully covering the metal oxide. Additionally, the converted oxide chemistry was related to the bonding mechanisms of amide functionalized molecules using ATR-FTIR and XPS. It was shown that inclusion of zirconium altered the acid-base properties, increasing the substrate proton donating capabilities in case of magnesium oxide and increasing hydrogen bonding and Bronsted interactions due to increased surface hydroxide fractions on zinc and aluminium substrates.

  4. Oxidized zirconium head on crosslinked polyethylene liner in total hip arthroplasty: a 7- to 12-year in vivo comparative wear study.

    PubMed

    Karidakis, George K; Karachalios, Theofilos

    2015-12-01

    Osteolysis resulting from wear debris production from the bearing surfaces is a major factor limiting long-term survival of hip implants. Oxidized zirconium head on crosslinked polyethylene (XLPE) is a modern bearing coupling. However, midterm in vivo wear data of this coupling are not known. The purpose of this study was to investigate in vivo whether the combination of an oxidized zirconium femoral head on XLPE produces less wear than a ceramic head on XLPE or a ceramic head on conventional polyethylene (CPE) couplings and whether any of these bearing combinations results in higher hip scores. Between 2003 and 2007, we performed 356 total hip arthroplasties in 288 patients; of those, 199 (69.1%) patients (199 hips) were enrolled in what began as a randomized trial. Unfortunately, after the 57(th) patient, the randomization process was halted because of patients' preference for the oxidized zirconium bearing instead of the ceramic after (as they were informed by the consent form), and after that, alternate allocation to the study groups was performed. Hips were allocated into four groups: in Group A, a 28-mm ceramic head on CPE was used; in Group B, a 28-mm ceramic head on XLPE; in Group C, a 28-mm Oxinium head on XLPE; and in Group D, a 32-mm Oxinium head on XLPE. The authors prospectively collected in vivo wear data (linear wear, linear wear rate, volumetric wear, and volumetric wear rate) using PolyWare software. Preoperative and postoperative clinical data, including Harris and Oxford hip scores, were also collected at regular intervals. Of those patients enrolled, 188 (95%) were available for final followup at a minimum of 7 years (mean, 9 years; range, 7-12 years). All bearing surfaces showed a varying high bedding-in effect (plastic deformation of the liner) up to the second postoperative year. At 5 years both oxidized zirconium on XLPE groups showed lower (p < 0.01) volumetric wear (mean ± SD mm(3)) and volumetric wear rates (mean ± SD mm(3)/year) (Group C: 310 ± 55-206 ± 55 mm(3)/year, Group D: 320 ± 58-205 ± 61 mm(3)/year) when compared with ceramic on CPE (Group A: 791 ± 124-306 ± 85 mm(3)/year) and ceramic on XLPE (Group B: 1420 ± 223-366 ± 88 mm(3)/year) groups. For those patients who had completed 10 years of followup (20 patients [44.5%] of Group A, 21 [45.7%] of Group B, 23 [47.9%] of Group C, and 22 [44.9%] of Group D), at 10 years, both oxidized zirconium on XLPE groups also showed lower (p < 0.01) volumetric wear (mean ± SD mm(3)) and volumetric wear rates (mean ± SD mm(3)/year) (Group C: 356 ± 64 to 215 ± 54 mm(3)/year, Group D: 354 ± 50 to 210 ± 64 mm(3)/year) when compared with ceramic on CPE (Group A: 895 ± 131 to 380 ± 80 mm(3)/year) and ceramic on XLPE (Group B: 1625 ± 253 to 480 ± 101 mm(3)/year) groups. When wear rates of both oxidized zirconium groups were compared, no differences were found at any time interval with the numbers available. Two hips (one from Group A and one from Group B) are scheduled for revision as a result of wear and osteolysis. There were no differences in hip scores among the groups with the numbers available. In this study, in vivo wear parameters were lower when the combination of an oxidized zirconium head on XLPE liner was used at an average of 9 years (range, 7-12 years) followup. Further larger-scale clinical studies should confirm these findings and evaluate osteolysis and revision rates in association with the use of this bearing coupling. Level II, therapeutic study.

  5. Bioactivity and biocompatibility of hydroxyapatite-based bioceramic coatings on zirconium by plasma electrolytic oxidation.

    PubMed

    Aktuğ, Salim Levent; Durdu, Salih; Yalçın, Emine; Çavuşoğlu, Kültigin; Usta, Metin

    2017-02-01

    In the present work, hydroxyapatite (HAP)-based plasma electrolytic oxide (PEO) coatings were produced on zirconium at different current densities in a solution containing calcium acetate and β-calcium glycerophosphate by a single step. The phase structure, surface morphology, functional groups, thickness and roughness of the coatings were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR), eddy current method and surface profilometer, respectively. The phases of cubic-zirconia, calcium zirconate and HAP were detected by XRD. The amount of HAP and calcium zirconate increased with increasing current density. The surface of the coatings was very porous and rough. Moreover, bioactivity and biocompatibility of the coatings were analyzed in vitro immersion simulated body fluid (SBF) and MTT (3-(4,5-dimethyl thiazol-2yl)-2,5-diphenyl tetrazolium bromide) assay, hemolysis assay and bacterial formation. The apatite-forming ability of the coatings was evaluated after immersion in SBF up to 28days. After immersion, the bioactivity of HAP-based coatings on zirconium was greater than the ones of uncoated zirconium and zirconium oxide-based surface. The bioactivity of PEO surface on zirconium was significantly improved under SBF conditions. The bacterial adhesion of the coatings decreased with increasing current density. The bacterial adhesion of the coating produced at 0.370A/cm 2 was minimum compared to uncoated zirconium coated at 0.260 and 0.292A/cm 2 . The hemocompatibility of HAP-based surfaces was improved by PEO. The cell attachment and proliferation of the PEO coatings were better than the one of uncoated zirconium according to MTT assay results. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Translucency and Strength of High-Translucency Monolithic Zirconium-Oxide Materials

    DTIC Science & Technology

    2016-05-12

    APPROV~, Col Drew W. Fallis Dean, Air Force Postgraduate Dental School r UNIFORMED SERVICES UNIVERSITY OF THE HEALTH SCIENCES AIR FORCE...POSTGRADUATE DENTAL SCHOOL 2450 Pepperrell Street Lackland AFB Texas, 78236-5345 http://www.usuhs.mil "The author hereby certifies that the use of any...Translucency Monolithic Zirconium-Oxide Materials Abstract Dental materials manufacturers have developed more translucent monolithic zirconium oxide

  7. 40 CFR 721.10598 - Lead strontium titanium zirconium oxide.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... 40 Protection of Environment 32 2013-07-01 2013-07-01 false Lead strontium titanium zirconium... Specific Chemical Substances § 721.10598 Lead strontium titanium zirconium oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as lead strontium...

  8. 40 CFR 721.10598 - Lead strontium titanium zirconium oxide.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... 40 Protection of Environment 31 2014-07-01 2014-07-01 false Lead strontium titanium zirconium... Specific Chemical Substances § 721.10598 Lead strontium titanium zirconium oxide. (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substance identified as lead strontium...

  9. Do oxidized zirconium femoral heads reduce polyethylene wear in cemented THAs? A blinded randomized clinical trial.

    PubMed

    Zaoui, Amine; Hage, Samer El; Langlois, Jean; Scemama, Caroline; Courpied, Jean Pierre; Hamadouche, Moussa

    2015-12-01

    Charnley low-friction torque total hip arthroplasty (THA) remains the gold standard in THA. The main cause for failure is wear of the socket. Highly crosslinked polyethylene (HXLPE) has been associated with reduced wear rates. Also, oxidized zirconium has shown in vitro reduced wear rates. However, to our knowledge, there are no data comparing oxidized zirconium femoral heads with metal heads against HXLPE or ultrahigh-molecular-weight polyethylene (UHMWPE) when 22.25-mm bearings were used, which was the same size that performed so well in Charnley-type THAs. We hypothesized that after a minimal 4-year followup (1) use of HXLPE would result in lower radiographic wear than UHMWPE when articulating with a stainless steel head or with an oxidized zirconium head; (2) use of oxidized zirconium would result in lower radiographic wear than stainless steel when articulating with UHMWPE and HXLPE; and (3) there would be no difference in terms of Merle d'Aubigné scores between the bearing couple combinations. One hundred patients were randomized to receive cemented THA with either oxidized zirconium or a stainless steel femoral head. UHMWPE was used in the first 50 patients, whereas HXLPE was used in the next 50 patients. There were 25 patients in each of the four bearing couple combinations. All other parameters were identical in both groups. Complete followup was available in 86 of these patients. Femoral head penetration was measured using a validated computer-assisted method dedicated to all-polyethylene sockets. Clinical results were compared between the groups using the Merle d'Aubigné score. In the UHMWPE series, the median steady-state penetration rate from 1 year onward was 0.03 mm/year (range, 0.003-0.25 mm/year) in the oxidized zirconium group versus 0.11 mm/year (range, 0.03-0.29 mm/year) in the metal group (difference of medians 0.08, p < 0.001). In the HXLPE series, the median steady-state penetration rate from 1 year onward was 0.02 mm/year (range, -0.32 to 0.07 mm/year) in the oxidized zirconium group versus 0.05 mm/year (range, -0.39 to 0.11 mm/year) in the metal group (difference of medians 0.03, p < 0.001). The Merle d'Aubigné scores were no different between the groups with a median of 18 in each of the groups (range, 16-18). This study demonstrated femoral head penetration was reduced by oxidized zirconium when compared with metal on both UHMWPE and HXLPE. However, apart the metal-UHMWE group, all other groups had a steady-state penetration rate well below the osteolysis threshold with a low difference between groups that might not be clinically important at this point. Longer-term followup is needed to warrant whether wear reduction will generate less occurrence of osteolysis and aseptic loosening. Level II, therapeutic study.

  10. Reliability and failure modes of implant-supported zirconium-oxide fixed dental prostheses related to veneering techniques

    PubMed Central

    Baldassarri, Marta; Zhang, Yu; Thompson, Van P.; Rekow, Elizabeth D.; Stappert, Christian F. J.

    2011-01-01

    Summary Objectives To compare fatigue failure modes and reliability of hand-veneered and over-pressed implant-supported three-unit zirconium-oxide fixed-dental-prostheses(FDPs). Methods Sixty-four custom-made zirconium-oxide abutments (n=32/group) and thirty-two zirconium-oxide FDP-frameworks were CAD/CAM manufactured. Frameworks were veneered with hand-built up or over-pressed porcelain (n=16/group). Step-stress-accelerated-life-testing (SSALT) was performed in water applying a distributed contact load at the buccal cusp-pontic-area. Post failure examinations were carried out using optical (polarized-reflected-light) and scanning electron microscopy (SEM) to visualize crack propagation and failure modes. Reliability was compared using cumulative-damage step-stress analysis (Alta-7-Pro, Reliasoft). Results Crack propagation was observed in the veneering porcelain during fatigue. The majority of zirconium-oxide FDPs demonstrated porcelain chipping as the dominant failure mode. Nevertheless, fracture of the zirconium-oxide frameworks was also observed. Over-pressed FDPs failed earlier at a mean failure load of 696 ± 149 N relative to hand-veneered at 882 ± 61 N (profile I). Weibull-stress-number of cycles-unreliability-curves were generated. The reliability (2-sided at 90% confidence bounds) for a 400N load at 100K cycles indicated values of 0.84 (0.98-0.24) for the hand-veneered FDPs and 0.50 (0.82-0.09) for their over-pressed counterparts. Conclusions Both zirconium-oxide FDP systems were resistant under accelerated-life-time-testing. Over-pressed specimens were more susceptible to fatigue loading with earlier veneer chipping. PMID:21557985

  11. 21 CFR 177.2910 - Ultra-filtration membranes.

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ... of a sintered carbon support that is coated with zirconium oxide (CAS Reg. No. 1314-23-4) containing... of an aluminum oxide support that is coated with zirconium oxide (CAS Reg. No. 1314-23-4) containing...

  12. Non-equilibrium oxidation states of zirconium during early stages of metal oxidation

    DOE PAGES

    Ma, Wen; Senanayake, Sanjaya D.; Herbert, F. William; ...

    2015-03-11

    The chemical state of Zr during the initial, self-limiting stage of oxidation on single crystal zirconium (0001), with oxide thickness on the order of 1 nm, was probed by synchrotron x-ray photoelectron spectroscopy. Quantitative analysis of the Zr 3d spectrum by the spectrum reconstruction method demonstrated the formation of Zr 1+, Zr 2+, and Zr 3+ as non-equilibrium oxidation states, in addition to Zr 4+ in the stoichiometric ZrO 2. This finding resolves the long-debated question of whether it is possible to form any valence states between Zr 0 and Zr 4+ at the metal-oxide interface. As a result, themore » presence of local strong electric fields and the minimization of interfacial energy are assessed and demonstrated as mechanisms that can drive the formation of these non-equilibrium valence states of Zr.« less

  13. Introduction of BaSnO3 and BaZrO3 artificial pinning centres into 2G HTS wires based on PLD-GdBCO films. Phase I of the industrial R&D programme at SuperOx

    NASA Astrophysics Data System (ADS)

    Chepikov, V.; Mineev, N.; Degtyarenko, P.; Lee, S.; Petrykin, V.; Ovcharov, A.; Vasiliev, A.; Kaul, A.; Amelichev, V.; Kamenev, A.; Molodyk, A.; Samoilenkov, S.

    2017-12-01

    An industrial R&D programme is ongoing at SuperOx, aimed at improving 2G HTS wire performance in magnetic field. We introduce perovskite artificial pinning centres (APC) into the HTS layer matrix. In contrast to most studies described in the literature, we use the high rate production processing parameters and PLD equipment at SuperOx. This paper reports the results of Phase I of this programme. We fabricated 2G HTS wires by pulsed laser deposition of GdBCO films doped with 6%, 12% and 18% (molar) of BaSnO3 and 6% (molar) of BaZrO3, and compared their performance with an undoped reference sample. The depositions were carried out at production growth rates of 375, 560 and 750 nm min-1 by varying laser pulse frequency. BaZrO3 and BaSnO3 formed columnar semi-coherent nanoinclusions in the GdBCO film matrix. The average transverse size of the nanocolumns was about 5 nm, and their volume density correlated with the dopant concentration. All doped samples exhibited much lower angular anisotropy of in-field critical current and higher lift-factors than the undoped sample. Samples containing 6% BaSnO3 and deposited at the lower growth rates, had higher I c than the undoped sample in the entire temperature range, in a wide range of magnetic field (B//c). The sample containing 6% BaZrO3 had higher I c than the undoped sample at 20 and 4.2 K. These results are an encouraging start of our programme, as they show a positive impact of APC introduced into 2G HTS wires fabricated at production throughput. Phase II work will be focussed on maximising the improvements in specific temperature and field conditions, as well as on the verification of reproducibility of the improvements in production wires.

  14. Effect of europium ion concentration on the structural and photoluminescence properties of novel Li2BaZrO4: Eu3+ nanocrystals

    NASA Astrophysics Data System (ADS)

    Ahemen, I.; Dejene, F. B.; Kroon, R. E.; Swart, H. C.

    2017-12-01

    This work reports the influence of Eu3+ ion concentration on the structure and photoluminescence properties of Li2BaZrO4 nanocrystals including its intrinsic quantum efficiency (IQE). Chemical bath method was employed in the synthesis procedure. X-ray diffraction results showed tetragonal phase for Eu3+ ion concentration in the range 1 and 7 mol% and cubic phase at 8 mol%. The presence of barium oxide (BaO) was confirmed from selected area electron diffraction (SAED). The excitation spectra for these phosphors consisted of broad charge transfer (CT) bands due to the combination of Zr4+ - O2- and Eu3+-O2- charge transfer states. Superimposed on the CT band were direct excitation levels of Eu3+ and Ba2+ ions, in the range 320-450 nm. At high Eu3+ ions concentrations, the intensities of CT bands decreased because some of the ions were coordinated with Ba2+ ions. Photoluminescence emissions for all the doped samples at room temperature appeared to be entirely from intraconfigurational Eu3+ emissions and depended both on the site symmetry as well as the ion concentration. The quadrupole-quadrupole multipolar process was found to be solely responsible for the luminescence quenching. The intensity parameters (Ω2 ,Ω4), asymmetry ratio, R0 and the average decay lifetime of the nanocrystals showed dependence on concentration. High internal quantum efficiency (IQE) values were obtained at low Eu3+ ion concentrations, but efficiency decreased with increasing ion concentration. The CIE coordinates values were comparable to existing red phosphors and in combination with the high IQE make this phosphor a good candidate for red light emitting applications.

  15. The 5-year Results of an Oxidized Zirconium Femoral Component for TKA

    PubMed Central

    Innocenti, Massimo; Carulli, Christian; Matassi, Fabrizio; Villano, Marco

    2009-01-01

    Osteolysis secondary to polyethylene wear is one of the major factors limiting long-term performance of TKA. Oxidized zirconium is a new material that combines the strength of a metal with the wear properties of a ceramic. It remains unknown whether implants with a zirconium femoral component can be used safely in TKA. To answer that question, we reviewed, at a minimum of 5 years, the clinical outcome and survivorship of a ceramic-surfaced oxidized zirconium femoral component implanted during 98 primary TKAs between April 2001 and December 2003. Survivorship was 98.7% at 7 years postoperatively. No revision was necessary and only one component failed because of aseptic loosening. Mean Knee Society score improved from 36 to 89. No adverse events were observed clinically or radiologically. These results justify pursuing the use of oxidized zirconium as an alternative bearing surface for a femoral component in TKA. Level of Evidence: Level IV, therapeutic study. See Guidelines for Authors for a complete description of levels of evidence. PMID:19798541

  16. Bonding of sapphire to sapphire by eutectic mixture of aluminum oxide and zirconium oxide

    NASA Technical Reports Server (NTRS)

    Deluca, J. J. (Inventor)

    1975-01-01

    Bonding of an element comprising sapphire, ruby or blue sapphire to another element of such material with a eutectic mixture of aluminum oxide and zirconium oxide is discussed. The bonding mixture may be applied in the form of a distilled water slurry or by electron beam vapor deposition. In one embodiment the eutectic is formed in situ by applying a layer of zirconium oxide and then heating the assembly to a temperature above the eutectic temperature and below the melting point of the material from which the elements are formed. The formation of a sapphire rubidium maser cell utilizing eutectic bonding is shown.

  17. Weight of Polyethylene Wear Particles is Similar in TKAs with Oxidized Zirconium and Cobalt-chrome Prostheses

    PubMed Central

    Kim, Jun-Shik; Huh, Wansoo; Lee, Kwang-Hoon

    2009-01-01

    Background The greater lubricity and resistance to scratching of oxidized zirconium femoral components are expected to result in less polyethylene wear than cobalt-chrome femoral components. Questions/purposes We examined polyethylene wear particles in synovial fluid and compared the weight, size (equivalent circle diameter), and shape (aspect ratio) of polyethylene wear particles in knees with an oxidized zirconium femoral component with those in knees with a cobalt-chrome femoral component. Patients and Methods One hundred patients received an oxidized zirconium femoral component in one knee and a cobalt-chrome femoral component in the other. There were 73 women and 27 men with a mean age of 55.6 years (range, 44–60 years). The minimum followup was 5 years (mean, 5.5 years; range, 5–6 years). Polyethylene wear particles were analyzed using thermogravimetric methods and scanning electron microscopy. Results The weight of polyethylene wear particles produced at the bearing surface was 0.0223 ± 0.0054 g in 1 g synovial fluid in patients with an oxidized zirconium femoral component and 0.0228 ± 0.0062 g in patients with a cobalt-chrome femoral component. Size and shape of polyethylene wear particles were 0.59 ± 0.05 μm and 1.21 ± 0.24, respectively, in the patients with an oxidized zirconium femoral component and 0.52 ± 0.03 μm and 1.27 ± 0.31, respectively, in the patients with a cobalt-chrome femoral component. Knee Society knee and function scores, radiographic results, and complication rate were similar between the knees with an oxidized zirconium and cobalt-chrome femoral component. Conclusions The weight, size, and shape of polyethylene wear particles were similar in the knees with an oxidized zirconium and a cobalt-chrome femoral component. We found the theoretical advantages of this surface did not provide the actual advantage. Level of Evidence Level I, therapeutic study. See the guidelines for Authors for a complete description of levels of evidence. PMID:19949906

  18. In Situ Enrichment of Phosphopeptides on MALDI Plates Functionalized by Reactive Landing of Zirconium(IV)–n-Propoxide Ions

    PubMed Central

    Blacken, Grady R.; Volný, Michael; Vaisar, Tomáš; Sadílek, Martin; Tureček, František

    2008-01-01

    We report substantial in situ enrichment of phosphopeptides in peptide mixtures using zirconium oxide coated plates for detection by MALDI-TOF mass spectrometry. The novel feature of this approach rests on the specific preparation of zirconium oxide coatings using reactive landing on stainless steel support of gas-phase positive ions produced by electrospray of zirconium(IV)–n-propoxide solutions in 1-propanol. Reactive landing was found to produce durable functionalized surfaces for selective phosphopeptide capture and desorption–ionization by MALDI. Enrichment factors on the order of 20–90 were achieved for several monophosphorylated peptides relative to abundant nonphosphorylated peptides in tryptic digests. We demonstrate the ability of the zirconium oxide functionalized MALDI surfaces to facilitate detection of enriched phosphopeptides in mid-femtomole amounts of α-casein digests per MALDI spot. PMID:17569507

  19. Pyroprocessing of Oxidized Sodium-Bonded Fast Reactor Fuel -- an Experimental Study of Treatment Options for Degraded EBR-II Fuel

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

    S. D. Herrmann; L. A. Wurth; N. J. Gese

    An experimental study was conducted to assess pyrochemical treatment options for degraded EBR-II fuel. As oxidized material, the degraded fuel would need to be converted back to metal to enable electrorefining within an existing electrometallurgical treatment process. A lithium-based electrolytic reduction process was studied to assess the efficacy of converting oxide materials to metal with a particular focus on the impact of zirconium oxide and sodium oxide on this process. Bench-scale electrolytic reduction experiments were performed in LiCl-Li2O at 650 °C with combinations of manganese oxide (used as a surrogate for uranium oxide), zirconium oxide, and sodium oxide. The experimentalmore » study illustrated how zirconium oxide and sodium oxide present different challenges to a lithium-based electrolytic reduction system for conversion of select metal oxides to metal.« less

  20. Oxygen partial pressure influenced structural and optical properties of DC magnetron sputtered ZrO{sub 2} films

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

    Kondaiah, P.; Madhavi, V.; Uthanna, S.

    2013-02-05

    Thin films of zirconium oxide (ZrO{sub 2}) were deposited on (100) p-silicon and quartz substrates by sputtering of metallic zirconium target under different oxygen partial pressures in the range 8 Multiplication-Sign 10{sup -3}-6 Multiplication-Sign 10{sup -2}Pa. The effect of oxygen partial pressure on the structural and optical properties of the deposited films was systematically investigated. The deposition rate of the films decreased from 3.3 to 1.83 nm/min with the increase of oxygen partial pressure from 8 Multiplication-Sign 10{sup -3}-6 Multiplication-Sign 10{sup -2}Pa respectively. The X-ray diffraction profiles revealed that the films exhibit (111) refection of zirconium oxide in monoclinic phase.more » The optical band gap of the films increased from 5.62 to 5.80 eV and refractive index increased from 2.01 to 2.08 with the increase of oxygen partial pressure from 8 Multiplication-Sign 10{sup -3}-6 Multiplication-Sign 10{sup -2}Pa respectively.« less

  1. Phase equilibria, crystal structures, and dielectric anomaly in the BaZrO 3-CaZrO 3 system

    NASA Astrophysics Data System (ADS)

    Levin, Igor; Amos, Tammy G.; Bell, Steven M.; Farber, Leon; Vanderah, Terrell A.; Roth, Robert S.; Toby, Brian H.

    2003-11-01

    Phase equilibria in the (1- x)BaZrO 3- xCaZrO 3 system were analyzed using a combination of X-ray and neutron powder diffraction, and transmission electron microscopy. The proposed phase diagram features two extended two-phase fields containing mixtures of a Ba-rich cubic phase and a tetragonal, or orthorhombic Ca-rich phase, all having perovskite-related structures. The symmetry differences in the Ca-rich phases are caused by different tilting patterns of the [ZrO 6] octahedra. In specimens quenched from 1650°C, CaZrO 3 dissolves only a few percent of Ba, whereas the solubility of Ca in BaZrO 3 is approximately 30 at% . The BaZrO 3-CaZrO 3 system features at least two tilting phase transitions, Pm3 m→ I4/ mcm and I4/ mcm→ Pbnm. Rietveld refinements of the Ba 0.8Ca 0.2ZrO 3 structure using variable-temperature neutron powder diffraction data confirmed that the Pm3 m→ I4/ mcm transition corresponds to a rotation of octahedra about one of the cubic axes; successive octahedra along this axis rotate in opposite directions. In situ variable-temperature electron diffraction studies indicated that the transition temperature increases with increasing Ca-substitution on the A-sites, from approximately -120°C at 5 at% Ca to 225°C at 20 at% Ca. Dielectric measurements revealed that the permittivity increases monotonically from 36 for BaZrO 3 to 53 for Ba 0.9Ca 0.1ZrO 3, and then decreases to 50 for Ba 0.8Ca 0.2ZrO 3. This later specimen was the Ca-richest composition for which pellets could be quenched from the single-phase cubic field with presently available equipment. Strongly non-monotonic behavior was also observed for the temperature coefficient of resonant frequency; however, in this case, the maximum occurred at a lower Ca concentration, 0.05⩽ x⩽0.1. The non-linear behavior of the dielectric properties was attributed to two competing structural effects: a positive effect associated with substitution of relatively small Ca cations on the A-sites, resulting in stretched Ca-O bonds, and a negative effect, related to the distortion of the A-site environment (bond strain relaxation) upon octahedral tilting.

  2. An experimental study of steam explosions involving chemically reactive metal

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

    Cho, D.H.; Armstrong, D.R.; Gunther, W.H.

    1997-07-01

    An experimental study of molten zirconium-water explosions was conducted. A 1-kg mass of zirconium melt was dropped into a column of water. Explosions took place only when an external trigger was used. In the triggered tests, the extent of oxidation of the zirconium melt was very extensive. However, the explosion energetics estimated were found to be very small compared to the potential chemical energy available from the oxidation reaction. Zirconium is of particular interest, since it is a component of the core materials of the current nuclear power reactors. This paper describes the test apparatus and summarizes the results ofmore » four tests conducted using pure zirconium melt.« less

  3. Generating mixed morphology BaZrO3 artificial pinning centers for strong and isotropic pinning in BaZrO3-Y2O3 double-doped YBCO thin films

    NASA Astrophysics Data System (ADS)

    Chen, Shihong; Sebastian, Mary Ann; Gautam, Bibek; Wilt, Jamie; Chen, Yanbin; Sun, Lei; Xing, Zhongwen; Haugan, Timothy; Wu, Judy

    2017-12-01

    High concentration artificial pinning centers (APCs), such as BaZrO3 nanorods (BZO 1D APCs) aligned along the c-axis of the high temperature superconductor YBa2Cu3O7 (YBCO) can provide strong pinning of magnetic vortices and are desirable for applications in high magnetic fields. Unfortunately, in YBCO films with single-doping (SD) of BZO 1D APCs, a monotonic decreasing superconducting T c and critical current density J c(H) with BZO doping has been observed due to strain field overlap at high-concentration perfectly c-axis aligned BZO 1D APCs. In order to resolve this issue, double-doping (DD) of 2-6 vol% BZO 1D APCs and 3.0 vol% Y2O3 nanoparticles (Y2O3-NPs) in YBCO films has been explored to promote BZO-NR orientation misalignment from the c-axis. Remarkably, a monotonic increasing J c(H) with BZO 1D APCs concentration has been obtained in the BZO DD samples. Such a microstructure change is evidenced in the much smaller c-lattice parameter expansion of 0.103% in the DD samples as opposed to 0.511% in the SD counterparts and reduced c-axis alignment of the BZO 1D APCs as revealed in TEM. This yields a mixed 1D + 2D + 3D APC morphology and enhanced isotropic pinning with respect to the orientation of the H-field in the BZO DD samples.

  4. Clinical Outcomes of Zirconium-Oxide Posts: Up-to-Date Systematic Review.

    PubMed

    Al-Thobity, Ahmad M

    2016-06-01

    The aim of this systematic review was to investigate the clinical outcomes of the use of zirconium-oxide posts in the past 20 years. The addressed question was: Do zirconium-oxide posts maintain the long-term survival rate of endodontically treated teeth? A database search was made of articles from January 1995 to December 2014; it included combinations of the following keywords: "zirconia," "zirconium oxide," "dowel/dowels," "post/posts," and "post and core." Exclusion criteria included review articles, experimental studies, case reports, commentaries, and articles published in a language other than English. Articles were reviewed by the titles, followed by the abstracts, and, finally, the full text of the selected studies. Four studies were included after filtering the selected studies according to the inclusion and exclusion criteria. In one study, the prefabricated zirconia posts with indirect glass-ceramic cores had significantly higher failure rates than other posts with direct composite cores. In two studies, no failure of the cemented posts was observed throughout the follow-up period. Due to the limited number of clinical studies, it can be concluded that the long-term success rate of prefabricated zirconium-oxide posts is unclear.

  5. Pyroprocessing of oxidized sodium-bonded fast reactor fuel - An experimental study of treatment options for degraded EBR-II fuel

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

    Hermann, S.D.; Gese, N.J.; Wurth, L.A.

    An experimental study was conducted to assess pyrochemical treatment options for degraded EBR-II fuel. As oxidized material, the degraded fuel would need to be converted back to metal to enable electrorefining within an existing electro-metallurgical treatment process. A lithium-based electrolytic reduction process was studied to assess the efficacy of converting oxide materials to metal with a particular focus on the impact of zirconium oxide and sodium oxide on this process. Bench-scale electrolytic reduction experiments were performed in LiCl-Li{sub 2}O at 650 C. degrees with combinations of manganese oxide (used as a surrogate for uranium oxide), zirconium oxide, and sodium oxide.more » In the absence of zirconium or sodium oxide, the electrolytic reduction of MnO showed nearly complete conversion to metal. The electrolytic reduction of a blend of MnO-ZrO{sub 2} in LiCl - 1 wt% Li{sub 2}O showed substantial reduction of manganese, but only 8.5% of the zirconium was found in the metal phase. The electrolytic reduction of the same blend of MnO-ZrO{sub 2} in LiCl - 1 wt% Li{sub 2}O - 6.2 wt% Na{sub 2}O showed substantial reduction of manganese, but zirconium reduction was even less at 2.4%. This study concluded that ZrO{sub 2} cannot be substantially reduced to metal in an electrolytic reduction system with LiCl - 1 wt% Li{sub 2}O at 650 C. degrees due to the perceived preferential formation of lithium zirconate. This study also identified a possible interference that sodium oxide may have on the same system by introducing a parasitic and cyclic reaction of dissolved sodium metal between oxidation at the anode and reduction at the cathode. When applied to oxidized sodium-bonded EBR-II fuel (e.g., U-10Zr), the prescribed electrolytic reduction system would not be expected to substantially reduce zirconium oxide, and the accumulation of sodium in the electrolyte could interfere with the reduction of uranium oxide, or at least render it less efficient.« less

  6. Low temperature solid oxide electrolytes (LT-SOE): A review

    NASA Astrophysics Data System (ADS)

    Singh, B.; Ghosh, S.; Aich, S.; Roy, B.

    2017-01-01

    Low temperature solid oxide fuel cell (LT-SOFC) can be a source of power for vehicles, online grid, and at the same time reduce system cost, offer high reliability, and fast start-up. A huge amount of research work, as evident from the literature has been conducted for the enhancement of the ionic conductivity of LT electrolytes in the last few years. The basic conduction mechanisms, advantages and disadvantages of different LT oxide ion conducting electrolytes {BIMEVOX systems, bilayer systems including doped cerium oxide/stabilised bismuth oxide and YSZ/DCO}, mixed ion conducting electrolytes {doped cerium oxides/alkali metal carbonate composites}, and proton conducting electrolytes {doped and undoped BaCeO3, BaZrO3, etc.} are discussed here based on the recent research articles. Effect of various material aspects (composition, doping, layer thickness, etc.), fabrication methods (to achieve different microstructures and particle size), design related strategies (interlayer, sintering aid etc.), characterization temperature & environment on the conductivity of the electrolytes and performance of the fuel cells made from these electrolytes are shown in tabular form and discussed. The conductivity of the electrolytes and performance of the corresponding fuel cells are compared. Other applications of the electrolytes are mentioned. A few considerations regarding the future prospects are pointed.

  7. METHOD OF MAKING WIRE FUEL ELEMENTS

    DOEpatents

    Zambrow, J.L.

    1960-08-01

    A method is given for making a nuclear reactor fuel element in the form of a uranium-bearing wire clad with zirconium. A uranium bar is enclosed in a zirconium sheath which is coated with an oxide of magnesium, beryllium, or zirconium. The sheathed bar is then placed in a steel tube and reduced to the desired diameter by swaging at 800 to 900 deg C, after which the steel and oxide are removed.

  8. Solid-state NMR calculations for metal oxides and gallates: Shielding and quadrupolar parameters for perovskites and related phases

    NASA Astrophysics Data System (ADS)

    Middlemiss, Derek S.; Blanc, Frédéric; Pickard, Chris J.; Grey, Clare P.

    2010-05-01

    The NMR parameters obtained from solid-state DFT calculations within the GIPAW approach for 17O- and 69/71Ga-sites in a range of predominantly oxide-based (group II monoxides, SrTiO 3, BaZrO 3, BaSnO 3, BaTiO 3, LaAlO 3, LaGaO 3, SrZrO 3, MgSiO 3 and Ba 2In 2O 5), and gallate (α- and β-Ga 2O 3, LiGaO 2, NaGaO 2, GaPO 4 and LaGaO 3) materials are compared with experimental values, with a view to the future application of a similar approach to doped phases of interest as candidate intermediate temperature solid oxide fuel cell (ITSOFC) electrolytes. Isotropic and anisotropic chemical shift parameters, quadrupolar coupling constants, and associated asymmetries are presented and analyzed. The unusual GaO 5 site occurring in LaGaGe 2O 7 is also fully characterised. In general, it is found that the theoretical results closely track the experimental trends, though some deviations are identified and discussed, particularly in regard to quadrupolar ηQ-values. The high quality of the computed results suggests that this approach can be extended to study more complex and disordered phases.

  9. Corrosion evaluation of zirconium doped oxide coatings on aluminum formed by plasma electrolytic oxidation.

    PubMed

    Bajat, Jelena; Mišković-Stanković, Vesna; Vasilić, Rastko; Stojadinović, Stevan

    2014-01-01

    The plasma electrolytic oxidation (PEO) of aluminum in sodium tungstate (Na(2)WO(4) · (2)H(2)O) and Na(2)WO(4) · (2)H(2)O doped with Zr was analyzed in order to obtain oxide coatings with improved corrosion resistance. The influence of current density in PEO process and anodization time was investigated, as well as the influence of Zr, with the aim to find out how they affect the chemical content, morphology, surface roughness, and corrosion stability of oxide coatings. It was shown that the presence of Zr increases the corrosion stability of oxide coatings for all investigated PEO times. Evolution of EIS spectra during the exposure to 3% NaCl, as a strong corrosive agent, indicated the highest corrosion stability for PEO coating formed on aluminum at 70 mA/cm(2) for 2 min in a zirconium containing electrolyte.

  10. Theoretical Investigation of oxides for batteries and fuel cell applications

    NASA Astrophysics Data System (ADS)

    Ganesh, Panchapakesan; Lubimtsev, Andrew A.; Balachandran, Janakiraman

    I will present theoretical studies of Li-ion and proton-conducting oxides using a combination of theory and computations that involve Density Functional Theory based atomistic modeling, cluster-expansion based studies, global optimization, high-throughput computations and machine learning based investigation of ionic transport in oxide materials. In Li-ion intercalated oxides, we explain the experimentally observed (Nature Materials 12, 518-522 (2013)) 'intercalation pseudocapacitance' phenomenon, and explain why Nb2O5 is special to show this behavior when Li-ions are intercalated (J. Mater. Chem. A, 2013,1, 14951-14956), but not when Na-ions are used. In addition, we explore Li-ion intercalation theoretically in VO2 (B) phase, which is somewhat structurally similar to Nb2O5 and predict an interesting role of site-trapping on the voltage and capacity of the material, validated by ongoing experiments. Computations of proton conducting oxides explain why Y-doped BaZrO3 , one of the fastest proton conducting oxide, shows a decrease in conductivity above 20% Y-doping. Further, using high throughput computations and machine learning tools we discover general principles to improve proton conductivity. Acknowledgements: LDRD at ORNL and CNMS at ORNL

  11. Assessment of wear coefficients of nuclear zirconium claddings without and with pre-oxidation

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

    Qu, Jun; Cooley, Kevin M.; Shaw, Austin H.

    In the cores of pressurized water nuclear reactors, water-flow induced vibration is known to cause claddings on the fuel rods to rub against their supporting grids. Such grid-to-rod-fretting (GTRF) may lead to fretting wear-through and the leakage of radioactive species. The surfaces of actual zirconium alloy claddings in a reactor are inevitably oxidized in the high-temperature pressurized water, and some claddings are even pre-oxidized. As a result, the wear process of the surface oxide film is expected to be quite different from the zirconium alloy substrate. In this paper, we attempt to measure the wear coefficients of zirconium claddings withoutmore » and with pre-oxidation rubbing against grid samples using a bench-scale fretting tribometer. Results suggest that the volumetric wear coefficient of the pre-oxidized cladding is 50 to 200 times lower than that of the untreated cladding. In terms of the linear rate of wear depth, the pre-oxidized alloy wears about 15 times more slowly than the untreated cladding. Finally, fitted with the experimentally-determined wear rates, a stage-wise GTRF engineering wear model demonstrates good agreement with in-reactor experience in predicting the trend of cladding lives.« less

  12. Assessment of wear coefficients of nuclear zirconium claddings without and with pre-oxidation

    DOE PAGES

    Qu, Jun; Cooley, Kevin M.; Shaw, Austin H.; ...

    2016-03-16

    In the cores of pressurized water nuclear reactors, water-flow induced vibration is known to cause claddings on the fuel rods to rub against their supporting grids. Such grid-to-rod-fretting (GTRF) may lead to fretting wear-through and the leakage of radioactive species. The surfaces of actual zirconium alloy claddings in a reactor are inevitably oxidized in the high-temperature pressurized water, and some claddings are even pre-oxidized. As a result, the wear process of the surface oxide film is expected to be quite different from the zirconium alloy substrate. In this paper, we attempt to measure the wear coefficients of zirconium claddings withoutmore » and with pre-oxidation rubbing against grid samples using a bench-scale fretting tribometer. Results suggest that the volumetric wear coefficient of the pre-oxidized cladding is 50 to 200 times lower than that of the untreated cladding. In terms of the linear rate of wear depth, the pre-oxidized alloy wears about 15 times more slowly than the untreated cladding. Finally, fitted with the experimentally-determined wear rates, a stage-wise GTRF engineering wear model demonstrates good agreement with in-reactor experience in predicting the trend of cladding lives.« less

  13. STUDY OF THE OXIDATION OF NON-ALLOYED ZIRCONIUM AND OF OXYGEN DIFFUSION IN THE OXIDE FILM AND IN THE METAL (in French)

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

    Debuigne, J.; Lehr, P.

    1963-12-01

    The oxidation processes of zirconium at 600-850 deg C were studied. A micrographic and radiocrystallographic analysis of the oxide layers formed at the surface of the metal was carried out. The kinetic results, weight gains as function nf time, were completed by the study of oxygen diffusion through the oxide layer formed and in the underlying metal. (auth)

  14. Molybdenum disilicide composites reinforced with zirconia and silicon carbide

    DOEpatents

    Petrovic, John J.

    1995-01-01

    Compositions consisting essentially of molybdenum disilicide, silicon carbide, and a zirconium oxide component. The silicon carbide used in the compositions is in whisker or powder form. The zirconium oxide component is pure zirconia or partially stabilized zirconia or fully stabilized zirconia.

  15. Mid-term survivorship and clinical outcomes of cobalt-chrome and oxidized zirconium on highly crosslinked polyethylene.

    PubMed

    Petis, Stephen M; Vasarhelyi, Edward M; Lanting, Brent A; Howard, James L; Naudie, Douglas D R; Somerville, Lyndsay E; McCalden, Richard W

    2016-02-01

    The choice of bearing articulation for total hip arthroplasty in younger patients is amenable to debate. We compared mid-term patient-reported outcomes and survivorship across 2 different bearing articulations in a young patient cohort. We reviewed patients with cobalt-chrome or oxidized zirconium on highly crosslinked polyethylene who were followed prospectively between 2004 and 2012. Kaplan-Meier analysis was used to determine predicted cumulative survivorship at 5 years with all-cause and aseptic revisions as the outcome. We compared patient-reported outcomes, including the Harris hip score (HHS), Western Ontario and McMaster University Osteoarthritis Index (WOMAC) and Short-form 12 (SF-12) scores. A total of 622 patients were followed during the study period. Mean follow-up was 8.2 (range 2.0-10.6) years for cobalt-chrome and 7.8 (range 2.1-10.7) years for oxidized zirconium. Mean age was 54.9 ± 10.6 years for cobalt-chrome and 54.8 ± 10.7 years for oxidized zirconium. Implant survivorship was 96.0% (95% confidence interval [CI] 94.9%-97.1%) for cobalt-chrome and 98.7% (95% CI 98.0%-99.4%) for oxidized zirconium on highly crosslinked polyethylene for all-cause revisions, and 97.2% (95% CI 96.2%-98.2%) for cobalt-chrome and 99.0% (95% CI 98.4%-99.6%) for oxidized zirconium for aseptic revisions. An age-, sex- and diagnosis-matched comparison of the HHS, WOMAC and SF-12 scores demonstrated no significant changes in clinical outcomes across the groups. Both bearing surface couples demonstrated excellent mid-term survivorship and outcomes in young patient cohorts. Future analyses on wear and costs are warranted to elicit differences between the groups at long-term follow-up.

  16. Molybdenum disilicide composites reinforced with zirconia and silicon carbide

    DOEpatents

    Petrovic, J.J.

    1995-01-17

    Compositions are disclosed consisting essentially of molybdenum disilicide, silicon carbide, and a zirconium oxide component. The silicon carbide used in the compositions is in whisker or powder form. The zirconium oxide component is pure zirconia or partially stabilized zirconia or fully stabilized zirconia.

  17. Thermal NF3 fluorination/oxidation of cobalt, yttrium, zirconium, and selected lanthanide oxides

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

    Scheele, Randall D.; McNamara, Bruce K.; Casella, Andrew M.

    2013-02-01

    This paper presents results of our continuing investigation on the use of nitrogen trifluoride as a fluorination or fluorination/oxidation agent for separating valuable constituents from used nuclear fuels by exploiting the different volatilities of the constituent fission product and actinide fluorides. This article focuses on fission products that do not have volatile fluorides or oxyfluorides at expected operations temperatures. Our thermodynamic calculations show that nitrogen trifluoride has the potential to completely fluorinate fission product oxides to their fluorides. Simultaneous thermogravimetric and differential thermal analyses show that the oxides of cobalt, zirconium, and the lanthanides are fluorinated but do not formmore » volatile fluorides when treated with nitrogen trifluoride at temperatures up to 550°C. Our studies of gadolinium-doped commercial nuclear fuel indicate that nitrogen trifluoride can extract uranium from the non-volatile gadolinium.« less

  18. Development of phase analysis methods of impurity elements in alloys based on iron and nickel

    NASA Astrophysics Data System (ADS)

    Andreeva, N. A.; Anuchkin, S. N.; Volchenkova, V. A.; Kazenas, E. K.; Penkina, T. N.; Fomina, A. A.

    2018-04-01

    Using the method of AES with ICP, new methods have been developed for quantifying the content of various forms of existence of impurity elements: Al-Al2O3; Zr-ZrO2 in alloys based on iron (Fe-Sn) and nickel (Ni-Sn). Open systems were used to dissolve Al and Zr. To translate difficult-to-open aluminum oxides (corundum) and zirconium oxide (baddeleyite) into the solution, accelerated techniques were developed using the microwave system Mars 5. To confirm the completeness of the dissolution of oxides, a classical scheme of alloy fusion with alkali metal salts was used. Optimal analytical parameters for determining the elements: Al and Zr were chosen. The influence of matrix elements (iron and nickel) and methods of its elimination were studied. This made it possible to determine the elements in a wide concentration range from 1 • 10-3 to n% Al and from 1 • 10-4 to n% Zr without preliminary separation of the matrix with good metrological characteristics. The relative standard deviation (Sr) does not exceed 0,2. The separate determination of the contents of aluminum and aluminium oxide in the model melt of Fe-Sn-Al2O3 and zirconium and zirconium oxide in the Ni-Sn-ZrO2 model melt allowed us to estimate the number of nanoparticles participating in the heterophase interaction with tin and retired to the interface in the form of ensembles and the number of nanoparticles present in the melt and affecting the crystallization process and the structure of the metal.

  19. Nanostructure multilayer dielectric materials for capacitors and insulators

    DOEpatents

    Barbee, Jr., Troy W.; Johnson, Gary W.

    1998-04-21

    A capacitor is formed of at least two metal conductors having a multilayer dielectric and opposite dielectric-conductor interface layers in between. The multilayer dielectric includes many alternating layers of amorphous zirconium oxide (ZrO.sub.2) and alumina (Al.sub.2 O.sub.3). The dielectric-conductor interface layers are engineered for increased voltage breakdown and extended service life. The local interfacial work function is increased to reduce charge injection and thus increase breakdown voltage. Proper material choices can prevent electrochemical reactions and diffusion between the conductor and dielectric. Physical vapor deposition is used to deposit the zirconium oxide (ZrO.sub.2) and alumina (Al.sub.2 O.sub.3) in alternating layers to form a nano-laminate.

  20. Nanostructure multilayer dielectric materials for capacitors and insulators

    DOEpatents

    Barbee, T.W. Jr.; Johnson, G.W.

    1998-04-21

    A capacitor is formed of at least two metal conductors having a multilayer dielectric and opposite dielectric-conductor interface layers in between. The multilayer dielectric includes many alternating layers of amorphous zirconium oxide (ZrO{sub 2}) and alumina (Al{sub 2}O{sub 3}). The dielectric-conductor interface layers are engineered for increased voltage breakdown and extended service life. The local interfacial work function is increased to reduce charge injection and thus increase breakdown voltage. Proper material choices can prevent electrochemical reactions and diffusion between the conductor and dielectric. Physical vapor deposition is used to deposit the zirconium oxide (ZrO{sub 2}) and alumina (Al{sub 2}O{sub 3}) in alternating layers to form a nano-laminate. 1 fig.

  1. Controlling BaZrO3 nanostructure orientation in YBa2Cu3O{}_{7-\\delta } films for a three-dimensional pinning landscape

    NASA Astrophysics Data System (ADS)

    Wu, J. Z.; Shi, J. J.; Baca, F. J.; Emergo, R.; Wilt, J.; Haugan, T. J.

    2015-12-01

    The orientation phase diagram of self-assembled BaZrO3 (BZO) nanostructures in c-oriented YBa2Cu3O{}7-δ (YBCO) films on flat and vicinal SrTiO3 substrates was studied experimentally with different dopant concentrations and vicinal angles and theoretically using a micromechanical model based on the theory of elasticity. The organized BZO nanostructure configuration was found to be tunable, between c-axis to ab-plane alignment, by the dopant concentration in the YBCO film matrix strained via lattice mismatched substrates. The correlation between the local strain caused by the BZO doping and the global strain on the matrix provides a unique approach for controllable growth of dopant nanostructure landscapes. In particular, a mixed phase of the c-axis-aligned nanorods and the ab-plane-aligned planar nanostructures can be obtained, leading to a three-dimensional pinning landscape with single impurity doping and much improved J c in almost all directions of applied magnetic field.

  2. Method to predict relative hydriding within a group of zirconium alloys under nuclear irradiation

    DOEpatents

    Johnson, Jr., A. Burtron; Levy, Ira S.; Trimble, Dennis J.; Lanning, Donald D.; Gerber, Franna S.

    1990-01-01

    An out-of-reactor method for screening to predict relative in-reactor hydriding behavior of zirconium-bsed materials is disclosed. Samples of zirconium-based materials having different composition and/or fabrication are autoclaved in a relatively concentrated (0.3 to 1.0M) aqueous lithium hydroxide solution at constant temperatures within the water reactor coolant temperature range (280.degree. to 316.degree. C.). Samples tested by this out-of-reactor procedure, when compared on the basis of the ratio of hydrogen weight gain to oxide weight gain, accurately predict the relative rate of hyriding for the same materials when subject to in-reactor (irradiated) corrision.

  3. Influence of frequency on the structure of zirconium oxide coatings deposited from aqueous electrolytes under microplasma oxidation

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

    Gubaidulina, Tatiana A., E-mail: goub2002@mail.ru; Sergeev, Viktor P., E-mail: vserg@mail.tomsknet.ru; Fedorischeva, Marina V., E-mail: fmw@ispms.tsc.ru

    2015-10-27

    The work describes the microplasma oxidation (MPO) of zirconium surface resulting in the formation of zirconium oxide Zr-Al-Nb-O. We have used novel power supply to deposit oxide ceramic coatings by MPO and studied the effect of current density on the phase structure of oxide ceramic coatings. The size of microcracks in the coatings was determined at different frequencies. We have also used EVO50c scanning election microscope with an attachment for elemental analysis to study the morphology and elemental composition of oxide ceramic coating. In addition, we have established the influence of the frequency on the phase composition of the coating:more » at the frequency of 2500 Hz, the fraction of monoclinic phase was 18%, while the fraction of tetragonal phase amounted to 72%. The oxide ceramic coating produced at 250 Hz contained 38% of monoclinic phase and 62% of tetragonal phase; in addition, it had no buildups and craters.« less

  4. Temperature-mediated phase transformation, pore geometry and pore hysteresis transformation of borohydride derived in-born porous zirconium hydroxide nanopowders

    PubMed Central

    Nayak, Nadiya B.; Nayak, Bibhuti B.

    2016-01-01

    Development of in-born porous nature of zirconium hydroxide nanopowders through a facile hydrogen (H2) gas-bubbles assisted borohydride synthesis route using sodium borohydride (NaBH4) and novel information on the temperature-mediated phase transformation, pore geometry as well as pore hysteresis transformation of in-born porous zirconium hydroxide nanopowders with the help of X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) isotherm and Transmission Electron Microscopy (TEM) images are the main theme of this research work. Without any surfactants or pore forming agents, the borohydride derived amorphous nature of porous powders was stable up to 500 °C and then the seed crystals start to develop within the loose amorphous matrix and trapping the inter-particulate voids, which led to develop the porous nature of tetragonal zirconium oxide at 600 °C and further sustain this porous nature as well as tetragonal phase of zirconium oxide up to 800 °C. The novel hydrogen (H2) gas-bubbles assisted borohydride synthesis route led to develop thermally stable porous zirconium hydroxide/oxide nanopowders with an adequate pore size, pore volume, and surface area and thus these porous materials are further suggested for promising use in different areas of applications. PMID:27198738

  5. The origin of 2.7 eV blue luminescence band in zirconium oxide

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

    Perevalov, T. V., E-mail: timson@isp.nsc.ru; Zhuravlev, K. S.; Gritsenko, V. A.

    2014-12-28

    The luminescence spectra of non-stoichiometric zirconium oxide film series with different oxygen vacancies' concentrations show the blue photoluminescence band centered near a 2.7 eV peak. There is a broad band at 5.2 eV in the luminescence excitation spectrum for blue emission. The ab-initio quantum-chemical calculation gives a peak in the optical absorption at 5.1 eV for the oxygen vacancy in cubic ZrO{sub 2}. It was concluded that the 2.7 eV blue luminescence excited near 5.2 eV in a zirconium oxide film is associated with the oxygen vacancy.

  6. PROCESS OF DISSOLVING ZIRCONIUM ALLOYS

    DOEpatents

    Shor, R.S.; Vogler, S.

    1958-01-21

    A process is described for dissolving binary zirconium-uranium alloys where the uranium content is about 2%. In prior dissolution procedures for these alloys, an oxidizing agent was added to prevent the precipitation of uranium tetrafluoride. In the present method complete dissolution is accomplished without the use of the oxidizing agent by using only the stoichiometric amount or slight excess of HF required by the zirconium. The concentration of the acid may range from 2M to 10M and the dissolution is advatageously carried out at a temperature of 80 deg C.

  7. Method for preparing dielectric composite materials

    DOEpatents

    Lauf, Robert J.; Anderson, Kimberly K.; Montgomery, Frederick C.; Collins, Jack L.; Felten, John J.

    2004-11-23

    The invention allows the fabrication of small, dense beads of dielectric materials with selected compositions, which are incorporated into a polymeric matrix for use in capacitors, filters, and the like. A porous, generally spherical bead of hydrous metal oxide containing titanium or zirconium is made by a sol-gel process to form a substantially rigid bead having a generally fine crystallite size and correspondingly finely distributed internal porosity. The resulting gel bead may be washed and hydrothermally reacted with a soluble alkaline earth salt (typically Ba or Sr) at elevated temperature and pressure to convert the bead into a mixed hydrous titanium- or zirconium-alkaline earth oxide while retaining the generally spherical shape. Alternatively, the gel bead may be made by coprecipitation. This mixed oxide bead is then washed, dried and calcined to produce the desired (BaTiO.sub.3, PbTiO.sub.3, SrZrO.sub.3) structure. The sintered beads are incorporated into a selected polymer matrix. The resulting dielectric composite material may be electrically "poled" if desired.

  8. Dielectric composite materials and method for preparing

    DOEpatents

    Lauf, Robert J.; Anderson, Kimberly K.; Montgomery, Frederick C.; Collins, Jack L.; Felten, John J.

    2003-07-29

    The invention allows the fabrication of small, dense beads of dielectric materials with selected compositions, which are incorporated into a polymeric matrix for use in capacitors, filters, and the like. A porous, generally spherical bead of hydrous metal oxide containing titanium or zirconium is made by a sol-gel process to form a substantially rigid bead having a generally fine crystallite size and correspondingly finely distributed internal porosity. The resulting gel bead may be washed and hydrothermally reacted with a soluble alkaline earth salt (typically Ba or Sr) at elevated temperature and pressure to convert the bead into a mixed hydrous titanium- or zirconium-alkaline earth oxide while retaining the generally spherical shape. Alternatively, the gel bead may be made by coprecipitation. This mixed oxide bead is then washed, dried and calcined to produce the desired (BaTiO.sub.3, PbTiO.sub.3, SrZrO.sub.3) structure. The sintered beads are incorporated into a selected polymer matrix. The resulting dielectric composite material may be electrically "poled" if desired.

  9. Solid-state NMR calculations for metal oxides and gallates: shielding and quadrupolar parameters for perovskites and related phases.

    PubMed

    Middlemiss, Derek S; Blanc, Frédéric; Pickard, Chris J; Grey, Clare P

    2010-05-01

    The NMR parameters obtained from solid-state DFT calculations within the GIPAW approach for (17)O- and (69/71)Ga-sites in a range of predominantly oxide-based (group II monoxides, SrTiO(3), BaZrO(3), BaSnO(3), BaTiO(3), LaAlO(3), LaGaO(3), SrZrO(3), MgSiO(3) and Ba(2)In(2)O(5)), and gallate (alpha- and beta-Ga(2)O(3), LiGaO(2), NaGaO(2), GaPO(4) and LaGaO(3)) materials are compared with experimental values, with a view to the future application of a similar approach to doped phases of interest as candidate intermediate temperature solid oxide fuel cell (ITSOFC) electrolytes. Isotropic and anisotropic chemical shift parameters, quadrupolar coupling constants, and associated asymmetries are presented and analyzed. The unusual GaO(5) site occurring in LaGaGe(2)O(7) is also fully characterised. In general, it is found that the theoretical results closely track the experimental trends, though some deviations are identified and discussed, particularly in regard to quadrupolar eta(Q)-values. The high quality of the computed results suggests that this approach can be extended to study more complex and disordered phases. Copyright 2010 Elsevier Inc. All rights reserved.

  10. Oven rack having integral lubricious, dry porcelain surface

    DOEpatents

    Ambrose, Jeffrey A; Mackiewicz-Ludtka, Gail; Sikka, Vinod K; Qu, Jun

    2014-06-03

    A lubricious glass-coated metal cooking article capable of withstanding repeated heating and cooling between room temperature and at least 500.degree. F. without chipping or cracking the glass coating, wherein the glass coating includes about 0.1 to about 20% by weight of a homogeneously distributed dry refractory lubricant material having a particle size less than about 200 .mu.m. The lubricant material is selected from the group consisting of carbon; graphite; boron nitride; cubic boron nitride; molybdenum (FV) sulfide; molybdenum sulfide; molybdenum (IV) selenide; molybdenum selenide, tungsten (IV) sulfide; tungsten disulfide; tungsten sulfide; silicon nitride (Si.sub.3N.sub.4); TiN; TiC; TiCN; TiO.sub.2; TiAlN; CrN; SiC; diamond-like carbon; tungsten carbide (WC); zirconium oxide (ZrO.sub.2); zirconium oxide and 0.1 to 40 weight % aluminum oxide; alumina-zirconia; antimony; antimony oxide; antimony trioxide; and mixtures thereof.

  11. Amperometric Biosensor Based on Zirconium Oxide/Polyethylene Glycol/Tyrosinase Composite Film for the Detection of Phenolic Compounds.

    PubMed

    Ahmad, Nor Monica; Abdullah, Jaafar; Yusof, Nor Azah; Ab Rashid, Ahmad Hazri; Abd Rahman, Samsulida; Hasan, Md Rakibul

    2016-06-29

    A phenolic biosensor based on a zirconium oxide/polyethylene glycol/tyrosinase composite film for the detection of phenolic compounds has been explored. The formation of the composite film was expected via electrostatic interaction between hexacetyltrimethylammonium bromide (CTAB), polyethylene glycol (PEG), and zirconium oxide nanoparticles casted on screen printed carbon electrode (SPCE). Herein, the electrode was treated by casting hexacetyltrimethylammonium bromide on SPCE to promote a positively charged surface. Later, zirconium oxide was mixed with polyethylene glycol and the mixture was dropped cast onto the positively charged SPCE/CTAB. Tyrosinase was further immobilized onto the modified SPCE. Characterization of the prepared nanocomposite film and the modified SPCE surface was investigated by scanning electron microscopy (SEM), Electrochemical Impedance Spectroscopy (EIS), and Cyclic voltamogram (CV). The developed biosensor exhibits rapid response for less than 10 s. Two linear calibration curves towards phenol in the concentrations ranges of 0.075-10 µM and 10-55 µM with the detection limit of 0.034 µM were obtained. The biosensor shows high sensitivity and good storage stability for at least 30 days.

  12. Mid-term survivorship and clinical outcomes of cobalt-chrome and oxidized zirconium on highly crosslinked polyethylene

    PubMed Central

    Petis, Stephen M.; Vasarhelyi, Edward M.; Lanting, Brent A.; Howard, James L.; Naudie, Douglas D.R.; Somerville, Lyndsay E.; McCalden, Richard W.

    2016-01-01

    Background The choice of bearing articulation for total hip arthroplasty in younger patients is amenable to debate. We compared mid-term patient-reported outcomes and survivorship across 2 different bearing articulations in a young patient cohort. Methods We reviewed patients with cobalt-chrome or oxidized zirconium on highly crosslinked polyethylene who were followed prospectively between 2004 and 2012. Kaplan–Meier analysis was used to determine predicted cumulative survivorship at 5 years with all-cause and aseptic revisions as the outcome. We compared patient-reported outcomes, including the Harris hip score (HHS), Western Ontario and McMaster University Osteoarthritis Index (WOMAC) and Short-form 12 (SF-12) scores. Results A total of 622 patients were followed during the study period. Mean follow-up was 8.2 (range 2.0–10.6) years for cobalt-chrome and 7.8 (range 2.1–10.7) years for oxidized zirconium. Mean age was 54.9 ± 10.6 years for cobalt-chrome and 54.8 ± 10.7 years for oxidized zirconium. Implant survivorship was 96.0% (95% confidence interval [CI] 94.9%–97.1%) for cobalt-chrome and 98.7% (95% CI 98.0%–99.4%) for oxidized zirconium on highly crosslinked polyethylene for all-cause revisions, and 97.2% (95% CI 96.2%–98.2%) for cobalt-chrome and 99.0% (95% CI 98.4%–99.6%) for oxidized zirconium for aseptic revisions. An age-, sex- and diagnosis-matched comparison of the HHS, WOMAC and SF-12 scores demonstrated no significant changes in clinical outcomes across the groups. Conclusion Both bearing surface couples demonstrated excellent mid-term survivorship and outcomes in young patient cohorts. Future analyses on wear and costs are warranted to elicit differences between the groups at long-term follow-up. PMID:26812409

  13. Method to predict relative hydriding within a group of zirconium alloys under nuclear irradiation

    DOEpatents

    Johnson, A.B. Jr.; Levy, I.S.; Trimble, D.J.; Lanning, D.D.; Gerber, F.S.

    1990-04-10

    An out-of-reactor method for screening to predict relative in-reactor hydriding behavior of zirconium-based materials is disclosed. Samples of zirconium-based materials having different compositions and/or fabrication methods are autoclaved in a relatively concentrated (0.3 to 1.0M) aqueous lithium hydroxide solution at constant temperatures within the water reactor coolant temperature range (280 to 316 C). Samples tested by this out-of-reactor procedure, when compared on the basis of the ratio of hydrogen weight gain to oxide weight gain, accurately predict the relative rate of hydriding for the same materials when subject to in-reactor (irradiated) corrosion. 1 figure.

  14. Zirconium carbide as an electrocatalyst for the chromous-chromic redox couple

    NASA Technical Reports Server (NTRS)

    Gahn, R. F.; Reid, M. A.; Yang, C. Y. (Inventor)

    1981-01-01

    Zirconium carbide is used as a catalyst in a REDOX cell for the oxidation of chromous ions to chromic ions and for the reduction of chromic ions to chromous ions. The zirconium carbide is coated on an inert electronically conductive electrode which is present in the anode fluid of the cell.

  15. Digital data acquisition for a CAD/CAM-fabricated titanium framework and zirconium oxide restorations for an implant-supported fixed complete dental prosthesis.

    PubMed

    Lin, Wei-Shao; Metz, Michael J; Pollini, Adrien; Ntounis, Athanasios; Morton, Dean

    2014-12-01

    This dental technique report describes a digital workflow with digital data acquisition at the implant level, computer-aided design and computer-aided manufacturing fabricated, tissue-colored, anodized titanium framework, individually luted zirconium oxide restorations, and autopolymerizing injection-molded acrylic resin to fabricate an implant-supported, metal-ceramic-resin fixed complete dental prosthesis in an edentulous mandible. The 1-step computer-aided design and computer-aided manufacturing fabrication of titanium framework and zirconium oxide restorations can provide a cost-effective alternative to the conventional metal-resin fixed complete dental prosthesis. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  16. Mesoporous zirconium titanium oxides. Part 2: Synthesis, porosity, and adsorption properties of beads.

    PubMed

    Sizgek, G Devlet; Sizgek, Erden; Griffith, Christopher S; Luca, Vittorio

    2008-11-04

    Mesoporous zirconium titanium mixed-oxide beads having disordered wormhole textures and mole fractions of Zr (x) ranging from x=0.25 to 0.67 have been prepared. The bead preparation method combined the forced hydrolysis of mixtures of zirconium-titanium alkoxides in the presence of long-chain carboxylates with external gelation. Uniformly sized beads could be produced in the size range 0.5-1.1 mm by varying the droplet size and viscosity of the mixed-oxide sol, thus making them suitable for large-scale column chromatographic applications. The beads exhibited narrow pore size distributions with similar mean pore diameters of around 3.7 nm. The specific surface areas of the beads were linked to the Zr mole fraction in the precursor solution and were generally greater than 350 m2/g for x=0.5. A combination of scanning transmission electron microscopy and X-ray absorption fine structure analysis indicated that the pore walls of the beads were composed of atomically dispersed Zr and Ti to form a continuous network of Zr-O-Ti bonds. Mass transport in the beads was evaluated by monitoring the kinetics of vanadate and vanadyl adsorption at pH 10.5 and 0.87, respectively.

  17. Ion Implantation-Modified Fluorine-Doped Tin Oxide by Zirconium with Continuously Tunable Work Function and Its Application in Perovskite Solar Cells.

    PubMed

    Han, Dong; Wu, Cuncun; Zhao, Yunbiao; Chen, Yi; Xiao, Lixin; Zhao, Ziqiang

    2017-12-06

    In recent years, perovskite solar cells have drawn a widespread attention. As an electrode material, fluorine-doped tin oxide (FTO) is widely used in various kinds of solar cells. However, the relatively low work function (WF) (∼4.6 eV) limits its application. The potential barrier between the transparent conductive oxide electrode and the hole transport layer (HTL) in inverted perovskite solar cells results in a decrease in device performance. In this paper, we propose a method to adjust WF of FTO by implanting zirconium ions into the FTO surface. The WF of FTO can be precisely and continuously tuned between 4.59 and 5.55 eV through different dopant concentration of zirconium. In the meantime, the modified FTO, which had a WF of 5.1 eV to match well the highest occupied molecular orbital energy level of poly(3,4-ethylenedioxylenethiophene):polystyrene sulfonate, was used as the HTL in inverted planar perovskite solar cells. Compared with the pristine FTO electrode-based device, the open circuit voltage increased from 0.82 to 0.91 V, and the power conversion efficiency increased from 11.6 to 14.0%.

  18. Zirconium Phosphate Supported MOF Nanoplatelets.

    PubMed

    Kan, Yuwei; Clearfield, Abraham

    2016-06-06

    We report a rare example of the preparation of HKUST-1 metal-organic framework nanoplatelets through a step-by-step seeding procedure. Sodium ion exchanged zirconium phosphate, NaZrP, nanoplatelets were judiciously selected as support for layer-by-layer (LBL) assembly of Cu(II) and benzene-1,3,5-tricarboxylic acid (H3BTC) linkers. The first layer of Cu(II) is attached to the surface of zirconium phosphate through covalent interaction. The successive LBL growth of HKUST-1 film is then realized by soaking the NaZrP nanoplatelets in ethanolic solutions of cupric acetate and H3BTC, respectively. The amount of assembled HKUST-1 can be readily controlled by varying the number of growth cycles, which was characterized by powder X-ray diffraction and gas adsorption analyses. The successful construction of HKUST-1 on NaZrP was also supported by its catalytic performance for the oxidation of cyclohexene.

  19. Controlling Reaction Selectivity through the Surface Termination of Perovskite Catalysts

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

    Polo-Garzon, Felipe; Yang, Shi-Ze; Fung, Victor

    2017-07-19

    Although perovskites have been widely used in catalysis, tuning their surface terminations to control reaction selectivities has not been well established. In this work, we employ multiple surface sensitive techniques to characterize the surface termination (one aspect of surface reconstruction) of SrTiO 3 (STO) after thermal pretreatment (Sr-enrichment) and chemical etching (Ti-enrichment). We show, using the conversion of 2-propanol as a probe reaction, that the surface termination of STO can be controlled to greatly tune catalytic acid/base properties and consequently the reaction selectivities in a wide range, which are inaccessible using single metal oxides, either SrO or TiO 2. Densitymore » functional theory (DFT) calculations well explain the selectivity tuning and reaction mechanism on different surface terminations of STO. Similar catalytic tunability is also observed on BaZrO 3, highlighting the generality of the finding from this work.« less

  20. Controlling Reaction Selectivity through the Surface Termination of Perovskite Catalysts

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

    Polo-Garzon, Felipe; Yang, Shi-Ze; Fung, Victor

    2017-07-19

    Although well known in the material science field, surface reconstruction of perovskites has not been implemented in heterogeneous catalysis. In this work, we employ multiple surface sensitive techniques to characterize the surface reconstruction of SrTiO3 (STO) after thermal pretreatment (Sr-enrichment) and chemical etching (Ti-enrichment). We show, using the conversion of 2-propanol as a probe reaction, that the surface reconstruction of STO can be controlled to greatly tune catalytic acid/base properties and consequently the reaction selectivities in a wide range, which are inaccessible using single metal oxides, either SrO or TiO2. Density functional theory (DFT) calculations well explain the selectivity tuningmore » and reaction mechanism on differently reconstructed surfaces of STO. Similar catalytic tunability is also observed on BaZrO3, highlighting the generality of the finding from this work.« less

  1. Lu2O3-SiO2-ZrO2 Coatings for Environmental Barrier Application by Solution Precursor Plasma Spraying and Influence of Precursor Chemistry

    NASA Astrophysics Data System (ADS)

    Darthout, Émilien; Quet, Aurélie; Braidy, Nadi; Gitzhofer, François

    2014-02-01

    As environmental barrier coatings are subjected to thermal stress in gas turbine engines, the introduction of a secondary phase as zircon (ZrSiO4) is likely to increase the stress resistance of Lu2Si2O7 coatings generated by induction plasma spraying using liquid precursors. In a first step, precursor chemistry effect is investigated by the synthesis of ZrO2-SiO2 nanopowders by induction plasma nanopowder synthesis technique. Tetraethyl orthosilicate (TEOS) as silicon precursor and zirconium oxynitrate and zirconium ethoxide as zirconium precursors are mixed in ethanol and produce a mixture of tetragonal zirconia and amorphous silica nanoparticles. The use of zirconium ethoxide precursor results in zirconia particles with diameter below 50 nm because of exothermic thermal decomposition of the ethoxide and its high boiling point with respect to solvent, while larger particles are formed when zirconium oxynitrate is employed. The formation temperature of zircon from zirconia and silica oxides is found at 1425 °C. Second, coatings are synthesized in Lu2O3-ZrO2-SiO2 system. After heat treatment, the doping effect of lutetium on zirconia grains totally inhibits the zircon formation. Dense coatings are obtained with the use of zirconium ethoxide because denser particles with a homogeneous diameter distribution constitute the coating.

  2. Retention of zirconium oxide ceramic crowns with three types of cement.

    PubMed

    Palacios, Rosario P; Johnson, Glen H; Phillips, Keith M; Raigrodski, Ariel J

    2006-08-01

    Information about the retentive strength of luting agents for zirconium oxide-based crowns is limited. It is unknown if this type of high-strength ceramic restoration requires adhesive cementation to enhance retention. The purpose of this in vitro study was to determine the ability of selected luting agents to retain a representative zirconium oxide ceramic crown under clinically simulated conditions. Recently extracted human molars were prepared with a flat occlusal surface, 20-degree taper, and approximately 4-mm axial length. The axial and occlusal surface areas were determined, and specimens were distributed equally by total surface area into 3 cementation groups (n=12). Zirconium oxide ceramic copings (Procera AllZirkon) with an occlusal bar to facilitate removal were fabricated using computer-aided design/computer-assisted manufacturing (CAD/CAM) technology. All copings were airborne-particle abraded with 50-mum Al(2)O(3) and then cleaned in an ultrasonic bath with isopropyl alcohol. Provisional cement was removed from the prepared teeth, followed by a pumice prophy. After trial insertion, the copings were cleaned with phosphoric acid, rinsed, dried, and dehydrated with isopropyl alcohol. They were then cemented with a seating force of 10 kg per tooth, using either a composite resin cement with adhesive agent (Panavia F 2.0 and ED Primer A & B [PAN]), a resin-modified glass ionomer cement (Rely X Luting [RXL]), or a self-adhesive modified composite resin (Rely X Unicem [RXU]). The cemented copings were thermal cycled at 5 degrees C and 55 degrees C for 5000 cycles with a 15 second dwell time, and then removed along the path of insertion using a universal testing machine at 0.5 mm/min. The removal force was recorded, and the stress of dislodgement was calculated using the surface area of each preparation. A 1-way analysis of variance was used to analyze the data (alpha=.05). The nature of failure was also recorded. Mean dislodgement stresses were 5.1, 6.1, and 5.0 MPa for PAN, RXL, and RXU, respectively. The 1-way analysis of variance revealed no differences in mean crown removal stress among the 3 cementation groups. The predominant mode of failure was cement remaining principally on the zirconium oxide copings in 46% of the specimens, followed by cement found on the tooth in 25.7% of the specimens. Within the limitations of this study, the 3 luting agents, with mean removal stresses ranging from 5.0 to 6.1 MPa were not significantly different. The use of a composite resin cement with a bonding agent did not yield higher coping retention compared to the other 2 cements tested.

  3. Synthesis of 0.1% & 0.2% neodymium doped barium zirconium titanate (BaZr{sub 0.2}Ti{sub 0.8}O{sub 3}) and study of their dielectric behaviour

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

    Kumar, Anil, E-mail: anilkantikumar@rediffmail.com; Kumar, Vipin; Gupta, Merry

    2015-08-28

    Efforts have been made to ease process of producing widely used multilayered ceramics of Barium Zirconium Titanium Oxides and study their dielectric behaviour and structural properties. For this purpose, adequate proportions of Barium Carbonate, Zirconium Oxide and Titanium Oxide were taken and hand milled for 2 hours. Neodymium composition of the order of 0.1% and 0.2% was used for doping to weight percentage of BaZr0.2Ti0.8O3. The samples were authenticated using raw data obtained from Bruker AXS D8 advance Copper KL alpha source XRD equipment. Further, the samples were studied for their phase transition, composition, single phase perovskite structure using XRDmore » technique. The technique has also been applied to know formation of stable homogeneous solid solution from XRD parameters. The other physical parameters like the morphology, micro structural information, crystal arrangements and topography have also been observed through SEM. The SEM has revealed information related to grain size development and composition of sample with fine agglomerates. For complete study of the compounds the atomic and weight composition has also been examined by Electron Dispersive Spectroscopy patterns. The comparison has been made with other works on ceramics at various frequencies and has yielded very interesting results.« less

  4. Physical characterization of a new composition of oxidized zirconium-2.5 wt% niobium produced using a two step process for biomedical applications

    NASA Astrophysics Data System (ADS)

    Pawar, V.; Weaver, C.; Jani, S.

    2011-05-01

    Zirconium and particularly Zr-2.5 wt%Nb (Zr2.5Nb) alloy are useful for engineering bearing applications because they can be oxidized in air to form a hard surface ceramic. Oxidized zirconium (OxZr) due to its abrasion resistant ceramic surface and biocompatible substrate alloy has been used as a bearing surface in total joint arthroplasty for several years. OxZr is characterized by hard zirconium oxide (oxide) formed on Zr2.5Nb using one step thermal oxidation carried out in air. Because the oxide is only at the surface, the bulk material behaves like a metal, with high toughness. The oxide, furthermore, exhibits high adhesion to the substrate because of an oxygen-rich diffusion hardened zone (DHZ) interposing between the oxide and the substrate. In this study, we demonstrate a two step process that forms a thicker DHZ and thus increased depth of hardening than that can be obtained using a one step oxidation process. The first step is thermal oxidation in air and the second step is a heat treatment in vacuum. The second step drives oxygen from the oxide formed in the first step deeper into the substrate to form a thicker DHZ. During the process only a portion of the oxide is dissolved. This new composition (DHOxZr) has approximately 4-6 μm oxide similar to that of OxZr. The nano-hardness of the oxide is similar but the DHZ is approximately 10 times thicker. The stoichiometry of the oxide is similar and a secondary phase rich in oxygen is present through the entire thickness. Due to the increased depth of hardening, the critical load required for the onset of oxide cracking is approximately 1.6 times more than that of the oxide of OxZr. This new composition has a potential to be used as a bearing surface in applications where greater depth of hardening is required.

  5. Effect of anodization on the surface characteristics and electrochemical behaviour of zirconium in artificial saliva.

    PubMed

    Romonti, Daniela E; Gomez Sanchez, Andrea V; Milošev, Ingrid; Demetrescu, Ioana; Ceré, Silvia

    2016-05-01

    The paper is focused on elaboration of ZrO2 films on pure zirconium via anodizing in phosphoric acid with and without fluoride at constant potentials of 30 V and 60 V. The structure and composition of the films were investigated using scanning electronic microscopy, Raman spectroscopy and X-ray photoelectron spectroscopy. The composition of the oxides formed at both potentials can be identified as monoclinic ZrO2. In addition to Zr and O, the layers formed in phosphoric acid contain phosphorus originating from the phosphoric acid. When the phosphoric acid solution contains NaF, fluorine is also incorporated into the oxide layer. The oxides formed at a higher voltage have greater roughness than those formed at 30 V. Anodized samples exhibit smaller current densities during anodic polarization compared to the as-received zirconium covered with native oxide. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. THERMAL FISSION REACTOR COMPOSITIONS AND METHOD OF FABRICATING SAME

    DOEpatents

    Blainey, A.

    1959-10-01

    A body is presented for use in a thermal fission reactor comprising a sintered compressed mass of a substance of the group consisting of uranium, thorium, and oxides and carbides of uranium and thorium, enclosed in an envelope of a sintered, compacted, heat-conductive material of the group consisting of beryllium, zirconium, and oxides and carbides of beryllium and zirconium.

  7. Amperometric Biosensor Based on Zirconium Oxide/Polyethylene Glycol/Tyrosinase Composite Film for the Detection of Phenolic Compounds

    PubMed Central

    Ahmad, Nor Monica; Abdullah, Jaafar; Yusof, Nor Azah; Ab Rashid, Ahmad Hazri; Abd Rahman, Samsulida; Hasan, Md. Rakibul

    2016-01-01

    A phenolic biosensor based on a zirconium oxide/polyethylene glycol/tyrosinase composite film for the detection of phenolic compounds has been explored. The formation of the composite film was expected via electrostatic interaction between hexacetyltrimethylammonium bromide (CTAB), polyethylene glycol (PEG), and zirconium oxide nanoparticles casted on screen printed carbon electrode (SPCE). Herein, the electrode was treated by casting hexacetyltrimethylammonium bromide on SPCE to promote a positively charged surface. Later, zirconium oxide was mixed with polyethylene glycol and the mixture was dropped cast onto the positively charged SPCE/CTAB. Tyrosinase was further immobilized onto the modified SPCE. Characterization of the prepared nanocomposite film and the modified SPCE surface was investigated by scanning electron microscopy (SEM), Electrochemical Impedance Spectroscopy (EIS), and Cyclic voltamogram (CV). The developed biosensor exhibits rapid response for less than 10 s. Two linear calibration curves towards phenol in the concentrations ranges of 0.075–10 µM and 10–55 µM with the detection limit of 0.034 µM were obtained. The biosensor shows high sensitivity and good storage stability for at least 30 days. PMID:27367738

  8. An Explanation for Bends of 1-Dimensional Nanorods

    NASA Astrophysics Data System (ADS)

    Mukaida, Masashi; Ichinose, Ataru; Mele, Paolo; Mtsumoto, Kaname; Horii, Shigeru; Yoshida, Yutaka

    Growth of artificial pinning centers (APCs) in YBa2Cu3O7-J (YBCO) films are discussed. The APCs used in this research are BaZrO3 and BaSnO3 nanorods which are reported by Mele et al. TEM images show these nanorods graduallybend accordinglywith approachingtoasurfaceof films. This featureshowedagrowth patternlikeafirework. Weexplainthe featureofthe nanorodsas follows;Atanearlygrowth stage, filmsgrowinalayerbylayergrowth mode. The surface of the films is flat and very smooth. After the early growth stage, the film surface gradually becomes rough, indicating the film grows in a Stranski-Krastanov growth mode. This roughness was caused by a spiral growth of films with manysteps. At the step of YBCO films, nanorod materials such as BaZrO3 are supplied from one direction. Then, the center of nanorods sifts to the same direction of the step flow. Then, the nanorods bend to the edge of the grains in the films. As a grain in spiral growth had a convex surface, nanorods bent to the direction perpendicular to the grain surface. Finally, nanorods in rough grains form firework structures.

  9. Metaloxide--ZrO2 catalysts for the esterification and transesterification of free fatty acids and triglycerides to obtain bio-diesel

    DOEpatents

    Kim, Manhoe; Salley, Steven O.; Ng, K. Y. Simon

    2016-09-06

    Mixed metal oxide catalysts (ZnO, CeO, La2O3, NiO, Al203, SiO2, TiO2, Nd2O3, Yb2O3, or any combination of these) supported on zirconia (ZrO2) or hydrous zirconia are provided. These mixed metal oxide catalysts can be prepared via coprecipitation, impregnation, or sol-gel methods from metal salt precursors with/without a Zirconium salt precursor. Metal oxides/ZrO2 catalyzes both esterification and transesterification of oil containing free fatty acids in one batch or in single stage. In particular, these mixed metal oxides supported or added on zirconium oxide exhibit good activity and selectivity for esterification and transesterification. The low acid strength of this catalyst can avoid undesirable side reaction such as alcohol dehydration or cracking of fatty acids. Metal oxides/ZrO2 catalysts are not sensitive to any water generated from esterification. Thus, esterification does not require a water free condition or the presence of excess methanol to occur when using the mixed metal oxide catalyst. The FAME yield obtained with metal oxides/ZrO2 is higher than that obtained with homogeneous sulfuric acid catalyst. Metal oxides/ZrO2 catalasts can be prepared as strong pellets and in various shapes for use directly in a flow reactor. Furthermore, the pellet has a strong resistance toward dissolution to aqueous or oil phases.

  10. Container for reprocessing and permanent storage of spent nuclear fuel assemblies

    DOEpatents

    Forsberg, Charles W.

    1992-01-01

    A single canister process container for reprocessing and permanent storage of spent nuclear fuel assemblies comprising zirconium-based cladding and fuel, which process container comprises a collapsible container, having side walls that are made of a high temperature alloy and an array of collapsible support means wherein the container is capable of withstanding temperature necessary to oxidize the zirconium-based cladding and having sufficient ductility to maintain integrity when collapsed under pressure. The support means is also capable of maintaining their integrity at temperature necessary to oxide the zirconium-based cladding. The process container also has means to introduce and remove fluids to and from the container.

  11. Transformational dynamics of BZO and BHO nanorods imposed by Y2O3 nanoparticles for improved isotropic pinning in YBa2Cu3O7 -δ thin films

    NASA Astrophysics Data System (ADS)

    Gautam, Bibek; Sebastian, Mary Ann; Chen, Shihong; Shi, Jack; Haugan, Timothy; Xing, Zhongwen; Zhang, Wenrui; Huang, Jijie; Wang, Haiyan; Osofsky, Mike; Prestigiacomo, Joseph; Wu, Judy Z.

    2017-07-01

    An elastic strain model was applied to evaluate the rigidity of the c-axis aligned one-dimensional artificial pinning centers (1D-APCs) in YBa2Cu3O7-δ matrix films. Higher rigidity was predicted for BaZrO3 1D-APCs than that of the BaHfO3 1D-APCs. This suggests a secondary APC doping of Y2O3 in the 1D-APC/YBa2Cu3O7-δ nanocomposite films would generate a stronger perturbation to the c-axis alignment of the BaHfO3 1D-APCs and therefore a more isotropic magnetic vortex pinning landscape. In order to experimentally confirm this, we have made a comparative study of the critical current density Jc (H, θ, T) of 2 vol.% BaZrO3 + 3 vol.%Y2O3 and 2 vol.%BaHfO3 + 3 vol.%Y2O3 double-doped (DD) YBa2Cu3O7-δ films deposited at their optimal growth conditions. A much enhanced isotropic pinning was observed in the BaHfO3 DD samples. For example, at 65 K and 9.0 T, the variation of the Jc across the entire θ range from θ=0 (H//c) to θ=90 degree (H//ab) is less than 18% for BaHfO3 DD films, in contrast to about 100% for the BaZrO3 DD counterpart. In addition, lower α values from the Jc(H) ˜ H-α fitting were observed in the BaHfO3 DD films in a large θ range away from the H//c-axis. Since the two samples have comparable Jc values at H//c-axis, the improved isotropic pinning in BaHfO3 DD films confirms the theoretically predicted higher tunability of the BaHfO3 1D-APCs in APC/YBa2Cu3O7-δ nanocomposite films.

  12. An In Vivo Evaluation of the Fit of Zirconium-Oxide Based, Ceramic Single Crowns with Vertical and Horizontal Finish Line Preparations.

    PubMed

    Vigolo, Paolo; Mutinelli, Sabrina; Biscaro, Leonello; Stellini, Edoardo

    2015-12-01

    Different types of tooth preparations influence the marginal precision of zirconium-oxide based ceramic single crowns. In this in vivo study, the marginal fits of zirconium-oxide based ceramic single crowns with vertical and horizontal finish lines were compared. Forty-six teeth were chosen in eight patients indicated for extraction for implant placement. CAD/CAM technology was used for the production of 46 zirconium-oxide-based ceramic single crowns: 23 teeth were prepared with vertical finishing lines, 23 with horizontal finishing lines. One operator accomplished all clinical procedures. The zirconia crowns were cemented with glass ionomer cement. The teeth were extracted 1 month later. Marginal gaps along vertical planes were measured for each crown, using a total of four landmarks for each tooth by means of a microscope at 50× magnification. On conclusion of microscopic assessment, ESEM evaluation was completed on all specimens. The comparison of the gap between the two types of preparation was performed with a nonparametric test (two-sample Wilcoxon rank-sum test) with a level of significance fixed at p < 0.05. All data were analyzed with STATA12. In the group with horizontal finish line preparations, the median value of the gap was 35.45 μm (Iqr, 0.33); for the vertical finish line group, the median value of the gap was 35.44 μm (Iqr, 0.40). The difference between the two groups was not statistically significant (two-sample Wilcoxon rank-sum test, p = 0.0872). Within the limitations of this study, the gaps of the zirconium-oxide-based ceramic CAD/CAM crowns with vertical and horizontal finish line preparations were not different. © 2015 by the American College of Prosthodontists.

  13. Enhancing the performance of single-chambered microbial fuel cell using manganese/palladium and zirconium/palladium composite cathode catalysts.

    PubMed

    Jadhav, Dipak A; Deshpande, Parag A; Ghangrekar, Makarand M

    2017-08-01

    Application of ZrO 2 , MnO 2 , palladium, palladium-substituted-zirconium oxide (Zr 0.98 Pd 0.02 O 2 ) and palladium-substituted-manganese oxide (Mn 0.98 Pd 0.02 O 2 ) cathode catalysts in a single-chambered microbial fuel cell (MFC) was explored. The highest power generation (1.28W/m 3 ) was achieved in MFC with Mn 0.98 Pd 0.02 O 2 catalyst, which was higher than that with MnO 2 (0.58W/m 3 ) alone; whereas, MFC having Zr 0.98 Pd 0.02 O 2 catalyzed cathode and non-catalyzed cathode produced powers of 1.02 and 0.23W/m 3 , respectively. Also, low-cost zirconium-palladium-composite showed better catalytic activity and capacitance over ZrO 2 with 20A/m 3 current production and demonstrated its suitability for MFC applications. Cyclic voltammetry analyses showed higher well-defined redox peaks in composite catalysts (Mn/Zr-Pd-C) over other catalyzed MFCs containing MnO 2 or ZrO 2 . Electrochemical behaviour of composite catalysts on cathode showed higher availability of adsorption sites for oxygen reduction and, hence, enhanced the rate of cathodic reactions. Thus, Mn/Zr-Pd-C-based composite catalysts exhibited superior cathodic performance and could be proposed as alternatives to costly Pd-catalyst for field applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

  14. Suspensions on the basis of stabilised zirconium oxide for three-dimensional printing

    NASA Astrophysics Data System (ADS)

    Sokolov, P. S.; Komissarenko, D. A.; Shmeleva, I. A.; Slyusar, I. V.; Dosovitskiy, G. A.; Evdokimov, P. V.; Putlyaev, V. I.; Dosovitskiy, A. E.

    2018-04-01

    Present work considers the first results on rheological and photo-curing behaviour of suspension consisting of nanocrystalline stabilised zirconium dioxide powders (19 - 27 vol. %) and a liquid UV-photosensitive organic monomer. At ambient temperature compositions showed a viscosity of 2.5 and 0.8 Pa×s at 10 and 100 s-1 shear rates, respectively. Printability of these compositions was subsequently investigated by using an stereolithography machine Ember (Autodesk). 3D objects were later sintered in a separate furnace into dense translucent ZrO2 ceramics.

  15. Translucency and Strength of High Translucency Monolithic Zirconium Oxide Materials

    DTIC Science & Technology

    2016-05-17

    Zirconium-Oxide Materials presented at/published to the Journal of General Dentistry with MDWI 41-108, and has been assigned local file #16208. 2...PUBLISHED/PRESENTED. D 11a. PUBLICATION/JOURNAL (list intended publication/journal.) General Dentistry D 11b. PUBLISHED ABSTRACT (List intended...the most esthetic full veneer restorative material in dentistry for many years. In the mid-1900’s, dental materials researchers began marketing and

  16. Container for reprocessing and permanent storage of spent nuclear fuel assemblies

    DOEpatents

    Forsberg, C.W.

    1992-03-24

    A single canister process container is described for reprocessing and permanent storage of spent nuclear fuel assemblies comprising zirconium-based cladding and fuel, which process container comprises a collapsible container, having side walls that are made of a high temperature alloy and an array of collapsible support means wherein the container is capable of withstanding temperature necessary to oxidize the zirconium-based cladding and having sufficient ductility to maintain integrity when collapsed under pressure. The support means is also capable of maintaining its integrity at a temperature necessary to oxidize the zirconium-based cladding. The process container also has means to introduce and remove fluids to and from the container. 10 figs.

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

    Campbell, Keri R.; Judge, Elizabeth J.; Barefield, James E.

    We show the analysis of light water reactor simulated used nuclear fuel using laser-induced breakdown spectroscopy (LIBS) is explored using a simplified version of the main oxide phase. The main oxide phase consists of the actinides, lanthanides, and zirconium. The purpose of this study is to develop a rapid, quantitative technique for measuring zirconium in a uranium dioxide matrix without the need to dissolve the material. A second set of materials including cerium oxide is also analyzed to determine precision and limit of detection (LOD) using LIBS in a complex matrix. Two types of samples are used in this study:more » binary and ternary oxide pellets. The ternary oxide, (U,Zr,Ce)O 2 pellets used in this study are a simplified version the main oxide phase of used nuclear fuel. The binary oxides, (U,Ce)O 2 and (U,Zr)O 2 are also examined to determine spectral emission lines for Ce and Zr, potential spectral interferences with uranium and baseline LOD values for Ce and Zr in a UO 2 matrix. In the spectral range of 200 to 800 nm, 33 cerium lines and 25 zirconium lines were identified and shown to have linear correlation values (R 2) > 0.97 for both the binary and ternary oxides. The cerium LOD in the (U,Ce)O 2 matrix ranged from 0.34 to 1.08 wt% and 0.94 to 1.22 wt% in (U,Ce,Zr)O 2 for 33 of Ce emission lines. The zirconium limit of detection in the (U,Zr)O 2 matrix ranged from 0.84 to 1.15 wt% and 0.99 to 1.10 wt% in (U,Ce,Zr)O 2 for 25 Zr lines. Finally, the effect of multiple elements in the plasma and the impact on the LOD is discussed.« less

  18. Development of Cold Spray Coatings for Accident-Tolerant Fuel Cladding in Light Water Reactors

    NASA Astrophysics Data System (ADS)

    Maier, Benjamin; Yeom, Hwasung; Johnson, Greg; Dabney, Tyler; Walters, Jorie; Romero, Javier; Shah, Hemant; Xu, Peng; Sridharan, Kumar

    2018-02-01

    The cold spray coating process has been developed at the University of Wisconsin-Madison for the deposition of oxidation-resistant coatings on zirconium alloy light water reactor fuel cladding with the goal of improving accident tolerance during loss of coolant scenarios. Coatings of metallic (Cr), alloy (FeCrAl), and ceramic (Ti2AlC) materials were successfully deposited on zirconium alloy flats and cladding tube sections by optimizing the powder size, gas preheat temperature, pressure and composition, and other process parameters. The coatings were dense and exhibited excellent adhesion to the substrate. Evaluation of the samples after high-temperature oxidation tests at temperatures up to 1300°C showed that the cold spray coatings significantly mitigate oxidation kinetics because of the formation of thin passive oxide layers on the surface. The results of the study indicate that the cold spray coating process is a viable near-term option for developing accident-tolerant zirconium alloy fuel cladding.

  19. Continuum model for hydrogen pickup in zirconium alloys of LWR fuel cladding

    NASA Astrophysics Data System (ADS)

    Wang, Xing; Zheng, Ming-Jie; Szlufarska, Izabela; Morgan, Dane

    2017-04-01

    A continuum model for calculating the time-dependent hydrogen pickup fractions in various Zirconium alloys under steam and pressured water oxidation has been developed in this study. Using only one fitting parameter, the effective hydrogen gas partial pressure at the oxide surface, a qualitative agreement is obtained between the predicted and previously measured hydrogen pickup fractions. The calculation results therefore demonstrate that H diffusion through the dense oxide layer plays an important role in the hydrogen pickup process. The limitations and possible improvement of the model are also discussed.

  20. Method for making fine and ultrafine spherical particles of zirconium titanate and other mixed metal oxide systems

    DOEpatents

    Hu, Michael Z.

    2006-05-23

    Disclosed is a method for making amorphous spherical particles of zirconium titanate and crystalline spherical particles of zirconium titanate comprising the steps of mixing an aqueous solution of zirconium salt and an aqueous solution of titanium salt into a mixed solution having equal moles of zirconium and titanium and having a total salt concentration in the range from 0.01 M to about 0.5 M. A stearic dispersant and an organic solvent is added to the mixed salt solution, subjecting the zirconium salt and the titanium salt in the mixed solution to a coprecipitation reaction forming a solution containing amorphous spherical particles of zirconium titanate wherein the volume ratio of the organic solvent to aqueous part is in the range from 1 to 5. The solution of amorphous spherical particles is incubated in an oven at a temperature .ltoreq.100.degree. C. for a period of time .ltoreq.24 hours converting the amorphous particles to fine or ultrafine crystalline spherical particles of zirconium titanate.

  1. High quality transparent conducting oxide thin films

    DOEpatents

    Gessert, Timothy A.; Duenow, Joel N.; Barnes, Teresa; Coutts, Timothy J.

    2012-08-28

    A transparent conducting oxide (TCO) film comprising: a TCO layer, and dopants selected from the elements consisting of Vanadium, Molybdenum, Tantalum, Niobium, Antimony, Titanium, Zirconium, and Hafnium, wherein the elements are n-type dopants; and wherein the transparent conducting oxide is characterized by an improved electron mobility of about 42 cm.sup.2/V-sec while simultaneously maintaining a high carrier density of .about.4.4e.times.10.sup.20 cm.sup.-3.

  2. Epitaxial YBa2Cu3O7-x nanocomposite films and coated conductors from BaMO3 (M = Zr, Hf) colloidal solutions

    NASA Astrophysics Data System (ADS)

    Obradors, X.; Puig, T.; Li, Z.; Pop, C.; Mundet, B.; Chamorro, N.; Vallés, F.; Coll, M.; Ricart, S.; Vallejo, B.; Pino, F.; Palau, A.; Gázquez, J.; Ros, J.; Usoskin, A.

    2018-04-01

    Superconducting nanocomposites are the best material choice to address the performance required in power applications and magnets working under high magnetic fields. However, it is still challenging to sort out how to achieve the highest superconducting performance using attractive and competitive manufacturing processes. Colloidal solutions have been recently developed as a novel and very promising low cost route to manufacture nanocomposite coated conductors. Well dispersed and stabilized preformance nanoparticle solutions are first prepared with high concentrations and then mixed with the YBa2Cu3O7 metalorganic precursor solutions to generate colloidal solutions to grow the nanocomposite films. Here we demonstrate, for the first time, that non-reactive BaZrO3 and BaHfO3 perovskite preformed nanoparticles are suitable for growing high quality thin and thick films, and coated conductors with a homogeneous distribution and controlled particle size using this fabrication method. Additionally, we extend the nanoparticle content of the nanocomposites up to 20%-25% mol without any degradation of the superconducting properties. Thick nanocomposite films, up to 0.8 μm, have been prepared with a single deposition of low-fluorine solutions using an ink jet printing dispenser and we demonstrate that the preformed nanoparticles display only a very limited coarsening during the growth process and so high critical current densities J c (B) under high magnetic fields. These films show the highest critical currents achieved so far based on the colloidal solution approach, I c = 220 A/cm-w at 77 K and self-field, and they still have a high potential for further increase in the film thickness. Finally, we also show that nanocomposite YBa2Cu3O7-BaZrO3 coated conductors based on an alternating beam assisted deposited YSZ buffer layer on stainless steel metallic substrates can be developed based on these novel colloidal solutions. Non-reactive preformed oxide perovskite nanoparticles are therefore very promising elements to further advance the colloidal solution approach in the implementation of low cost and high performance coated conductors for high magnetic field applications.

  3. Obtaining composite Zr-Al-O coating on the surface of zirconium by microplasma oxidation

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

    Gubaidulina, Tatiana A., E-mail: goub2002@mail.ru, E-mail: ostk@mail2000ru; Kuzmin, Oleg S., E-mail: goub2002@mail.ru, E-mail: ostk@mail2000ru; Fedorischva, Marina V., E-mail: fmw@ispms.tsc.ru, E-mail: kmp1980@mail.ru

    2014-11-14

    The paper describes the application of the microplasma oxidation for production of Zr-Al-O composition on the surface of zirconium. Certification of a new-type power supply for depositing oxide ceramic coatings by microplasma oxidation was also carried out. The growth rate of Zr-Al-O coating amounted around 0.2 nm/s, which around 10 times exceeds that for depositing similar coatings using the similar equipment. We have studied the change of surface morphology and the chemical composition of the formed ceramic coating by means of EVO 50 scanning electron microscope and X-ray spectral analysis.

  4. Integral neutron kerma coefficient ratios for silicon, iron, and oxygen to carbon on the energy range from 15 to 30 MeV

    NASA Astrophysics Data System (ADS)

    Miranda, Juan Gustavo

    2001-07-01

    Kerma coefficient ratios are reported for carbon to oxygen, silicon, and iron in the energy range of 15 to 30 MeV. The determination was done by measuring dose to the gas of proportional counters exposed to a well characterized neutron field. The measured dose in the proportional counter gas was then converted to dose in the proportional counter wall material applying Bragg-Gray theory. The proportional counters were made of the material of interest. The oxygen measurement was done by irradiating simultaneously zirconium and zirconium oxide proportional counters and substracting the dose to the zirconium from the zirconium oxide. Neutrons were generated with the UW Tandem Accelerator. The reaction 3H(d, n)4 He provided our neutron source which consisted of monoenergetic neutrons. Neutron spectra measurements were carried out for the 27.3 MeV neutron energy. This was necessary because of the presence of contaminating breakup neutrons at this energy. The spectra were measured with a pulse beam time-of-flight spectrometer and a NE-213 liquid scintillator. The dose conversion factor r is reported for carbon, oxygen, silicon, iron, zirconium, and zirconium oxide relative to TE-propane gas at neutron energies of 20, 23 and 27 MeV. The factor r, which relates the dose to the gas to that of the proportional counter through the Bragg-Gray theory, was calculated from angle integrated differential cross sections. This required a calculation of the initial energy spectra as well as the differential secondary charged particle energy spectra and for the first time a complete treatment of all heavy ions is considered. Furthermore, as the conditions required to apply the Bragg-Gray theory are difficult to satisfy (infinitesimal cavity), we report the calculation of the dose conversion factor r for the finite cavity case for carbon/TE-gas in order to test the validity of the application of the theory to this type of applications. We found that the two conditions of the Bragg-Gray theory are violated: the differential secondary charged particle spectrum is perturbed by the presence of the cavity and that the dose absorbed in the cavity is not enteraly deposited by the particles crossing it. However, these changes in the spectra and the dose deposition are not very sensitive to the conversion factor r because this factor only reflects the ratio of these changes. Our results are found to be in agreement, within the uncertainty associated to the determination, with previous published values when comparable data exits.

  5. Superconducting Generators for Airborne Applications and YBCO-Coated Conductors (Preprint)

    DTIC Science & Technology

    2008-10-01

    Maiorov, M. E. Hawley , M. P. Maley, D. E. Peterson, “Strongly enhanced current densities in superconducting coated conductors of YBa2Cu3O7-x + BaZrO3...ed., New York: Taylor and Francis, 2001. [17] S. P. Ashworth, M. Maley, M. Suenaga, S. R. Foltyn, and J. O. Willis , J. Appl. Phys., vol. 88, p

  6. Incorporating YBCO Coated Conductors in High-speed Superconducting Generators

    DTIC Science & Technology

    2008-07-01

    Maiorov, M. E. Hawley , M. P. Maley, D. E. Peterson, ―Strongly enhanced current densities in superconducting coated conductors of YBa2Cu3O7-x + BaZrO3...2nd ed., New York: Taylor and Francis, 2001. [23] S. P. Ashworth, M. Maley, M. Suenaga, S. R. Foltyn, and J. O. Willis , J. Appl. Phys., vol. 88

  7. Pyroelectric response in crystalline hafnium zirconium oxide (Hf 1- x Zr x O 2 ) thin films

    DOE PAGES

    Smith, S. W.; Kitahara, A. R.; Rodriguez, M. A.; ...

    2017-02-13

    Pyroelectric coefficients were measured for 20 nm thick crystalline hafnium zirconium oxide (Hf 1-xZr xO 2) thin films across a composition range of 0 ≤ x ≤ 1. Pyroelectric currents were collected near room temperature under zero applied bias and a sinusoidal oscillating temperature profile to separate the influence of non-pyroelectric currents. The pyroelectric coefficient was observed to correlate with zirconium content, increased orthorhombic/tetragonal phase content, and maximum polarization response. The largest measured absolute value was 48 μCm -2K -1 for a composition with x = 0.64, while no pyroelectric response was measured for compositions which displayed no remanent polarizationmore » (x = 0, 0.91, 1).« less

  8. Anisotropy of the Irreversibility Field for Zr-doped (Y,Gd)Ba 2<\\sub>Cu3<\\sub>O<7-x<\\sub> Thin Films up to 45 T

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

    Tarantini, C.; Jaroszynski, J.; Kametani, F.

    2011-01-01

    The anisotropic irreversibility fieldBIrr of twoYBa2Cu3O7 x thin films dopedwith additional rare earth (RE)= (Gd, Y) and Zr and containing strong correlated pins (splayed BaZrO3 nanorods and RE2O3 anoprecipitates) has been measured over a very broad range up to 45 T at temperatures 56 K < T < Tc. We found that the experimental angular dependence of BIrr ( ) does not follow the mass anisotropy scaling BIrr ( ) = BIrr (0)(cos2 + 2 sin2 ) 1/2, where = (mc/mab)1/2 = 5 6 for the RE-doped Ba2Cu3O7 x (REBCO) crystals, mab and mc are the effective masses along themore » ab plane and the c-axis, respectively, and is the angle between B and the c-axis. For B parallel to the ab planes and to the c-axis correlated pinning strongly enhances BIrr , while at intermediate angles, BIrr ( ) follows the scaling behavior BIrr ( ) (cos2 + 2 RP sin2 ) 1/2 with the effective anisotropy factor RP 3 significantly smaller than the ass anisotropy would suggest. In spite of the strong effects of c-axis BaZrO3 nanorods, we found even greater enhancements of BIrr for fields along the ab planes than for fields parallel to the c-axis, as well as different temperature dependences of the correlated pinning contributions to BIrr for B//ab and B//c. Our results show that the dense and strong pins, which can now be incorporated into REBCO thin films in a controlled way, exert major and diverse effects on the measured vortex pinning anisotropy and the irreversibility field over wide ranges of B and T . In particular, we show that the relative contribution of correlated pinning to BIrr for B//c increases as the temperature increases due to the suppression of thermal fluctuations of vortices by splayed distribution of BaZrO3 nanorods.« less

  9. Finite element analysis of the tetragonal to monoclinic phase transformation during oxidation of zirconium alloys

    NASA Astrophysics Data System (ADS)

    Platt, P.; Frankel, P.; Gass, M.; Howells, R.; Preuss, M.

    2014-11-01

    Corrosion is a key limiting factor in the degradation of zirconium alloys in light water reactors. Developing a mechanistic understanding of the corrosion process offers a route towards improving safety and efficiency as demand increases for higher burn-up of fuel. Oxides formed on zirconium alloys are composed of both monoclinic and meta-stable tetragonal phases, and are subject to a number of potential mechanical degradation mechanisms. The work presented investigates the link between the tetragonal to monoclinic oxide phase transformation and degradation of the protective character of the oxide layer. To achieve this, Abaqus finite element analysis of the oxide phase transformation has been carried out. Study of the change in transformation strain energy shows how relaxation of oxidation induced stress and fast fracture at the metal-oxide interface could destabilise the tetragonal phase. Central to this is the identification of the transformation variant most likely to form, and understanding why twinning of the transformed grain is likely to occur. Development of transformation strain tensors and analysis of the strain components allows some separation of dilatation and shear effects. Maximum principal stress is used as an indication of fracture in the surrounding oxide layer. Study of the stress distributions shows the way oxide fracture is likely to occur and the differing effects of dilatation and shape change. Comparison with literature provides qualitative validation of the finite element simulations.

  10. Formation and reduction behaviors of zirconium oxide compounds in LiCl-Li2O melt at 923 K

    NASA Astrophysics Data System (ADS)

    Sakamura, Yoshiharu; Iizuka, Masatoshi; Kitawaki, Shinichi; Nakayoshi, Akira; Kofuji, Hirohide

    2015-11-01

    The reduction behaviors of ZrO2, Li2ZrO3 and (U,Pu,Zr)O2 in a LiCl-Li2O salt bath at 923 K were investigated. This study was conducted as part of a feasibility study on the pyrochemical treatment of damaged fuel debris generated by severe accidents at light water reactors. It was demonstrated in electrolytic reduction tests that the uranium in synthetic corium specimens of (U,Pu,Zr)O2 with various ZrO2 contents could be reduced to the metallic form and that part of the zirconium was converted to Li2ZrO3. Zirconium metal and Li2ZrO3 were obtained by the reduction of ZrO2. The reduction of Li2ZrO3 did not proceed even in LiCl containing no Li2O. Moreover, the stable chemical forms of the ZrO2-Li2O complex oxide were investigated as a function of the Li2O concentration in LiCl. ZrO2 was converted to Li2ZrO3 at a Li2O concentration of 0.018 wt%. As the Li2O concentration was increased, Li2ZrO3 was converted to Li6Zr2O7 and then to Li8ZrO6. It is suggested that the removal of Li2ZrO3 from the reduction product is a key point in the pyrochemical treatment of corium.

  11. Experimental Calcium Silicate-Based Cement with and without Zirconium Oxide Modulates Fibroblasts Viability.

    PubMed

    Slompo, Camila; Peres-Buzalaf, Camila; Gasque, Kellen Cristina da Silva; Damante, Carla Andreotti; Ordinola-Zapata, Ronald; Duarte, Marco Antonio Hungaro; de Oliveira, Rodrigo Cardoso

    2015-01-01

    The aim of this study was to verify whether the use of zirconium oxide as a radiopacifier of an experimental calcium silicate-based cement (WPCZO) leads to cytotoxicity. Fibroblasts were treated with different concentrations (10 mg/mL, 1 mg/mL, and 0.1 mg/mL) of the cements diluted in Dulbecco's modified Eagle's medium (DMEM) for periods of 12, 24, and 48 h. Groups tested were white Portland cement (WPC), white Portland cement with zirconium oxide (WPCZO), and white mineral trioxide aggregate Angelus (MTA). Control group cells were not treated. The cytotoxicity was evaluated through mitochondrial-activity (MTT) and cell-density (crystal violet) assays. All cements showed low cytotoxicity. In general, at the concentration of 10 mg/mL there was an increase in viability of those groups treated with WPC and WPCZO when compared to the control group (p<0.05). A similar profile for the absorbance values was noted among the groups: 10 mg/mL presented an increase in viability compared to the control group. On the other hand, smaller concentrations presented a similar or lower viability compared to the control group, in general. A new dental material composed of calcium silicate-based cement with 20% zirconium oxide as the radiopacifier showed low cytotoxicity as a promising material to be exploited for root-end filling.

  12. Enhanced Proton Conductivity in Y-Doped BaZrO3 via Strain Engineering.

    PubMed

    Fluri, Aline; Marcolongo, Aris; Roddatis, Vladimir; Wokaun, Alexander; Pergolesi, Daniele; Marzari, Nicola; Lippert, Thomas

    2017-12-01

    The effects of stress-induced lattice distortions (strain) on the conductivity of Y-doped BaZrO 3 , a high-temperature proton conductor with key technological applications for sustainable electrochemical energy conversion, are studied. Highly ordered epitaxial thin films are grown in different strain states while monitoring the stress generation and evolution in situ. Enhanced proton conductivity due to lower activation energies is discovered under controlled conditions of tensile strain. In particular, a twofold increased conductivity is measured at 200 °C along a 0.7% tensile strained lattice. This is at variance with conclusions coming from force-field simulations or the static calculations of diffusion barriers. Here, extensive first-principles molecular dynamic simulations of proton diffusivity in the proton-trapping regime are therefore performed and found to agree with the experiments. The simulations highlight that compressive strain confines protons in planes parallel to the substrate, while tensile strain boosts diffusivity in the perpendicular direction, with the net result that the overall conductivity is enhanced. It is indeed the presence of the dopant and the proton-trapping effect that makes tensile strain favorable for proton conduction.

  13. Characterization of nanoscale oxide and oxyhydroxide powders using EXAFS spectroscopy

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

    Darab, J.G.; Linehan, J.C.; Matson, D.W.

    1993-06-01

    Extended x-ray absorption fine structure (EXAFS) spectroscopy has been used to determine the structural environment local to iron(HI) and zircorium(IV) cations in respectively, nanoscale iron oxyhydroxide and nanoscale zirconium oxide powders. The iron oxyhydroxide powder, produced by the modified reverse micelle (MRM) technology, was found to have a short-range structure most similar to that of goethite ([alpha]-FeOOH). The short-range structure of the zirconium oxide powder, produced using the rapid thermal decomposition of solutes (RTDS) technology, was found to be a mixture of monoclinic zirconia and cubic zirconia environments.

  14. Characterization of nanoscale oxide and oxyhydroxide powders using EXAFS spectroscopy

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

    Darab, J.G.; Linehan, J.C.; Matson, D.W.

    1993-06-01

    Extended x-ray absorption fine structure (EXAFS) spectroscopy has been used to determine the structural environment local to iron(HI) and zircorium(IV) cations in respectively, nanoscale iron oxyhydroxide and nanoscale zirconium oxide powders. The iron oxyhydroxide powder, produced by the modified reverse micelle (MRM) technology, was found to have a short-range structure most similar to that of goethite ({alpha}-FeOOH). The short-range structure of the zirconium oxide powder, produced using the rapid thermal decomposition of solutes (RTDS) technology, was found to be a mixture of monoclinic zirconia and cubic zirconia environments.

  15. Synthesis of zirconium oxynitride in air under DC electric fields

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

    Morisaki, Nobuhiro; Tokunaga, Tomoharu; Sasaki, Katsuhiro

    We synthesized zirconium oxynitride from yttria-stabilized zirconia (YSZ) in air by applying DC electric fields that produced a controlled electric current in the specimen. When YSZ was heated under an applied DC electric field, the electric current of the specimen steeply increased at a critical temperature, called a flash event, during flash sintering. By keeping the electric current of the specimen constant during the flash event and then holding the specimen at the critical temperature, YSZ was transformed into zirconium oxynitride under the optimal conditions of 50 V/cm, 500 mA, and 1000 °C. We confirmed that zirconium oxynitride formed using high-resolution transmission electronmore » microscopy, electron energy-loss spectroscopy, and energy-dispersive spectrometry. To convert oxides to nitrides, reducing conditions are necessary to form excess oxygen vacancies. Our technique produced the strong reducing conditions necessary to form nitrides from the oxides by delivering a controlled electric current to the specimen.« less

  16. Laser-induced breakdown spectroscopy of light water reactor simulated used nuclear fuel: Main oxide phase

    DOE PAGES

    Campbell, Keri R.; Judge, Elizabeth J.; Barefield, James E.; ...

    2017-04-22

    We show the analysis of light water reactor simulated used nuclear fuel using laser-induced breakdown spectroscopy (LIBS) is explored using a simplified version of the main oxide phase. The main oxide phase consists of the actinides, lanthanides, and zirconium. The purpose of this study is to develop a rapid, quantitative technique for measuring zirconium in a uranium dioxide matrix without the need to dissolve the material. A second set of materials including cerium oxide is also analyzed to determine precision and limit of detection (LOD) using LIBS in a complex matrix. Two types of samples are used in this study:more » binary and ternary oxide pellets. The ternary oxide, (U,Zr,Ce)O 2 pellets used in this study are a simplified version the main oxide phase of used nuclear fuel. The binary oxides, (U,Ce)O 2 and (U,Zr)O 2 are also examined to determine spectral emission lines for Ce and Zr, potential spectral interferences with uranium and baseline LOD values for Ce and Zr in a UO 2 matrix. In the spectral range of 200 to 800 nm, 33 cerium lines and 25 zirconium lines were identified and shown to have linear correlation values (R 2) > 0.97 for both the binary and ternary oxides. The cerium LOD in the (U,Ce)O 2 matrix ranged from 0.34 to 1.08 wt% and 0.94 to 1.22 wt% in (U,Ce,Zr)O 2 for 33 of Ce emission lines. The zirconium limit of detection in the (U,Zr)O 2 matrix ranged from 0.84 to 1.15 wt% and 0.99 to 1.10 wt% in (U,Ce,Zr)O 2 for 25 Zr lines. Finally, the effect of multiple elements in the plasma and the impact on the LOD is discussed.« less

  17. Probing the bulk ionic conductivity by thin film hetero-epitaxial engineering

    NASA Astrophysics Data System (ADS)

    Pergolesi, Daniele; Roddatis, Vladimir; Fabbri, Emiliana; Schneider, Christof W.; Lippert, Thomas; Traversa, Enrico; Kilner, John A.

    2015-02-01

    Highly textured thin films with small grain boundary regions can be used as model systems to directly measure the bulk conductivity of oxygen ion conducting oxides. Ionic conducting thin films and epitaxial heterostructures are also widely used to probe the effect of strain on the oxygen ion migration in oxide materials. For the purpose of these investigations a good lattice matching between the film and the substrate is required to promote the ordered film growth. Moreover, the substrate should be a good electrical insulator at high temperature to allow a reliable electrical characterization of the deposited film. Here we report the fabrication of an epitaxial heterostructure made with a double buffer layer of BaZrO3 and SrTiO3 grown on MgO substrates that fulfills both requirements. Based on such template platform, highly ordered (001) epitaxially oriented thin films of 15% Sm-doped CeO2 and 8 mol% Y2O3 stabilized ZrO2 are grown. Bulk conductivities as well as activation energies are measured for both materials, confirming the success of the approach. The reported insulating template platform promises potential application also for the electrical characterization of other novel electrolyte materials that still need a thorough understanding of their ionic conductivity.

  18. Mineral resource of the month: zirconium and hafnium

    USGS Publications Warehouse

    Gambogi, Joseph

    2007-01-01

    Zirconium and hafnium are corrosion-resistant metals that are grouped in the same family as titanium on the periodic table. The two elements commonly occur in oxide and silicate minerals and have significant economic importance in everything from ink, ceramics and golf shoes to nuclear fuel rods.

  19. Preparation of highly-oxidized starch using hydrogen peroxide and its application as a novel ligand for zirconium tanning of leather.

    PubMed

    Yu, Yue; Wang, Ya-Nan; Ding, Wei; Zhou, Jianfei; Shi, Bi

    2017-10-15

    A series of highly-oxidized starch (HOS) were prepared using H 2 O 2 and a copper-iron catalyst as a desired ligand for zirconium tanning of leather. The effects of catalyst and H 2 O 2 dosages, and reaction temperature on the oxidation degree (OD, represented as the amount of carbonyl and carboxyl groups derived) of starch were investigated. The OD reached 76.2% when oxidation was conducted using 60% H 2 O 2 and 0.015% catalyst at 98°C for 2h. 13 C NMR and FT-IR illustrated carbonyl and carboxyl groups were formed in HOS after oxidation. GPC and laser particle size analyses indicated the decrease of HOS molecular size with increasing H 2 O 2 dosage and OD. HOS with moderate OD and molecular weight was able to coordinate with zirconium and remarkably improve tanning process. Leather tanned by Zr complexes using HOS-60 (60% H 2 O 2 , Mn 3516g/mol) as ligand presented considerably better physical and organoleptic properties than those of traditional Zr-tanned leather. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Vacuum-Induction, Vacuum-Arc, and Air-Induction Melting of a Complex Heat-Resistant Alloy

    NASA Technical Reports Server (NTRS)

    Decker, R. F.; Rowe, John P.; Freeman, J. W.

    1959-01-01

    The relative hot-workability and creep-rupture properties at 1600 F of a complex 55Ni-20Cr-15Co-4Mo-3Ti-3Al alloy were evaluated for vacuum-induction, vacuum-arc, and air-induction melting. A limited study of the role of oxygen and nitrogen and the structural effects in the alloy associated with the melting process was carried out. The results showed that the level of boron and/or zirconium was far more influential on properties than the melting method. Vacuum melting did reduce corner cracking and improve surface during hot-rolling. It also resulted in more uniform properties within heats. The creep-rupture properties were slightly superior in vacuum heats at low boron plus zirconium or in heats with zirconium. There was little advantage at high boron levels and air heats were superior at high levels of boron plus zirconium. Vacuum heats also had fewer oxide and carbonitride inclusions although this was a function of the opportunity for separation of the inclusions from high oxygen plus nitrogen heats. The removal of phosphorous by vacuum melting was not found to be related to properties. Oxygen plus nitrogen appeared to increase ductility in creep-rupture tests suggesting that vacuum melting removes unidentified elements detrimental to ductility. Oxides and carbonitrides in themselves did not initiate microcracks. Carbonitrides in the grain boundaries of air heats did initiate microcracks. The role of microcracking from this source and as a function of oxygen and nitrogen content was not clear. Oxygen and nitrogen did intensify corner cracking during hot-rolling but were not responsible for poor surface which resulted from rolling heats melted in air.

  1. Materials Coating Techniques

    DTIC Science & Technology

    1980-03-01

    applications from decorative to utilitarian over significant segments of the engineering, chemical, nuclear , microelectronics, and related Industries. PVD...Thermal-control coating. Boron 2430 Cermet component, nuclear shielding and controlrod material; Carbide wear- and temperature-resistant. Calcium...Zirconium Oxide (Hafnia-Pree � Thermal-barrier coatings for nuclear applications. Lime Stabi!Aed) Zirconium 2563 Resistant to high-temperature

  2. Physicochemical properties of precursors of Al2O3-ZrO2 oxide ceramics prepared by electrochemical method

    NASA Astrophysics Data System (ADS)

    Petrova, E. V.; Dresvyannikov, A. F.; Ahmadi Daryakenari, M.; Khairullina, A. I.

    2016-05-01

    Scanning electron microscopy, X-ray, and thermal analysis are used to examine the structure and properties of dispersive systems based on aluminum and zirconium oxides prepared electrochemically. The effect the conditions of synthesis have on the structure and morphology of Al2O3-ZrO2 particles is studied. It is shown that the effect of an electric field on the reaction medium allows us to adjust the physicochemical properties and morphology.

  3. In-situ surface science studies of the interaction between sulfur dioxide and two-dimensional palladium loaded-cerium/zirconium mixed metal oxide model catalysts

    NASA Astrophysics Data System (ADS)

    Romano, Esteban Javier

    2005-07-01

    Cerium and zirconium oxides are important materials in industrial catalysis. Particularly, the great advances attained in the past 30 years in controlling levels of gaseous pollutants released from internal combustion engines can be attributed to the development of catalysts employing these materials. Unfortunately, oxides of sulfur are known threats to the longevity of many catalytic systems by irreversibly interacting with catalytic materials. In this work, polycrystalline cerium-zirconium mixed-metal-oxide (MMO) solid solutions were synthesized. High resolution x-ray photoelectron spectroscopy (XPS) spectral data was collected and examined for revelation of the surface species that form on these metal oxides after in-situ exposures to sulfur dioxide. The model catalysts were exposed to sulfur dioxide using a custom modified in-situ reaction cell and platen heater. The results of this study demonstrate the formation of sulfate and sulfite surface sulfur species. Temperature and compositional dependencies were displayed, with higher temperatures and ceria molar ratios displaying a larger propensity for forming surface sulfur species. In addition to analysis of sulfur photoemission, the photoemission regions of oxygen, zirconium, and cerium were examined for the materials used in this study before and after the aforementioned treatments with sulfur dioxide. The presence of surface hydroxyl groups was observed and metal oxidation state changes were probed to further enhance the understanding of sulfur dioxide adsorption on the synthesized materials. Palladium loaded mixed-metal oxides were synthesized using a unique solid-state methodology to probe the effect of palladium addition on sulfur dioxide adsorption. The addition of palladium to this model system is shown to have a strong effect on the magnitude of adsorption for sulfur dioxide on some material/exposure condition combinations. Ceria/zirconia sulfite and sulfate species are identified on the palladium-loaded MMO materials with adsorption sites located on the exposed oxide sites.

  4. Extensive Bone Reaction From Catastrophic Oxidized Zirconium Wear.

    PubMed

    Cassar-Gheiti, Adrian J; Collins, Dennis; McCarthy, Tom

    2016-01-01

    The use of alternative bearing surfaces for total hip arthroplasty has become popular to minimize wear and increase longevity, especially in young patients. Oxidized zirconium (Oxinium; Smith & Nephew, Memphis, Tennessee) femoral heads were introduced in the past decade for use in total hip arthroplasty. The advantages of oxidized zirconium include less risk of fracture compared with traditional ceramic heads. This case report describes a patient with a history of bilateral avascular necrosis of the femoral head after chemotherapy for acute lymphoblastic leukemia. Nonoperative management of avascular necrosis failed, and the patient was treated with bilateral total hip arthroplasty. The patient was followed at regular intervals and had slow eccentric polyethylene wear during a 10-year period. After 10 years, the patient had accelerated wear, with femoral and acetabular bone changes as a result of Oxinium and ultrahigh-molecular-weight polyethylene wear during a 6-month period. This article highlights the unusual accelerated bone changes that occurred as a result of Oxinium wear particles. Copyright 2016, SLACK Incorporated.

  5. High Temperature Corrosion and Heat Transfer Studies of Zirconium-Silicide Coatings for Light Water Reactor Cladding Applications

    NASA Astrophysics Data System (ADS)

    Yeom, Hwasung

    Experimental results investigating the feasibility of zirconium-silicide coating for accident tolerance of LWR fuel cladding coating was presented. The oxidation resistance of ZrSi2 appeared to be superior to bare Zircaloy-4 in high temperature air. It was shown that micro- and nanostructures consisting of alternating SiO2 and ZrO2 evolved during transient oxidation of ZrSi2, which was explained by spinodal phase decomposition of Zr-Si-O oxide. Coating optimization regarding oxidation resistance was performed mainly using magnetron sputter deposition method. ZrSi 2 coatings ( 3.9 microm) showed improvement of almost two orders of magnitude when compared to bare Zircaloy-4 after air-oxidation at 700 °C for 20-hours. Pre-oxidation of ZrSi2 coating at 700 °C for 5 h significantly mitigated oxygen diffusion in air-oxidation tests at 1000 °C for 1-hour and 1200 °C for 10-minutes. The ZrSi2 coating with the pre-oxidation was found to be the best condition to prevent oxide formation in Zircaloy-4 substrate in the steam condition even if the top surface of the coating was degraded by formation of zirconium-rich oxide layer. Only the ZrSiO4 phase, formed by exposing the ZrSi2 coating at 1400 °C in air, allowed for immobilization of silicon species in the oxide scale in the aqueous environments. A quench test facility was designed and built to study transient boiling heat transfer of modified Zircaloy-4 surfaces (e.g., roughened surfaces, oxidized surfaces, ZrSi2 coated surfaces) at various system conditions (e.g., elevated pressures and water subcooling). The minimum film boiling temperature increased with increasing system pressure and water subcooling, consistent with past literature. Quenching behavior was affected by the types of surface modification regardless of the environmental conditions. Quenching heat transfer was improved by the ZrSi 2 coating, a degree of surface oxidation (deltaox = 3 to 50 microm), and surface roughening (Ra 20 microm). A plausible hypothesis based on transient heat conduction models for liquid-solid contact in quenching process was proposed to explain the enhanced quenching performance. The theoretical model incorporated localized temperature behavior on superheated surface and elucidated bubble dynamics qualitatively, and predicts minimum film boiling temperature of oxidized Zirc-4 surfaces, which were in good agreement with experimental data.

  6. Chemical solution route to self-assembled epitaxial oxide nanostructures.

    PubMed

    Obradors, X; Puig, T; Gibert, M; Queraltó, A; Zabaleta, J; Mestres, N

    2014-04-07

    Self-assembly of oxides as a bottom-up approach to functional nanostructures goes beyond the conventional nanostructure formation based on lithographic techniques. Particularly, chemical solution deposition (CSD) is an ex situ growth approach very promising for high throughput nanofabrication at low cost. Whereas strain engineering as a strategy to define nanostructures with tight control of size, shape and orientation has been widely used in metals and semiconductors, it has been rarely explored in the emergent field of functional complex oxides. Here we will show that thermodynamic modeling can be very useful to understand the principles controlling the growth of oxide nanostructures by CSD, and some attractive kinetic features will also be presented. The methodology of strain engineering is applied in a high degree of detail to form different sorts of nanostructures (nanodots, nanowires) of the oxide CeO2 with fluorite structure which then is used as a model system to identify the principles controlling self-assembly and self-organization in CSD grown oxides. We also present, more briefly, the application of these ideas to other oxides such as manganites or BaZrO3. We will show that the nucleation and growth steps are essentially understood and manipulated while the kinetic phenomena underlying the evolution of the self-organized networks are still less widely explored, even if very appealing effects have been already observed. Overall, our investigation based on a CSD approach has opened a new strategy towards a general use of self-assembly and self-organization which can now be widely spread to many functional oxide materials.

  7. Oxidation resistant high temperature thermal cycling resistant coatings on silicon-based substrates and process for the production thereof

    DOEpatents

    Sarin, V.K.

    1990-08-21

    An oxidation resistant, high temperature thermal cycling resistant coated ceramic article for ceramic heat engine applications is disclosed. The substrate is a silicon-based material, i.e. a silicon nitride- or silicon carbide-based monolithic or composite material. The coating is a graded coating of at least two layers: an intermediate AlN or Al[sub x]N[sub y]O[sub z] layer and an aluminum oxide or zirconium oxide outer layer. The composition of the coating changes gradually from that of the substrate to that of the AlN or Al[sub x]N[sub y]O[sub z] layer and further to the composition of the aluminum oxide or zirconium oxide outer layer. Other layers may be deposited over the aluminum oxide layer. A CVD process for depositing the graded coating on the substrate is also disclosed.

  8. Oxidation resistant high temperature thermal cycling resistant coatings on silicon-based substrates and process for the production thereof

    DOEpatents

    Sarin, Vinod K.

    1990-01-01

    An oxidation resistant, high temperature thermal cycling resistant coated ceramic article for ceramic heat engine applications. The substrate is a silicon-based material, i.e. a silicon nitride- or silicon carbide-based monolithic or composite material. The coating is a graded coating of at least two layers: an intermediate AlN or Al.sub.x N.sub.y O.sub.z layer and an aluminum oxide or zirconium oxide outer layer. The composition of the coating changes gradually from that of the substrate to that of the AlN or Al.sub.x N.sub.y O.sub.z layer and further to the composition of the aluminum oxide or zirconium oxide outer layer. Other layers may be deposited over the aluminum oxide layer. A CVD process for depositing the graded coating on the substrate is also disclosed.

  9. Effects of compositional changes on the performance of a thermal barrier coating system. [for aircraft gas turbine engines

    NASA Technical Reports Server (NTRS)

    Stecura, S.

    1979-01-01

    Systems consisting of Ni-base bond coatings containing about 16Cr, 6Al, and from 0.15 to 1.08Y (all in wt %) and zirconium oxide layers containing from 4.0 to 24.4Y2O3 were evaluated for suitability as thermal barrier systems for advanced aircraft gas turbine engine components. The evaluations were performed in a cyclic furnace between 990 and 280 C as well as between 1095 and 280 C on solid specimens; in a natural gas-oxygen torch rig between about 1200 and 100 C on solid specimens and up to 1580 C surface temperatures on air-cooled blades; and in a Mach 1.0 burner rig up to 1570 C surface temperatures on air-cooled blades. The data indicate that the best systems consist of combinations involving the Ni-16.4Cr-5.1Al-0.15Y and Ni-17.0Cr-5.4Al-0.35Y bond coatings and the 6.2Y2O3- and 7.9Y2O3- (all in wt %) stabilized zirconium oxide layers.

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

    Beavin, P. Jr.

    A rapid direct dilution procedure for the estimation of soluble zirconium and a fusion procedure for the determination of total zirconium (soluble and insoluble forms) in cream base concentrates prepared from antiperspirant aerosols are described. The direct dilution procedure involves extraction of soluble zirconium with HCl (55 + 45). The filtered extract is reacted with alizarin red S to form a stable colored complex which is measured spectrophotometrically. The fusion procedure involves ashing the aerosol concentrate followed by fusion of the ash with potassium pyrosulfate to form an acid-soluble melt. Zirconium is precipitated from solution as the hydroxide and washedmore » to eliminate interfering ions, particularly sulfate. After redissolving in HCl (55 + 45) and reacting with alizarin red S, total zirconium is measured. Zirconyl chloride octahydrate, assayed gravimetrically by hydroxide precipitation and conversion to the oxide, is used as the zirconium reference standard. Concentration range of zirconium measured was 200 to 500 ..mu..g/100 ml. Recoveries of standard zirconium added to commercial aerosols labeled to contain aluminum and zirconyl hydroxychlorides ranged from 97 to 101 percent by the fusion procedure. Analysis of these aerosols by direct dilution gave generally slightly lower results than by fusion.« less

  11. Preparation of lead-zirconium-titanium film and powder by electrodeposition

    DOEpatents

    Bhattacharya, Raghu N.; Ginley, David S.

    1995-01-01

    A process for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications.

  12. Preparation of lead-zirconium-titanium film and powder by electrodeposition

    DOEpatents

    Bhattacharya, R.N.; Ginley, D.S.

    1995-10-31

    A process is disclosed for the preparation of lead-zirconium-titanium (PZT) film and powder compositions. The process comprises the steps of providing an electrodeposition bath, providing soluble salts of lead, zirconium and titanium metals to this bath, electrically energizing the bath to thereby direct ions of each respective metal to a substrate electrode and cause formation of metallic particles as a recoverable film of PZT powder on the electrode, and also recovering the resultant film as a powder. Recovery of the PZT powder can be accomplished by continually energizing the bath to thereby cause powder initially deposited on the substrate-electrode to drop therefrom into the bath from which it is subsequently removed. A second recovery alternative comprises energizing the bath for a period of time sufficient to cause PZT powder deposition on the substrate-electrode only, from which it is subsequently recovered. PZT film and powder so produced can be employed directly in electronic applications, or the film and powder can be subsequently oxidized as by an annealing process to thereby produce lead-zirconium-titanium oxide for use in electronic applications. 4 figs.

  13. Enhanced pinning in YBCO films with BaZrO.sub.3 nanoparticles

    DOEpatents

    Driscoll, Judith L.; Foltyn, Stephen R.

    2010-06-15

    A process and composition of matter are provided and involve flux pinning in thin films of high temperature superconductive oxides such as YBCO by inclusion of particles including barium and a group 4 or group 5 metal, such as zirconium, in the thin film.

  14. Raman spectroscopy analysis of air grown oxide scale developed on pure zirconium substrate

    NASA Astrophysics Data System (ADS)

    Kurpaska, L.; Favergeon, J.; Lahoche, L.; El-Marssi, M.; Grosseau Poussard, J.-L.; Moulin, G.; Roelandt, J.-M.

    2015-11-01

    Using Raman spectroscopy technique, external and internal parts of zirconia oxide films developed at 500 °C and 600 °C on pure zirconium substrate under air at normal atmospheric pressure have been examined. Comparison of Raman peak positions of tetragonal and monoclinic zirconia phases, recorded during the oxide growth at elevated temperature, and after cooling at room temperature have been presented. Subsequently, Raman peak positions (or shifts) were interpreted in relation with the stress evolution in the growing zirconia scale, especially closed to the metal/oxide interface, where the influence of compressive stress in the oxide is the biggest. Reported results, for the first time show the presence of a continuous layer of tetragonal zirconia phase developed in the proximity of pure zirconium substrate. Based on the Raman peak positions we prove that this tetragonal layer is stabilized by the high compressive stress and sub-stoichiometry level. Presence of the tetragonal phase located in the outer part of the scale have been confirmed, yet its Raman characteristics suggest a stress-free tetragonal phase, therefore different type of stabilization mechanism. Presented study suggest that its stabilization could be related to the lattice defects introduced by highstoichiometry of zirconia or presence of heterovalent cations.

  15. Nickel aluminides and nickel-iron aluminides for use in oxidizing environments

    DOEpatents

    Liu, Chain T.

    1988-03-15

    Nickel aluminides and nickel-iron aluminides treated with hafnium or zirconium, boron and cerium to which have been added chromium to significantly improve high temperature ductility, creep resistance and oxidation properties in oxidizing environments.

  16. Oxidation behaviour of zirconium alloys and their precipitates - A mechanistic study

    NASA Astrophysics Data System (ADS)

    Proff, C.; Abolhassani, S.; Lemaignan, C.

    2013-01-01

    The precipitate oxidation behaviour of binary zirconium alloys containing 1 wt.% Fe, Ni, Cr or 0.6 wt.% Nb was characterised in TEM on FIB prepared transverse sections of the oxide and reported in previous studies [1,2]. In the present study the following alloys: Zr1%Cu, Zr0.5%Cu0.5%Mo and pure Zr are analysed to add to the available information. In all cases, the observed precipitate oxidation behaviour in the oxide close to the metal-oxide interface could be described either with delayed oxidation with respect to the matrix or simultaneous oxidation as the surrounding zirconium matrix. Attempt was made to explain these observations, with different parameters such as precipitate size and structure, composition and thermodynamic properties. It was concluded that the thermodynamics with the new approach presented could explain most precisely their behaviour, considering the precipitate stoichiometry and the free energy of oxidation of the constituting elements. The surface topography of the oxidised materials, as well as the microstructure of the oxide presenting microcracks have been examined. A systematic presence of microcracks above the precipitates exhibiting delayed oxidation has been found; the height of these crack calculated using the Pilling-Bedworth ratios of different phases present, can explain their origin. The protrusions at the surface in the case of materials containing large precipitates can be unambiguously correlated to the presence of these latter, and the height can be correlated to the Pilling-Bedworth ratios of the phases present as well as the diffusion of the alloying elements to the surface and their subsequent oxidation. This latter behaviour was much more considerable in the case of Fe and Cu with Fe showing systematically diffusion to the outer surface.

  17. Doping and defect structure of mixed-conducting ceramics for gas separation

    NASA Astrophysics Data System (ADS)

    Zuo, Chendong

    A worldwide energy crisis and increasing environmental concerns are strong incentives for using hydrogen as a sustainable and clean energy source. "Hydrogen economy" has been around since 1970s, but it started to look practicable only in recent years. The trend in the future is to switch from using hydrogen as the basic raw material in the chemical industry to the energy carrier in the transportation and distributed energy industries. To meet the expected rising demand, hydrogen has to be generated in a more cost-effective manner. As one of the most important operation units in the hydrogen production, a high performance hydrogen separation membrane system is essential to the coming hydrogen economy. The project of hydrogen separation membrane based on Mixed ionic and electronic conductor (MIEC) composite was initiated by DoE years ago, and the MIEC membrane has been developed in Argonne National Laboratory (ANL) for several years. The goal at ANL is to develop a dense, ceramic-based MIEC membrane that is highly selective, chemical stable in practical environments at operative temperatures up to ≈900°C, and can separate hydrogen from mixed gases at commercially significant fluxes under industrially relevant operating conditions, without the need for electrodes or electrical circuitry. The effort at ANL initially focused on BCY20 (BaCe0.8Y 0.2O3). BCY20 forms the matrix of ANL-1a and -2a ceramic-metal composite membranes (40-50 vol.% of a metal is dispersed in a ceramic matrix) and its bulk transport properties, including ionic transfer number, ionic and electronic conductivity, and chemical and mechanical stability have been systematically studied. However, exposure to CO2 and H2O-containing atmospheres, as would be present in a practical environment, will degrade the material as it reacts to form insulating barium carbonate (BaCO3 ) and cerium oxide (CeO2). This decomposition greatly limits its applicability in hydrogen separation, despite the promising properties of this material. The combination of high proton conductivity and good chemical stability, which is a prerequisite for the application of MIEC compounds, is generally considered to be a key problem. In choosing good materials for H2 separation membrane, defect structure, and hence transport properties of perovskites, which are strongly influenced by the oxidation states and ionic radii of dopants, are very critical. Therefore it is the goal of this research to gain a fundamental understanding of the correlation between the defect chemistry and the properties of perovskite structure materials, so as to allow the engineering of these materials with the desired properties for the application in industry, such as developing membranes of mixed conductors which have good stability in practical atmospheres. With respect to thermodynamic stability, water solubility limit and mobility of protonic defects the occupation of the A-site does not require much of a compromise. Except for the stability with acidic gases, which is almost independent of the choice of the A-cation, all relevant properties are superior for an A-site occupation by the big barium compared to other alkaline earth ions. Addition of acceptor dopants into ABO3 is crucial to proton uptake. A high concentration of protonic defects requires a high acceptor dopants concentration. Dopants are incorporated into the lattice at either A or B-sites with the respective creation of charge-compensating oxygen vacancies and A-site vacancies. Smaller dopants preferentially substitute at the B-site, while larger cations substitute at the A-site. Partial occupation of the A sublattice can explain the low uptake of protons. The yttrium seems to be perfect acceptor dopant choice for BaZrO3, BaCeO3-based materials, and both the proton mobility and the thermodynamics of hydration are practically unchanged for dopant levels up to 20% Y. The choice of the B-cation, however, requires some compromising. It should be of medium size. High packing densities as a result of small B-cations reduce the water solubility limit, while though the high proton mobilities are compatible with loosely packed structure; the poor compatibility of big B-cations with the perovskite structure reduces the thermodynamic stability including the stability in acidic gases. Empirically high chemical stability and high proton conductivity still seem to exclude one another for simple alkaline earth perovskites. But there is seemingly still room for discoveries among 'old and new' oxide material. We are investigating various possible alternatives to BCY based on the understanding of defect chemistry of doped perovskite structure materials. BCY20 is one of the best proton conductors among this class of conductors, however, not stable in the CO2, H2O-containing atmospheres. In contrast, yttrium-doped barium zirconates have good chemical stability but are undesirable because of their relatively low conductivity and high sintering temperature. Since BaCeO3 and BaZrO3 can easily form solid solutions, it is possible to replace any desired fraction of the Ce in BaCeO3 with Zr, and the solid solution between cerate and zirconate has both high protonic conductivity and good chemical stability. BZCY proton conductors with various compositions (0.0≤x≤0.8) have been synthesized and characterized. The absence of low-angle supercell reflections indicates a random B-site cation distribution. The substitution of Zr led to a decrease in cell volume and an enhanced structural stability against reactions with CO2. The total conductivity for BZCY pellets of all composition increased with temperature increased and decreased as the zirconium content increased from 10% to 40% at each fixed temperature in wet 4% H2/N2 atmosphere. BZCY7 [Ba(Zr0.1Ce 0.7Y0.2)O3] showed pronounced proton conduction within the bulk and along the grain boundaries. Total conductivity increased from 0.015 S/cm at 550°C to 0.043 S/cm at 850°C for BZCY7 smaple, which is highest among all Ba(Zr0.8-xCexY0.2)O 3 (0.4≤x≤0.7) compositions. However, the relatively low electronic conductivity is not adequate for the hydrogen separation membrane to be used in a non-galvanic operation mode, electronic conduction must been introduced into the proton conductor to create mixed ionic-electronic conductors. Dense Ni-BZCY [Ni-Ba(Zr0.8-xCexY0.2)O 3-alpha] cermet composite membranes have been successfully fabricated for evaluating hydrogen permeability, and stability. Nickel phase enhances the hydrogen permeability of the ceramic phase by increasing the electronic conductivity of the composite, surface exchange kinetics, and improving mechanical stability. By comparing the BEI images of BZCY cermets with different Zirconium content, we can tell the grain size, shape and distribution of two phases are insensitive to the zirconium content. Doping Zirconium in the B-site only slightly reduced the hydrogen permeation at high temperatures (e.g. 900°C), but dramatically increased the chemical stability in CO2- and H2O-containing gases. The hydrogen permeation fluxes of Ni-BZCY cermet membrane increased with temperature for all the compositions and the flux decreased as the zirconium content increased at each fixed temperature, but they are comparable to that of Ni-BCY for the lower zirconium content samples (x=0.6, 0.7). While the hydrogen permeation flux through a Ni-BCY cermet membrane decreased sharply upon exposure to wet CO2 atmospheres, the hydrogen permeation flux of a Ni-BZCY was relatively stable for 80 h in atmospheres containing up to 30% CO2 at 900°C after a small initial decrease. Among the compositions studied (0.4≤x≤0.7), the Ni-BZCY7 (x=0.7) composition exhibited both highest H2 permeation rate and good chemistry stability, thus having potential for practical applications. The Ni-BZCY7 membrane was chose to further study based on the best overall performance. The hydrogen flux through a Ni-BZCY7 cermet membrane increased with temperature under both dry and wet conditions. The fact of increasing hydrogen flux by adding moisture to the feed gas or increasing the hydrogen partial pressure gradient across the membrane implies that the hydrogen flux through the Ni-BZCY7 cermet membrane is limited by the proton transport through the ceramic BZCY7 phase. The dependence of hydrogen flux on membrane thickness indicates that the flux is limited by the bulk diffusion of hydrogen through the ceramic phase over the range of thicknesses that were studied (0.25-1.0 mm). Although interfacial reactions are expected to become important for thinner membranes, these results suggest that we can further increase the hydrogen flux by decreasing the membrane thickness. The highest measured hydrogen flux was 0.805 cm3/min-cm 2 for a dense 266-mum-thick membrane at 900°C using 100% H 2 as the feed gas. The hydrogen fluxes through membrane were stable, after a small initial decrease, for 80 h in atmospheres containing up to 30% CO2 at 900°C, implying that Ni-BZCY7 membranes might be suitable for practical applications.

  18. Effects of surface stability on the morphological transformation of metals and metal oxides as investigated by first-principles calculations.

    PubMed

    Andrés, Juan; Gracia, Lourdes; Gouveia, Amanda Fernandes; Ferrer, Mateus Meneghetti; Longo, Elson

    2015-10-09

    Morphology is a key property of materials. Owing to their precise structure and morphology, crystals and nanocrystals provide excellent model systems for joint experimental and theoretical investigations into surface-related properties. Faceted polyhedral crystals and nanocrystals expose well-defined crystallographic planes depending on the synthesis method, which allow for thoughtful investigations into structure-reactivity relationships under practical conditions. This feature article introduces recent work, based on the combined use of experimental findings and first-principles calculations, to provide deeper knowledge of the electronic, structural, and energetic properties controlling the morphology and the transformation mechanisms of different metals and metal oxides: Ag, anatase TiO2, BaZrO3, and α-Ag2WO4. According to the Wulff theorem, the equilibrium shapes of these systems are obtained from the values of their respective surface energies. These investigations are useful to gain further understanding of how to achieve morphological control of complex three-dimensional crystals by tuning the ratio of the surface energy values of the different facets. This strategy allows the prediction of possible morphologies for a crystal and/or nanocrystal by controlling the relative values of surface energies.

  19. Oxidized zirconium versus cobalt-chromium against the native patella in total knee arthroplasty: Patellofemoral outcomes.

    PubMed

    Matassi, Fabrizio; Paoli, Tommaso; Civinini, Roberto; Carulli, Christian; Innocenti, Massimo

    2017-10-01

    Oxidized zirconium (OxZr) has demonstrated excellent mechanical properties in vitro when used against articular cartilage; less coefficient of friction and less chondral damage have been found when compared with cobalt-chromium (CoCr) implants. However, controversy exists as to whether implants with a zirconium femoral component articulate safely with a native patella in total knee arthroplasty (TKA). To answer this question, the clinical and radiographic results were analysed from a group of patients who underwent a TKA with patella retention; the OxZr versus CoCr femoral components were compared. The present study prospectively evaluated 83 knees of 74 patients from 2009 to 2010. Each patient was evaluated clinically (visual analogue scale, Knee Society score, patellar score) and radiographically (long leg standing radiograph, anterior-posterior and latero-lateral projections, axial view of the patella) pre-operatively and postoperatively with a mean follow-up of 4.47years. The patellar tilt and shift, and progression of patellofemoral osteoarthritis were calculated with the axial view. There were no patient reported adverse reactions and none of the evaluated prostheses failed. Both the clinical and radiographic evaluations showed no statistically significant between-group differences. No adverse events were observed clinically or radiologically. These results justify pursuing the use of oxidized zirconium as an alternative bearing surface for a femoral component associated with patellar retention in TKA. Published by Elsevier B.V.

  20. Method of forming dynamic membrane on stainless steel support

    NASA Technical Reports Server (NTRS)

    Gaddis, Joseph L. (Inventor); Brandon, Craig A. (Inventor)

    1988-01-01

    A suitable member formed from sintered, powdered, stainless steel is contacted with a nitrate solution of a soluble alkali metal nitrate and a metal such as zirconium in a pH range and for a time sufficient to effect the formation of a membrane of zirconium oxide preferably including an organic polymeric material such as polyacrylic acid.

  1. Concentration and immobilization of 137Cs from liquid radioactive waste using sorbents based on hydrated titanium and zirconium oxides

    NASA Astrophysics Data System (ADS)

    Voronina, A. V.; Noskova, A. Y.; Gritskevich, E. Y.; Mashkovtsev, M. A.; Semenishchev, V. S.

    2017-09-01

    The possibility of use of sorbents based on hydrated titanium and zirconium oxides (T-3A, T-35, NPF-HTD) for concentration and immobilization of 137Cs from liquid radioactive waste of various chemical composition (fresh water, seawater, solutions containing NaNO3, ammonium acetate, EDTA) was evaluated. It was shown that the NPF-HTD and T-35 sorbents separate 137Cs from fresh water and seawater with distribution coefficients as high as 6.2.104 and 6.1.104, 4.0.105 and 1.6.105 L kg-1 respectively; in 1 M ammonium acetate these values were 2.0.103 and 1.0.103 L kg-1. The NPF-HTD sorbent showed the highest selectivity for cesium in NaNO3 solution: cesium distribution coefficients in 1M NaNO3 was 1.4.106 L kg-1. All studied sorbents are suitable for deactivation of solutions containing EDTA. Cesium distribution coefficients were around 102-103 L kg-1 depending on EDTA concentration. Chemical stability of the sorbents was also studied. It was shown that 137Cs leaching rate from all sorbents meet the requirements for matrix materials.

  2. Zirconium oxide nanotube-Nafion composite as high performance membrane for all vanadium redox flow battery

    NASA Astrophysics Data System (ADS)

    Aziz, Md. Abdul; Shanmugam, Sangaraju

    2017-01-01

    A high-performance composite membrane for vanadium redox flow battery (VRB) consisting of ZrO2 nanotubes (ZrNT) and perfluorosulfonic acid (Nafion) was fabricated. The VRB operated with a composite (Nafion-ZrNT) membrane showed the improved ion-selectivity (ratio of proton conductivity to permeability), low self-discharge rate, high discharge capacity and high energy efficiency in comparison with a pristine commercial Nafion-117 membrane. The incorporation of zirconium oxide nanotubes in the Nafion matrix exhibits high proton conductivity (95.2 mS cm-1) and high oxidative stability (99.9%). The Nafion-ZrNT composite membrane exhibited low vanadium ion permeability (3.2 × 10-9 cm2 min-1) and superior ion selectivity (2.95 × 107 S min cm-3). The VRB constructed with a Nafion-ZrNT composite membrane has lower self-discharge rate maintaining an open-circuit voltage of 1.3 V for 330 h relative to a pristine Nafion membrane (29 h). The discharge capacity of Nafion-ZrNT membrane (987 mAh) was 3.5-times higher than Nafion-117 membrane (280 mAh) after 100 charge-discharge cycles. These superior properties resulted in higher coulombic and voltage efficiencies with Nafion-ZrNT membranes compared to VRB with Nafion-117 membrane at a 40 mA cm-2 current density.

  3. Preliminary calculations related to the accident at Three Mile Island

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

    Kirchner, W.L.; Stevenson, M.G.

    This report discusses preliminary studies of the Three Mile Island Unit 2 (TMI-2) accident based on available methods and data. The work reported includes: (1) a TRAC base case calculation out to 3 hours into the accident sequence; (2) TRAC parametric calculations, these are the same as the base case except for a single hypothetical change in the system conditions, such as assuming the high pressure injection (HPI) system operated as designed rather than as in the accident; (3) fuel rod cladding failure, cladding oxidation due to zirconium metal-steam reactions, hydrogen release due to cladding oxidation, cladding ballooning, cladding embrittlement,more » and subsequent cladding breakup estimates based on TRAC calculated cladding temperatures and system pressures. Some conclusions of this work are: the TRAC base case accident calculation agrees very well with known system conditions to nearly 3 hours into the accident; the parametric calculations indicate that, loss-of-core cooling was most influenced by the throttling of High-Pressure Injection (HPI) flows, given the accident initiating events and the pressurizer electromagnetic-operated valve (EMOV) failing to close as designed; failure of nearly all the rods and gaseous fission product gas release from the failed rods is predicted to have occurred at about 2 hours and 30 minutes; cladding oxidation (zirconium-steam reaction) up to 3 hours resulted in the production of approximately 40 kilograms of hydrogen.« less

  4. A study into the impact of interface roughness development on mechanical degradation of oxides formed on zirconium alloys

    NASA Astrophysics Data System (ADS)

    Platt, P.; Wedge, S.; Frankel, P.; Gass, M.; Howells, R.; Preuss, M.

    2015-04-01

    As a cladding material used to encapsulate nuclear fuel pellets, zirconium alloys are the primary barrier separating the fuel and a pressurised steam or lithiated water environment. Degradation mechanisms such as oxidation can be the limiting factor in the life-time of the fuel assembly. Key to controlling oxidation, and therefore allowing increased burn-up of fuel, is the development of a mechanistic understanding of the corrosion process. In an autoclave, the oxidation kinetics for zirconium alloys are typically cyclical, with periods of accelerated kinetics being observed in steps of ∼2 μm oxide growth. These periods of accelerated oxidation are immediately preceded by the development of a layer of lateral cracks near the metal-oxide interface, which may be associated with the development of interface roughness. The present work uses scanning electron microscopy to carry out a statistical analysis of changes in the metal-oxide interface roughness between three different alloys at different stages of autoclave oxidation. The first two alloys are Zircaloy-4 and ZIRLO™ for which analysis is carried out at stages before, during and after first transition. The third alloy is an experimental low tin alloy, which under the same oxidation conditions and during the same time period does not appear to go through transition. Assessment of the metal-oxide interface roughness is primarily carried out based on the root mean square of the interface slope known as the Rdq parameter. Results show clear trends with relation to transition points in the corrosion kinetics. Discussion is given to how this relates to the existing mechanistic understanding of the corrosion process, and the components required for possible future modelling approaches.

  5. Joint Test Protocol: Environmentally Friendly Zirconium Oxide Pretreatment Demonstration

    DTIC Science & Technology

    2013-12-01

    coatings . Loss of paint adhesion is the primary failure mode on aluminum and steel. 3.7.3 Test Methodology The test methodology for pencil hardness...conversion pretreatment coatings . Loss of paint adhesion is the primary failure mode on aluminum and steel. 3.8.3 Test Methodology The test...SUPPLEMENTARY NOTES 14. ABSTRACT There is a need to implement innovative and cost- effective replacement technologies to address the multiple health, safety

  6. Metal Organic Framework-Metal Oxide Composites for Toxic Gas Adsorption and Sensing

    DTIC Science & Technology

    2014-05-01

    zeolitic imidazolate framework Zn(NO3)2 zinc nitrate ZrCl4 zirconium chloride 21 SUMMARY Metal organic frameworks (MOFs) and metal oxide-MOF...performed better for the other gases and conditions. Compared to the standard adsorbents BPL carbon and zeolite 13X, the cobalt and magnesium MOF...g)24 and zeolite 5A (1.25 mmol/g),25 compared to 3.5 mmol/g for Ni-MOF-74, 4 mmol/g for Mg-MOF-74, and 6 mmol/g for Co-MOF-74. Mg-MOF-74 shows the

  7. Synthesis of ultrafine ZrB2 powders by sol-gel process

    NASA Astrophysics Data System (ADS)

    Yang, Li-Juan; Zhu, Shi-Zhen; Xu, Qiang; Yan, Zhen-Yu; Liu, Ling

    2010-09-01

    Ultrafine zirconium diboride (ZrB2) powders have been synthesized by sol-gel process using zirconium oxychloride (ZrOCl2·8H2O), boric acid (H3BO3) and phenolic resin as sources of zirconia, boron oxide and carbon, respectively. The effects of the reaction temperature, B/Zr ratio, holding time, and EtOH/H2O ratio on properties of the synthesized ZrB2 powders were investigated. It was revealed that ultrafine (average crystallite size between 100 and 400 nm) ZrB2 powders can be synthesized with the optimum processing parameters as follows: (i) the ratio of B/Zr is 4; (ii) the solvent is pure ethanol; (iii) the condition of carbothermal reduction heat treatment is at 1550°C for 20 min.

  8. Wear Analysis in THA Utilizing Oxidized Zirconium and Crosslinked Polyethylene

    PubMed Central

    Garvin, Kevin L.; Mangla, Jimmi; Murdoch, Nathan; Martell, John M.

    2008-01-01

    Oxidized zirconium, a material with a ceramic surface on a metal substrate, and highly cross-linked polyethylene are two materials developed to reduce wear. We measured in vivo femoral head penetration in patients with these advanced bearings. We hypothesized the linear wear rates would be lower than those published for cobalt-chrome and standard polyethylene. We retrospectively reviewed a select series of 56 THAs in a relatively young, active patient population utilizing oxidized zirconium femoral heads and highly cross-linked polyethylene acetabular liners. Femoral head penetration was determined using the Martell computerized edge-detection method. All patients were available for 2-year clinical and radiographic followup. True linear wear was 4 μm/year (95% confidence intervals, ± 59 μm/year). The early wear rates in this cohort of relatively young, active patients were low and we believe justify the continued study of these alternative bearing surfaces. Level of Evidence: Level IV, therapeutic study. See the Guidelines for Authors for a complete description of levels of evidence. PMID:18946711

  9. 77 FR 52765 - Dominion Nuclear Connecticut, Inc. Millstone Power Station, Unit 3; Exemption

    Federal Register 2010, 2011, 2012, 2013, 2014

    2012-08-30

    ... energy release, hydrogen generation, and cladding oxidation from the metal/water reaction to be calculated using the Baker-Just equation (Baker, L., Just, L.C., ``Studies of Metal Water Reactions at High Temperatures, III. Experimental and Theoretical Studies of the Zirconium-Water Reaction,'' ANL-6548, page 7...

  10. Facile Synthesis and Characterization of ZrO₂ Nanoparticles via Modified Co-Precipitation Method.

    PubMed

    Ramachandran, M; Subadevi, R; Liu, Wei-Ren; Sivakumar, M

    2018-01-01

    The crystalline Zirconium oxide (ZrO2) nano particles were synthesized using optimized content of Zirconium nitrate (Zr(NO3)2·3H2O) with varying KOH concentration (0.5, 1 and 1.5 M) by co-precipitation method. The thermal history of the precursor was carefully analyzed through Thermogravimetric (TG/DTA) measurement. The as prepared samples were characterized to ensure structural, functional, morphological, compositional, chemical composition and band gap by X-ray diffractometer (XRD), Fourier transform infrared spectroscopy (FTIR), Laser Raman, scanning electron microscopy (SEM), High resolution Transverse Electron Microscopy (HR-TEM), X-ray photo electron spectroscopy (XPS), EDX, Photo luminescence spectroscopy (PL). The monoclinic structure with space group P21/c has been confirmed from XRD (JCPDS 89-9066). The Zr-O stretching vibration and Zr-O2-Zr bending vibrations were confirmed through FTIR analysis. The well dispersed particles with spherical morphology were confirmed through SEM and TEM analysis. The oxidation states of Zr, O and C were confirmed through XPS analysis. The oxygen vacancies and band gap of the particles were investigated through PL analysis.

  11. On the determination of growth stress during oxidation of pure zirconium at elevated temperature

    NASA Astrophysics Data System (ADS)

    Kurpaska, L.; Favergeon, J.; Lahoche, L.; Moulin, G.

    2018-07-01

    An experimental approach have been proposed to evaluate growth of stress during high temperature oxidation of pure zirconium. The development of stress in the oxide scale has been investigated experimentally in in-situ conditions by combining the Deflection Test in Monofacial Oxidation (DTMO) with Acoustic Emission analysis (AE). Microstructure of the sample were studied by using Scanning Electron Microscopy technique. Oxidation experiments were performed continuously during 24 h at 400 °C and 500 °C in air under normal atmospheric pressure. Taking into account purely elastic behaviour of the material, primary evolution of growth stress developed in the oxide scale during oxidation process have been estimated. Presented study of the Zr/ZrO2 system revealed two opposite phenomena of stress relief when cooling from 400 °C and 500 °C to room temperature. This study is presented as a tool to understand the phenomena of stress evolution in the zirconia layer during isothermal treatment at high temperature and after cooling.

  12. Structural properties of zirconia - in-situ high temperature XRD characterization

    NASA Astrophysics Data System (ADS)

    Kurpaska, Lukasz

    2018-07-01

    In this work, the effect of high temperature on structural properties of pure zirconium have been investigated. In-situ X-ray diffraction analysis of the oxide layer formed at temperature window 25-600 °C on pure zirconium were performed. Conducted experiment aimed at investigation of the zirconia phases developed on surface of the metallic substrate. Based on the conducted studies, possible stress state (during heating, continuous oxidation and cooling), cell parameters and HWHM factor were analyzed. A tetragonal and monoclinic phases peak shifts and intensities change were observed, suggesting that different phases react in different way upon temperature effect.

  13. Zirconium-modified materials for selective adsorption and removal of aqueous arsenic

    DOEpatents

    Zhao, Hongting; Moore, Robert C.

    2004-11-30

    A method, composition, and apparatus for removing contaminant species from an aqueous medium comprising: providing a material to which zirconium has been added, the material selected from one or more of zeolites, cation-exchangeable clay minerals, fly ash, mesostructured materials, activated carbons, cellulose acetate, and like porous and/or fibrous materials; and contacting the aqueous medium with the material to which zirconium has been added. The invention operates on all arsenic species in the form of arsenate, arsenite and organometallic arsenic, with no pretreatment necessary (e.g., oxidative conversion of arsenite to arsenate).

  14. Synthesis and Characterization of a Perovskite Barium Zirconate (BaZrO[subscript 3]): An Experiment for an Advanced Inorganic Chemistry Laboratory

    ERIC Educational Resources Information Center

    Thananatthanachon, Todsapon

    2016-01-01

    In this experiment, the students explore the synthesis of a crystalline solid-state material, barium zirconate (BaZrO3) by two different synthetic methods: (a) the wet chemical method using BaCl[subscript 2]·2H[subscript 2]O and ZrOCl[subscript 2]·8H[subscript 2]O as the precursors, and (b) the solid-state reaction from BaCO[subscript 3] and…

  15. Monochloro non-bridged half-metallocene-type zirconium complexes containing phosphine oxide-(thio)phenolate chelating ligands as efficient ethylene polymerization catalysts.

    PubMed

    Tang, Xiao-Yan; Wang, Yong-Xia; Liu, San-Rong; Liu, Jing-Yu; Li, Yue-Sheng

    2013-01-14

    A series of novel monochloro half-zirconocene complexes containing phosphine oxide-(thio)phenolate chelating ligands of the type, ClCp'Zr[X-2-R(1)-4-R(2)-6-(Ph(2)P=O)C(6)H(2)](2) (Cp' = C(5)H(5), 2a: X = O, R(1) = Ph, R(2) = H; 2b: X = O, R(1) = F, R(2) = H; 2c: X = O, R(1) = (t)Bu, R(2) = H; 2d: X = O, R(1) = R(2) = (t)Bu; 2e: X = O, R(1) = SiMe(3), R(2) = H; 2f: X = S, R(1) = SiMe(3), R(2) = H; Cp' = C(5)Me(5), 2g: X = O, R(1) = SiMe(3), R(2) = H), have been synthesized in high yields. These complexes were identified by (1)H {(13)C} NMR and elemental analyses. Structures for 2b, 2c and 2f were further confirmed by X-ray crystallography. Structural characterization of these complexes reveals crowded environments around the zirconium. Complexes 2b and 2c adopt six-coordinate, distorted octahedral geometry around the zirconium center, in which the equatorial positions are occupied by three oxygen atoms of two chelating phosphine oxide-bridged phenolate ligands and a chlorine atom. The cyclopentadienyl ring and one oxygen atom of the ligand are coordinated on the axial position. Complex 2f also folds a six-coordinate, distorted octahedral geometry around the Zr center, consisting of a Cp-Zr-O (in P=O) axis [177.16°] and a distorted plane of two sulfur atoms and one oxygen atom of two chelating phosphine oxide-bridged thiophenolate ligands as well as a chlorine atom. When activated by modified methylaluminoxane (MMAO), all the complexes exhibited high activities towards ethylene polymerization at high temperature (75 °C), giving high molecular weight polymers with unimodal molecular weight distribution. The formation of 14-electron, cationic metal alkyl species might come from the Zr-O (in phenol ring) bond cleavage based on the DFT calculations study.

  16. Nanoscale Zirconium-(oxyhydr)oxide in Contaminated Sediments From Hanford, WA - A New Host for Uranium

    NASA Astrophysics Data System (ADS)

    Stubbs, J. E.; Elbert, D. C.; Veblen, L. A.; Zachara, J. M.; Davis, J. A.; Veblen, D. R.

    2008-12-01

    Zirconium-, uranium-, and copper-bearing wastes have leached from former disposal ponds into vadose zone sediments in the 300 Area at the Department of Energy's Hanford Site. Zirconium is enriched in the shallow portion of the vadose zone, and we have discovered an amorphous Zr-(oxyhydr)oxide that contains 16% of the total uranium budget (84.24 ppm) in one of the shallow samples. We have characterized the oxide using electron microprobe analysis (EMPA), a focused ion beam (FIB) instrument, and transmission electron microscopy (TEM). It occurs in fine-grained coatings found on lithic and mineral fragments in these sediments. The oxide is intimately intergrown with the phyllosilicates and other minerals of the coatings, and in places can be seen coating individual, nano-sized phyllosilicate mineral grains. Electron energy-loss spectroscopy (EELS) shows that the Zr-(oxyhydr)oxide has a P:Zr atomic ratio around 0.2, suggesting it is either intergrown with minor amounts of a Zr-phosphate or has adsorbed a significant amount of phosphate. This material has adsorbed or incorporated a substantial amount of uranium. Thus, understanding its nature is critical to predicting the long-term fate of U in the Hanford vadose zone. While the low-temperature uptake of U by Zr-(oxhydr)oxides and phosphates has been studied for several decades in laboratory settings, to our knowledge ours is the first report of such uptake in the field.

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

    Ikeuchi, Hirotomo; Yano, Kimihiko; Kaji, Naoya

    For the decommissioning of the Fukushima-Daiichi Nuclear Power Station (1F), the characterization of fuel-debris in cores of Units 1-3 is necessary. In this study, typical phases of the in-vessel fuel-debris were estimated using a thermodynamic equilibrium (TDE) calculation. The FactSage program and NUCLEA database were applied to estimate the phase equilibria of debris. It was confirmed that the TDE calculation using the database can reproduce the phase separation behavior of debris observed in the Three Mile Island accident. In the TDE calculation of 1F, the oxygen potential [G(O{sub 2})] was assumed to be a variable. At low G(O{sub 2}) wheremore » metallic zirconium remains, (U,Zr)O{sub 2}, UO{sub 2}, and ZrO{sub 2} were found as oxides, and oxygen-dispersed Zr, Fe{sub 2}(Zr,U), and Fe{sub 3}UZr{sub 2} were found as metals. With an increase in zirconium oxidation, the mass of those metals, especially Fe{sub 3}UZr{sub 2}, decreased, but the other phases of metals hardly changed qualitatively. Consequently, (U,Zr)O{sub 2} is suggested as a typical phase of oxide, and Fe{sub 2}(Zr,U) is suggested as that of metal. However, a more detailed estimation is necessary to consider the distribution of Fe in the reactor pressure vessel through core-melt progression. (authors)« less

  18. Effect of surface treatments on the bond strength between resin cement and differently sintered zirconium-oxide ceramics.

    PubMed

    Yenisey, Murat; Dede, Doğu Ömür; Rona, Nergiz

    2016-01-01

    This study investigated the effects of surface treatments on bond strength between resin cement and differently sintered zirconium-oxide ceramics. 220 zirconium-oxide ceramic (Ceramill ZI) specimens were prepared, sintered in two different period (Short=Ss, Long=Ls) and divided into ten treatment groups as: GC, no treatment; GSil, silanized (ESPE-Sil); GSilPen, silane flame treatment (Silano-Pen); GSb, sandblasted; GSbSil, sandblasted+silanized; GSbCoSil, sandblasted+silica coated (CoJet)+silanized; GSbRoSil, sandblasted+silica coated (Rocatech-Plus)+silanized; GSbDSil, sandblasted+diamond particle abraded (Micron MDA)+silanized; GSbSilPen, sandblasted+silane flame treatment+silanized; GSbLSil, sandblasted+Er:Yag (Asclepion-MCL30) laser treated+silanized. The composite resin (Filtek Z-250) cylinders were cemented to the treated ceramic surfaces with a resin cement (Panavia F2.0). Shear bond strength test was performed after specimens were stored in water for 24h and thermo-cycled for 6000 cycles (5-55 °C). Data were statistically analyzed with two-way analysis of variance (ANOVA) and Tamhane's multiple comparison test (α=0.05). According to the ANOVA, sintering time, surface treatments and their interaction were statistically significant (p<0.05). The highest bond strengths were obtained in GSbCoSil (Ss=13.36/Ls=11.19MPa) and lowest values were obtained in GC (Ss=4.70/Ls=4.62 MPa) for both sinter groups. Sintering time may be effective on the bond strength and 30 μm silica coating (Cojet) with silane coupling application technique increased the bond strength between resin cement and differently sintered zirconium-oxide ceramics. Copyright © 2015 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

  19. Influence of chemical composition of zirconium alloy E110 on embrittlement under LOCA conditions - Part 1: Oxidation kinetics and macrocharacteristics of structure and fracture

    NASA Astrophysics Data System (ADS)

    Nikulin, S. A.; Rozhnov, A. B.; Belov, V. A.; Li, E. V.; Glazkina, V. S.

    2011-11-01

    Exploratory investigations of the influence of alloying and impurity content in the E110 alloy cladding tubes on the behavior under conditions of Loss of Coolant Accidents (LOCA) has been performed. Three alloys of E110 type have been tested: E110 alloy of nominal composition Zr-1%Nb (E110), E110 alloy of modified composition Zr-1%Nb-0.12%Fe-0.13%O (E110M), E110 alloy of nominal composition Zr-1%Nb with reduced impurity content (E110G). Alloys E110 and E110M were manufactured on the electrolytic basis and alloy E110G was manufactured on the basis of zirconium sponge. The high temperature oxidation tests in steam ( T = 1100 °C, 18% of equivalent cladding reacted (ECR)) have been conducted, kinetics of oxidation was investigated. Quantitative research of structure and fracture macrocharacteristics was performed by means of optical and electron microscopy. The results received were compared with the residual ductility of specimens. The results of the investigation showed the existence of "breakaway oxidation" kinetics and white spalling oxide in E110 and E110M alloys while the specimen oxidation kinetics in E110G alloy was characterized by a parabolic law and specimens had a dense black oxide. Oxygen and iron alloying in the E110 alloy positively changed the macrocharacteristics of structure and fracture. However, in general, it did not improve the resistance to embrittlement in LOCA conditions apparently because of a strong impurity influence caused by electrolytic process of zirconium production.

  20. In vitro and in vivo characterization of anodised zirconium as a potential material for biomedical applications.

    PubMed

    Katunar, Maria R; Gomez Sanchez, Andrea; Santos Coquillat, Ana; Civantos, Ana; Martinez Campos, Enrique; Ballarre, Josefina; Vico, Tamara; Baca, Matias; Ramos, Viviana; Cere, Silvia

    2017-06-01

    In vitro studies offer the insights for the understanding of the mechanisms at the tissue-implant interface that will provide an effective functioning in vivo. The good biocompatibility of zirconium makes a good candidate for biomedical applications and the attractive in vivo performance is mainly due to the presence of a protective oxide layer. The aim of this study is to evaluate by in vitro and in vivo approach, the influence of surface modification achieved by anodisation at 30 and 60V on zirconium implants on the first steps of the osseointegration process. In this study cell attachment, proliferation and morphology of mouse myoblast C2C12-GFP and in mouse osteoprogenitor MC3T3-E1 cells was evaluated. Also, together with the immune system response, osteoclast differentiation and morphology with RAW 264.7 murine cell line were analysed. It was found that anodisation treatment at 60V enhanced cell spreading and the osteoblastic and osteoclastic cells morphology, showing a strong dependence on the surface characteristics. In vivo tests were performed in a rat femur osteotomy model. Dynamical and static histological and histomorphometric analyses were developed 15 and 30days after surgery. Newly formed bone around Zr60V implants showed a continuous newly compact and homogeneous bone just 15 after surgery, as judged by the enhanced thickness and mineralization rate. The results indicate that anodising treatment at 60V could be an effective improvement in the osseointegration of zirconium by stimulating adhesion, proliferation, morphology, new bone thickness and bone mineral apposition, making zirconium an emerging candidate material for biomedical applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  1. INTERMEDIATE STAGES OF REACTIONS FORMING CARBIDES OF TITANIUM, ZIRCONIUM, VANADIUM, NIOBIUM, AND TANTALIUM

    DTIC Science & Technology

    Tensimetric examination was made of the formation of the carbides TiC , ZrC, VC, NbC and TaC in a vacuum. During x-ray and chemical analysis of...for obtaining TiC , and ZrC through the stage of intermediate oxides Ti2O3, Ti3O5, TiO and Zr2O3, ZrO, respectively and also for the reaction of

  2. Zirconia in fixed prosthesis. A literature review

    PubMed Central

    Román-Rodríguez, Juan L.; Ferreiroa, Alberto; Solá-Ruíz, María F.; Fons-Font, Antonio

    2014-01-01

    Statement of problem: Evidence is limited on the efficacy of zirconia-based fixed dental prostheses. Objective: To carry out a literature review of the behavior of zirconium oxide dental restorations. Material and Methods: This literature review searched the Pubmed, Scopus, Medline and Cochrane Library databases using key search words “zirconium oxide,” “zirconia,” “non-metal restorations,” “ceramic oxides,” “veneering ceramic,” “zirconia-based fixed dental prostheses”. Both in vivo and in vitro studies into zirconia-based prosthodontic restoration behavior were included. Results: Clinical studies have revealed a high rate of fracture for porcelain-veneered zirconia-based restorations that varies between 6% and 15% over a 3- to 5-year period, while for ceramo-metallic restorations the fracture rate ranges between 4 and 10% over ten years. These results provoke uncertainty as to the long-term prognosis for this material in the oral medium. The cause of veneering porcelain fractures is unknown but hypothetically they could be associated with bond failure between the veneer material and the zirconia sub-structure. Key words:Veneering ceramic, zirconia-based ceramic restoration, crown, zirconia, tooth-supported fixed prosthesis. PMID:24596638

  3. Plasma-sprayed zirconia gas path seal technology: A state-of-the-art review

    NASA Technical Reports Server (NTRS)

    Bill, R. C.

    1979-01-01

    The benefits derived from application of ceramic materials to high pressure turbine gas path seal components are described and the developmental backgrounds of various approaches are reviewed. The most fully developed approaches are those employing plasma sprayed zirconium oxide as the ceramic material. Prevention of cracking and spalling of the zirconium oxide under cyclic thermal shock conditions imposed by the engine operating cycle is the most immediate problem to be solved before implementation is undertaken. Three promising approaches to improving cyclic thermal shock resistance are described and comparative rig performance of each are reviewed. Advanced concepts showing potential for performance improvements are described.

  4. Systematic technology evaluation program for SiC/SiC composite-based accident-tolerant LWR fuel cladding and core structures: Revision 2015

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

    Katoh, Yutai; Terrani, Kurt A.

    2015-08-01

    Fuels and core structures in current light water reactors (LWR’s) are vulnerable to catastrophic failure in severe accidents as unfortunately evidenced by the March 2011 Fukushima Dai-ichi Nuclear Power Plant Accident. This vulnerability is attributed primarily to the rapid oxidation kinetics of zirconium alloys in a water vapor environment at very high temperatures. Zr alloys are the primary material in LWR cores except for the fuel itself. Therefore, alternative materials with reduced oxidation kinetics as compared to zirconium alloys are sought to enable enhanced accident-tolerant fuels and cores.

  5. [Influence of different types of posts and cores on color of IPS-Empress 2 crown].

    PubMed

    Li, Dong-fang; Yang, Jing-yuan; Yang, Xing-mei; Yang, Liu; Xu, Qiang; Guan, Hong-yu; Wan, Qian-bing

    2007-10-01

    To evaluate the influence of different types of posts and cores on the final color of the IPS-Emperss 2 crown. Five types of posts and cores (Cerapost with Empress cosmo, Cerapost with composite resin, gilded Ni-Cr alloy, gold alloy and Ni-Cr alloy) were made. The shifts in color of three points of IPS-Empress 2 crown surface (cervical, middle and incisal) with different posts and cores was measured with a spectroradiometer (PR-650). The L* a* b* values of zirconium oxide and gilded Ni-Cr alloy posts and cores with ceramic crown were the highest. The L* a* values of zirconium oxide posts composite cores were higher while the b* values were lower. The L* a* b* values of Ni-Cr alloy were lower than that of gold alloy and were the lowest. In combination with IPS-Empress 2 crown, zirconium oxide posts are suitable for routine use in the anterior dentition, and gilded Ni-Cr alloy and gold alloy posts and cores can be recommended for clinical practice. Ni-Cr alloy posts and cores can not be recommended for clinical practice.

  6. Evaluation of steam corrosion and water quenching behavior of zirconium-silicide coated LWR fuel claddings

    NASA Astrophysics Data System (ADS)

    Yeom, Hwasung; Lockhart, Cody; Mariani, Robert; Xu, Peng; Corradini, Michael; Sridharan, Kumar

    2018-02-01

    This study investigates steam corrosion of bulk ZrSi2, pure Si, and zirconium-silicide coatings as well as water quenching behavior of ZrSi2 coatings to evaluate its feasibility as a potential accident-tolerant fuel cladding coating material in light water nuclear reactor. The ZrSi2 coating and Zr2Si-ZrSi2 coating were deposited on Zircaloy-4 flats, SiC flats, and cylindrical Zircaloy-4 rodlets using magnetron sputter deposition. Bulk ZrSi2 and pure Si samples showed weight loss after the corrosion test in pure steam at 400 °C and 10.3 MPa for 72 h. Silicon depletion on the ZrSi2 surface during the steam test was related to the surface recession observed in the silicon samples. ZrSi2 coating (∼3.9 μm) pre-oxidized in 700 °C air prevented substrate oxidation but thin porous ZrO2 formed on the coating. The only condition which achieved complete silicon immobilization in the oxide scale in aqueous environments was the formation of ZrSiO4 via ZrSi2 coating oxidation in 1400 °C air. In addition, ZrSi2 coatings were beneficial in enhancing quenching heat transfer - the minimum film boiling temperature increased by 6-8% in the three different environmental conditions tested. During repeated thermal cycles (water quenching from 700 °C to 85 °C for 20 s) performed as a part of quench tests, no spallation and cracking was observed and the coating prevented oxidation of the underlying Zircaloy-4 substrate.

  7. Carbonaceous cathode with enhanced wettability for aluminum production

    DOEpatents

    Keller, Rudolf; Gatty, David G.; Barca, Brian J.

    2003-09-09

    A method of preparing carbonaceous blocks or bodies for use in a cathode in an electrolytic cell for producing aluminum wherein the cell contains an electrolyte and has molten aluminum contacting the cathode, the cathode having improved wettability with molten aluminum. The method comprises the steps of providing a carbonaceous block and a boron oxide containing melt. The carbonaceous block is immersed in the melt and pressure is applied to the melt to impregnate the melt into pores in the block. Thereafter, the carbonaceous block is withdrawn from the melt, the block having boron oxide containing melt intruded into pores therein, the boron oxide capable of reacting with a source of titanium or zirconium or like metal to form titanium or zirconium diboride during heatup or operation of said cell.

  8. Zirconia-molybdenum disilicide composites

    DOEpatents

    Petrovic, John J.; Honnell, Richard E.

    1991-01-01

    Compositions of matter comprised of molybdenum disilicide and zirconium oxide in one of three forms: pure, partially stabilized, or fully stabilized and methods of making the compositions. The stabilized zirconia is crystallographically stabilized by mixing it with yttrium oxide, calcium oxide, cerium oxide, or magnesium oxide and it may be partially stabilized or fully stabilized depending on the amount of stabilizing agent in the mixture.

  9. Composite construction for nuclear fuel containers

    DOEpatents

    Cheng, Bo-Ching [Fremont, CA; Rosenbaum, Herman S [Fremont, CA; Armijo, Joseph S [Saratoga, CA

    1987-01-01

    An improved method for producing nuclear fuel containers of a composite construction having components providing therein a barrier system for resisting destructive action by volatile fission products or impurities and also interdiffusion of metal constituents, and the product thereof. The composite nuclear fuel containers of the method comprise a casing of zirconium or alloy thereof with a layer of copper overlying an oxidized surface portion of the zirconium or alloy thereof.

  10. METHOD FOR DISSOLVING LANTHANUM FLUORIDE CARRIER FOR PLUTONIUM

    DOEpatents

    Koshland, D.E. Jr.; Willard, J.E.

    1961-08-01

    A method is described for dissolving lanthanum fluoride precipitates which is applicable to lanthanum fluoride carrier precipitation processes for recovery of plutonium values from aqueous solutions. The lanthanum fluoride precipitate is contacted with an aqueous acidic solution containing dissolved zirconium in the tetravalent oxidation state. The presence of the zirconium increases the lanthanum fluoride dissolved and makes any tetravalent plutonium present more readily oxidizable to the hexavalent state. (AEC)

  11. Publications - RDF 2005-5 | Alaska Division of Geological & Geophysical

    Science.gov Websites

    content DGGS RDF 2005-5 Publication Details Title: Major-oxide, minor-oxide, and trace-element geochemical ., and Lessard, R.R., 2005, Major-oxide, minor-oxide, and trace-element geochemical data from rocks ; Zinc; Zirconium Top of Page Department of Natural Resources, Division of Geological & Geophysical

  12. Investigation of Ce(3+) Dopant in Appropriate Hosts for Blue Green Lasers.

    DTIC Science & Technology

    1986-11-25

    crystal of La(A10 .8Sc 0 .2 )0 3 doped with 0.01% Ce. During one experiment a small amount of the charge was fused in an iridium crucible. The...from ordering was not observed. Similar results were achieved in Experiment #47 with (LaAlO3 ) 0 .5 (SrZrO 3 )0 5 composition. Small additions of...compositions evaluated, enlarged cubic cells could not be formed by ordering. Small additions of less than 5% of BaZrO 3 or SrZrO 3 to LaAIO 3 produced

  13. The role of hydrogen in zirconium alloy corrosion

    NASA Astrophysics Data System (ADS)

    Ensor, B.; Lucente, A. M.; Frederick, M. J.; Sutliff, J.; Motta, A. T.

    2017-12-01

    Hydrogen enters zirconium metal as a result of the corrosion process and forms hydrides when present in quantities above the solubility limit at a given temperature. Zircaloy-4 coupons of different thicknesses (0.4 mm-2.3 mm) but identical chemistry and processing were corroded in autoclave at 360 °C for various times up to 2800 days. Coupons were periodically removed and weighed to determine weight gain, which allows follow of the corrosion kinetics. Coupon thickness differences resulted in different volumetric concentrations of hydrogen, as quantified using hot vacuum extraction. The thinnest coupons, having the highest concentration of hydrogen, demonstrated acceleration in their corrosion kinetics and shorter transition times when compared to thicker coupons. Furthermore, it was seen that the post-transition corrosion rate was increased with increasing hydrogen concentration. Corrosion rates increased only after the terminal solid solubility (TSS) was exceeded for hydrogen in Zircaloy-4 at 360 °C. Therefore, it is hypothesized that the corrosion acceleration is caused by the formation of hydrides. Scanning electron microscope (SEM) examinations of fractured oxide layers demonstrate the oxide morphology changed with hydrogen content, with more equiaxed oxide grains in the high hydrogen samples than in those with lower hydrogen content. Additionally, locations of advanced oxide growth were correlated with locations of hydrides in the metal. A hypothesis is proposed to explain the accelerated corrosion due to the presence of the hydrides, namely that the metal, locally, is less able to accommodate oxide growth stresses and this leads to earlier loss of oxide protectiveness in the form of more frequent oxide kinetic transitions.

  14. Assessment of color stability of white mineral trioxide aggregate angelus and bismuth oxide in contact with tooth structure.

    PubMed

    Marciano, Marina Angélica; Costa, Reginaldo Mendonça; Camilleri, Josette; Mondelli, Rafael Francisco Lia; Guimarães, Bruno Martini; Duarte, Marco Antonio Hungaro

    2014-08-01

    Dental discoloration with use of materials containing bismuth oxide has been reported. It is postulated that the discoloration is a result of chemical interaction of bismuth oxide with dentin. The aim of the study was to analyze dental color alteration and the chemical interaction of bismuth oxide with the main components present in composite (methacrylate) and in dentin (collagen). Fifty bovine teeth were prepared and filled with white mineral trioxide aggregate (MTA) Angelus, Portland cement (PC) with 20% zirconium oxide, or PC with 20% calcium tungstate and then sealed with composite. Triple antibiotic paste and unfilled samples were the positive and negative controls, respectively. The specimens were stored in separate flasks immersed in tap water at 37°C with ambient light blocked out. The color assessment was performed with a spectrophotometer at different intervals, namely before filling and 24 hours, 15 days, and 30 days after filling. The color change and the luminosity were calculated. The statistical analysis was performed by using nonparametric Kruskal-Wallis and Dunn tests (P < .05). The interaction of the bismuth oxide, zirconium oxide, and calcium tungstate with collagen and methacrylate was assessed by placing the materials in contact, followed by color assessment. The analysis of color change values showed that all the materials presented color alteration after the evaluated periods. Statistically higher luminosity was verified for PC/20% zirconium oxide in comparison with white MTA Angelus (P < .05). The teeth filled with white MTA Angelus demonstrated a grayish discoloration with evident dentin staining. Bismuth oxide exhibited a color change when in contact with collagen. The color of white MTA Angelus was altered in contact with dental structures. Collagen, which is present in dentin matrix, reacted with bismuth oxide, resulting in a grayish discoloration. The use of an alternative radiopacifier to replace bismuth in white MTA is indicated. Copyright © 2014 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  15. PROCESS OF MAKING SHAPED FUEL FOR NUCLEAR REACTORS

    DOEpatents

    O'Leary, W.J.; Fisher, E.A.

    1964-02-11

    A process for making uranium dioxide fuel of great strength, density, and thermal conductivity by mixing it with 0.1 to 1% of a densifier oxide (tin, aluminum, zirconium, ferric, zinc, chromium, molybdenum, titanium, or niobium oxide) and with a plasticizer (0.5 to 3% of bentonite and 0.05 to 2% of methylcellulose, propylene glycol alginate, or ammonium alginate), compacting the mixture obtained, and sintering the bodies in an atmosphere of carbon monoxide or carbon dioxide, with or without hydrogen, or of a nitrogen-hydrogen mixture is described. (AEC)

  16. Comparing XPS on bare and capped ZrN films grown by plasma enhanced ALD: Effect of ambient oxidation

    NASA Astrophysics Data System (ADS)

    Muneshwar, Triratna; Cadien, Ken

    2018-03-01

    In this article we compare x-ray photoelectron spectroscopy (XPS) measurements on bare- and capped- zirconium nitride (ZrN) films to investigate the effect of ambient sample oxidation on the detected bound O in the form of oxide ZrO2 and/or oxynitride ZrOxNy. ZrN films in both bare- and Al2O3/AlN capped- XPS samples were grown by plasma-enhanced atomic layer deposition (PEALD) technique using tetrakis dimethylamino zirconium (TDMAZr) precursor, forming gas (5% H2, rest N2) inductively coupled plasma (ICP), and as received research grade process gases under identical process conditions. Capped samples were prepared by depositing 1 nm thick PEALD AlN on ZrN, followed by additional deposition of 1 nm thick ALD Al2O3, without venting of ALD reactor. On bare ZrN sample at room temperature, spectroscopic ellipsometry (SE) measurements with increasing ambient exposure times (texp) showed a self-limiting surface oxidation with the oxide thickness (dox) approaching 3.7 ± 0.02 nm for texp > 120 min. In XPS data measured prior to sample sputtering (tsput = 0), ZrO2 and ZrOxNy were detected in bare- samples, whereas only ZrN and Al2O3/AlN from capping layer were detected in capped- samples. For bare-ZrN samples, appearance of ZrO2 and ZrOxNy up to sputter depth (dsput) of 15 nm in depth-profile XPS data is in contradiction with measured dox = 3.7 nm, but explained from sputtering induced atomic inter-diffusion within analyzed sample. Appearance of artifacts in the XPS spectra from moderately sputtered (dsput = 0.2 nm and 0.4 nm) capped-ZrN sample, provides an evidence to ion-bombardment induced modifications within analyzed sample.

  17. Composite construction for nuclear fuel containers

    DOEpatents

    Cheng, B. C.; Rosenbaum, H. S.; Armijo, J. S.

    1987-04-21

    Disclosed is an improved method for producing nuclear fuel containers of a composite construction having components providing therein a barrier system for resisting destructive action by volatile fission products or impurities and also interdiffusion of metal constituents, and the product thereof. The composite nuclear fuel containers of the method comprise a casing of zirconium or alloy thereof with a layer of copper overlying an oxidized surface portion of the zirconium or alloy thereof. 1 fig.

  18. Electrochemical Study of Corrosion Phenomena in Zirconium Alloys

    DTIC Science & Technology

    2005-06-01

    required reaction rates [1.1]. Based predominantly on this fact, zirconium alloys were chosen to sheath, or clad, the fuel. With the increasing demand...cathode or anode. As the oxidation and reduction reactions occur, a galvanic cell is developed. The electrons on the anode are released from the metallic...matrix as the ions are released into the aqueous solution in the initial half-cell reaction . The second half-cell reaction , taking place on the

  19. Effect of protective release coatings on the basis of superdispersersed zirconium oxide powder on the formation of gas defects in bronze casting

    NASA Astrophysics Data System (ADS)

    Martyushev, Nikita V.; Risto, Nikolay A.

    2014-10-01

    This paper investigates the use of nanopowders in the composition of foundry coatings when casting leaded tin bronzes. Influence of the composition of the applied protective coating on surface finish is studied. The effects of the coatings of the following compositions are compared: non-stick coating (a mixture of low-dispersed chromium oxide powder and heat-treated vegetable oil); non-stick lubricant ASPF-2/RgU on the basis of low- dispersed graphite powder and heat-treated vegetable oil; patent #2297300 (a mixture of superdispersed zirconium dioxide powder with industrial oil). It is demonstrated that application of foundry coatings containing superdispersed metal oxide powders with low thermal conductivity makes it possible to significantly reduce irregularities and eliminate gas porosity on the surface of tin-leaded bronze castings.

  20. Residual stresses in high temperature corrosion of pure zirconium using elasto-viscoplastic model: Application to the deflection test in monofacial oxidation

    NASA Astrophysics Data System (ADS)

    Fettré, D.; Bouvier, S.; Favergeon, J.; Kurpaska, L.

    2015-12-01

    The paper is devoted to modeling residual stresses and strains in an oxide film formed during high temperature oxidation. It describes the deflection test in isothermal high-temperature monofacial oxidation (DTMO) of pure zirconium. The model incorporates kinetics and mechanism of oxidation and takes into account elastic, viscoplastic, growth and chemical strains. Different growth strains models are considered, namely, isotropic growth strains given by Pilling-Bedworth ratio, anisotropic growth strains defined by Parise and co-authors and physically based model for growth strain proposed by Clarke. Creep mechanisms based on dislocation slip and core diffusion, are used. A mechanism responsible for through thickness normal stress gradient in the oxide film is proposed. The material parameters are identified using deflection tests under 400 °C, 500 °C and 600 °C. The effect of temperature on creep and stress relaxation is analyzed. Numerical sensitivity study of the DTMO experiment is proposed in order to investigate the effects of the initial foil thickness and platinum coating on the deflection curves.

  1. Hysteresis in Lanthanide Zirconium Oxides Observed Using a Pulse CV Technique and including the Effect of High Temperature Annealing.

    PubMed

    Lu, Qifeng; Zhao, Chun; Mu, Yifei; Zhao, Ce Zhou; Taylor, Stephen; Chalker, Paul R

    2015-07-29

    A powerful characterization technique, pulse capacitance-voltage (CV) technique, was used to investigate oxide traps before and after annealing for lanthanide zirconium oxide thin films deposited on n-type Si (111) substrates at 300 °C by liquid injection Atomic Layer Deposition (ALD). The results indicated that: (1) more traps were observed compared to the conventional capacitance-voltage characterization method in LaZrO x ; (2) the time-dependent trapping/de-trapping was influenced by the edge time, width and peak-to-peak voltage of a gate voltage pulse. Post deposition annealing was performed at 700 °C, 800 °C and 900 °C in N₂ ambient for 15 s to the samples with 200 ALD cycles. The effect of the high temperature annealing on oxide traps and leakage current were subsequently explored. It showed that more traps were generated after annealing with the trap density increasing from 1.41 × 10 12 cm -2 for as-deposited sample to 4.55 × 10 12 cm -2 for the 800 °C annealed one. In addition, the leakage current density increase from about 10 - ⁶ A/cm² at V g = +0.5 V for the as-deposited sample to 10 -3 A/cm² at V g = +0.5 V for the 900 °C annealed one.

  2. Zirconium oxide ceramic foam: a promising supporting biomaterial for massive production of glial cell line-derived neurotrophic factor*

    PubMed Central

    Liu, Zhong-wei; Li, Wen-qiang; Wang, Jun-kui; Ma, Xian-cang; Liang, Chen; Liu, Peng; Chu, Zheng; Dang, Yong-hui

    2014-01-01

    This study investigated the potential application of a zirconium oxide (ZrO2) ceramic foam culturing system to the production of glial cell line-derived neurotrophic factor (GDNF). Three sets of ZrO2 ceramic foams with different pore densities of 10, 20, and 30 pores per linear inch (PPI) were prepared to support a 3D culturing system. After primary astrocytes were cultured in these systems, production yields of GDNF were evaluated. The biomaterial biocompatibility, cell proliferation and activation of cellular signaling pathways in GDNF synthesis and secretion in the culturing systems were also assessed and compared with a conventional culturing system. In this study, we found that the ZrO2 ceramic foam culturing system was biocompatible, using which the GDNF yields were elevated and sustained by stimulated cell proliferation and activation of signaling pathways in astrocytes cultured in the system. In conclusion, the ZrO2 ceramic foam is promising for the development of a GDNF mass production device for Parkinson’s disease treatment. PMID:25471830

  3. Monitoring bisphosphonate surface functionalization and acid stability of hierarchically porous titanium zirconium oxides.

    PubMed

    Ide, Andreas; Drisko, Glenna L; Scales, Nicholas; Luca, Vittorio; Schiesser, Carl H; Caruso, Rachel A

    2011-11-01

    To take advantage of the full potential of functionalized transition metal oxides, a well-understood nonsilane based grafting technique is required. The functionalization of mixed titanium zirconium oxides was studied in detail using a bisphosphonic acid, featuring two phosphonic acid groups with high surface affinity. The bisphosphonic acid employed was coupled to a UV active benzamide moiety in order to track the progress of the surface functionalization in situ. Using different material compositions, altering the pH environment, and looking at various annealing conditions, key features of the functionalization process were identified that consequently will allow for intelligent material design. Loading with bisphosphonic acid was highest on supports calcined at 650 °C compared to lower calcination temperatures: A maximum capacity of 0.13 mmol g(-1) was obtained and the adsorption process could be modeled with a pseudo-second-order rate relationship. Heating at 650 °C resulted in a phase transition of the mixed binary oxide to a ternary oxide, titanium zirconium oxide in the srilankite phase. This phase transition was crucial in order to achieve high loading of the bisphosphonic acid and enhanced chemical stability in highly acidic solutions. Due to the inert nature of phosphorus-oxygen-metal bonds, materials functionalized by bisphosphonic acids showed increased chemical stability compared to their nonfunctionalized counterparts in harshly acidic solutions. Leaching studies showed that the acid stability of the functionalized material was improved with a partially crystalline srilankite phase. The materials were characterized using nitrogen sorption, X-ray powder diffraction, and UV-vis spectroscopy; X-ray photoelectron spectroscopy was used to study surface coverage with the bisphosphonic acid molecules.

  4. Mesoporous zirconium titanium oxides. Part 1: Porosity modulation and adsorption properties of xerogels.

    PubMed

    Griffith, Christopher S; Sizgek, G Devlet; Sizgek, Erden; Scales, Nicholas; Yee, Patrick J; Luca, Vittorio

    2008-11-04

    A series of zirconium titanium oxide mesophases containing 33 atom % Zr have been prepared using carboxylic acids of different alkyl chain lengths (Cy ) from y=4-18 through organic-inorganic polymer phase segregation as the gel transition is approached. Thermal treatment of these transparent gels up to 450 degrees C eliminated the organic template, and domain coarsening occurred affording stable worm-hole mesoporous materials of homogeneous composition and pore diameters varying from about 3 to 4 nm in fine increments. With such materials, it was subsequently possible to precisely study the adsorption of vanadium oxo-anions and cations from aqueous solutions and, more particularly, probe the kinetics of intraparticle mass transport as a function of the associated pore dimension. The kinetics of mass transport through the pore systems was investigated using aqueous vanadyl (VO2+) and orthovanadate (VO3(OH)2-) probe species at concentrations ranging from 10 to 200 ppm (0.2 to 4 mmol/L) and pH values of 0 and 10.5, respectively. In the case of both of these vanadium species, the zirconium titanate mesophases displayed relatively slow kinetics, taking in excess of about 500 min to achieve maximum uptake. By using a pseudo-second-order rate law, it was possible to extract the instantaneous and overall rate of the adsorption processes and then relate these to the pore diameters. Both the instantaneous and overall rates of adsorption increased with increasing surface area and pore diameter over the studied pore size range. However, the equilibrium adsorption capacity increased linearly with pore diameter only for the higher concentrations and was independent of pore diameter for the lower concentration. These results have been interpreted using a model in which discrete adsorption occurs at low concentrations and is then followed by multilayer adsorption at higher concentration.

  5. Mössbauer study of oxide films of Fe-, Sn-, Cr- doped zirconium alloys during corrosion in autoclave

    NASA Astrophysics Data System (ADS)

    Filippov, V. P.; Bateev, A. B.; Lauer, Yu. A.

    2016-12-01

    Mössbauer investigations were used to compare iron atom states in oxide films of binary Zr-Fe, ternary Zr-Fe-Cu and quaternary Zr-Fe-Cr-Sn alloys. Oxide films are received in an autoclave at a temperature of 350-360 °C and at pressure of 16.8 MPa. The corrosion process decomposes the intermetallic precipitates in alloys and forms metallic iron with inclusions of chromium atoms α-Fe(Cr), α-Fe(Cu), α-Fe 2O3 and Fe 3O4 compounds. Some iron ions are formed in divalent and in trivalent paramagnetic states. The additional doping influences on corrosion kinetics and concentration of iron compounds and phases formed in oxide films. It was shown the correlation between concentration of iron in different chemical states and corrosion resistance of alloys.

  6. Oxygen Interaction With Space-Power Materials

    NASA Technical Reports Server (NTRS)

    Eck, Thomas G.; Hoffman, Richard W.

    1996-01-01

    Four investigations were undertaken during the period of this grant: (1 ) oxidation of molybdenum and of niobium-1 % zirconium, (2) preparation of and examination of EOIM-3 samples, (3) sputtering of Teflon by oxygen ion bombardment,and (4) sputtering of Ions from copper and aluminum by oxygen and argon ion bombardment. Investigations (1), (3), and (4) used a low-energy Ion gun to bombard surfaces within an ultra-high vacuum system. Particles ejected from the surfaces were detected by a mass spectrometer.

  7. Retention of implant-supported zirconium oxide ceramic restorations using different luting agents.

    PubMed

    Nejatidanesh, Farahnaz; Savabi, Omid; Shahtoosi, Mojtaba

    2013-08-01

    The aim of this study was to evaluate the retention value of implant-supported zirconium oxide ceramic copings using different luting agents. Twenty ITI solid abutments of 5.5 mm height and ITI implant analogs were mounted vertically into autopolymerizing acrylic resin blocks. Ninety zirconium oxide copings (Cercon, Degudent) with a loop on the occlusal portion were made. All samples were airborne particle abraded with 110 μm Al₂O₃ and luted using different types of luting agents: resin cements (Clearfil SA, Panavia F2.0, Fuji Plus), conventional cements (Fleck's, Poly F, Fuji I), and temporary cements (Temp Bond, GC free eugenol, TempSpan) with a load of 5 Kg. (N = 10) All copings were incubated at 37°C for 24 h and conditioned in artificial saliva for 1 week, and thermal cycled for 5000 cycles 5-55°C with a 30-s dwell time. The dislodging force of the copings along the long axis of the implant-abutment complex was recorded using universal testing machine with 5 mm/min crosshead speed. Data were subjected to Kruskal-Wallis (α = 0.05) and Mann-Whitney tests with Bonferroni step down correction (α = 0.001). There was significant difference between the mean rank retention values of different luting agents (P < 0.001). The resin cements showed the highest retention (Clearfil SA, 203.49 ± 52.86; Fuji Plus, 190.61 ± 48.00; Panavia F 2.0, 172.16 ± 70.76 N). The conventional cements had more retention than the temporary cements and glass ionomer cement (P < 0.001). The retention of zircona ceramic restorations, over ITI solid abutments may be influenced by the type of cement. The application of an MDP-containing resin and resin-modified glass ionomer luting agents increase the retentive value of implant-supported zirconium oxide restorations. © 2011 John Wiley & Sons A/S.

  8. Tension-Compression Fatigue of an Oxide/Oxide Ceramic Matrix Composite at Elevated Temperature in Air and Steam Environments

    DTIC Science & Technology

    2015-03-26

    method has been successfully used with several materials such as silicon carbide fiber - silicon carbide matrix ( SiC / SiC ) CMCs with carbon and boron...elements [14]. These advanced ceramics include oxides, nitrides and carbides of silicon , aluminum, titanium, and zirconium [12]. One of the most...oxides over silicon carbide and other non-oxide materials. In fact, it is the inherent stability of oxides in oxidizing environments which originally

  9. Method for forming nuclear fuel containers of a composite construction and the product thereof

    DOEpatents

    Cheng, Bo-Ching; Rosenbaum, Herman S.; Armijo, Joseph S.

    1984-01-01

    An improved method for producing nuclear fuel containers of a composite construction having components providing therein a barrier system for resisting destructive action by volatile fission products or impurities and also interdiffusion of metal constituents, and the product thereof. The composite nuclear fuel containers of the method comprise a casing of zirconium or alloy thereof with a layer of copper overlying an oxidized surface portion of the zirconium or alloy thereof.

  10. Effect of rare earth doping on optical and spectroscopic characteristics of BaZrO3:Eu3+,Tb3+ perovskites.

    PubMed

    Katyayan, Shambhavi; Agrawal, Sadhana

    2018-04-04

    This paper reports structural investigations of rare earth doped BaZrO 3 phosphors synthesized by Solid state reaction technique with varying concentrations of Eu 3+ and Tb 3+ from 0 mol% to 2 mol%. The synthesized phosphors show enhanced variable emissions in the visible region corresponding to different hypersensitive electronic transitions of Eu 3+ and Tb 3+ ions. With cubic structure confirmed in XRD analysis, the FESEM images show uniform grain connectivity and homogeneity of prepared samples. The TEM micrographs of the synthesized phosphors show agglomerated irregular structures. The synthesized phosphors were also subjected to FTIR, Raman, EDXS analysis along with studies of thermoluminescent and photoluminescent characteristics. On subjecting to 229 nm (UV) excitation, the phosphors show enhanced PL emissions corresponding to 571 nm ( 5 D 0 - 7 F 0 ), 591 nm ( 5 D 0 - 7 F 1 ), 615 nm ( 5 D 0 - 7 F 2 ) and 678 nm ( 5 D 0 - 7 F 4 ) hypersensitive transitions of Eu 3+ ions and emission peaks at 489 nm ( 5 D 4 - 7 F 6 ), 539 nm ( 5 D 4 - 7 F 5 ), 589 nm ( 5 D 4 - 7 F 4 ) and 632 nm ( 5 D 4 - 7 F 3 ) accounting for electronic transitions of Tb 3+ ions respectively. The computed average PL lifetime is 14.014 s. In the TL analysis, the second order of kinetics with the activation energy varying from 5.0 × 10 -1 eV to 6.6 × 10 -1 eV is reported. The maximum TL lifetime is estimated as 19.4985 min in the TL lifetime analysis.

  11. Effect of rare earth doping on optical and spectroscopic characteristics of BaZrO3:Eu3+,Tb3+ perovskites

    NASA Astrophysics Data System (ADS)

    Katyayan, Shambhavi; Agrawal, Sadhana

    2018-06-01

    This paper reports structural investigations of rare earth doped BaZrO3 phosphors synthesized by Solid state reaction technique with varying concentrations of Eu3+ and Tb3+ from 0 mol% to 2 mol%. The synthesized phosphors show enhanced variable emissions in the visible region corresponding to different hypersensitive electronic transitions of Eu3+ and Tb3+ ions. With cubic structure confirmed in XRD analysis, the FESEM images show uniform grain connectivity and homogeneity of prepared samples. The TEM micrographs of the synthesized phosphors show agglomerated irregular structures. The synthesized phosphors were also subjected to FTIR, Raman, EDXS analysis along with studies of thermoluminescent and photoluminescent characteristics. On subjecting to 229 nm (UV) excitation, the phosphors show enhanced PL emissions corresponding to 571 nm (5D0-7F0), 591 nm (5D0-7F1), 615 nm (5D0-7F2) and 678 nm (5D0-7F4) hypersensitive transitions of Eu3+ ions and emission peaks at 489 nm (5D4-7F6), 539 nm (5D4-7F5), 589 nm (5D4-7F4) and 632 nm (5D4-7F3) accounting for electronic transitions of Tb3+ ions respectively. The computed average PL lifetime is 14.014 s. In the TL analysis, the second order of kinetics with the activation energy varying from 5.0 × 10‑1 eV to 6.6 × 10‑1 eV is reported. The maximum TL lifetime is estimated as 19.4985 min in the TL lifetime analysis.

  12. Air oxidation of Zircaloy-4 in the 600-1000 °C temperature range: Modeling for ASTEC code application

    NASA Astrophysics Data System (ADS)

    Coindreau, O.; Duriez, C.; Ederli, S.

    2010-10-01

    Progress in the treatment of air oxidation of zirconium in severe accident (SA) codes are required for a reliable analysis of severe accidents involving air ingress. Air oxidation of zirconium can actually lead to accelerated core degradation and increased fission product release, especially for the highly-radiotoxic ruthenium. This paper presents a model to simulate air oxidation kinetics of Zircaloy-4 in the 600-1000 °C temperature range. It is based on available experimental data, including separate-effect experiments performed at IRSN and at Forschungszentrum Karlsruhe. The kinetic transition, named "breakaway", from a diffusion-controlled regime to an accelerated oxidation is taken into account in the modeling via a critical mass gain parameter. The progressive propagation of the locally initiated breakaway is modeled by a linear increase in oxidation rate with time. Finally, when breakaway propagation is completed, the oxidation rate stabilizes and the kinetics is modeled by a linear law. This new modeling is integrated in the severe accident code ASTEC, jointly developed by IRSN and GRS. Model predictions and experimental data from thermogravimetric results show good agreement for different air flow rates and for slow temperature transient conditions.

  13. Ternary cobalt-molybdenum-zirconium coatings for alternative energies

    NASA Astrophysics Data System (ADS)

    Yar-Mukhamedova, Gulmira; Ved', Maryna; Sakhnenko, Nikolay; Koziar, Maryna

    2017-11-01

    Consistent patterns for electrodeposition of Co-Mo-Zr coatings from polyligand citrate-pyrophosphate bath were investigated. The effect of both current density amplitude and pulse on/off time on the quality, composition and surface morphology of the galvanic alloys were determined. It was established the coating Co-Mo-Zr enrichment by molybdenum with current density increasing up to 8 A dm-2 as well as the rising of pulse time and pause duration promotes the content of molybdenum because of subsequent chemical reduction of its intermediate oxides by hydrogen ad-atoms. It was found that the content of the alloying metals in the coating Co-Mo-Zr depends on the current density and on/off times extremely and maximum Mo and Zr content corresponds to the current density interval 4-6 A dm-2, on-/off-time 2-10 ms. Chemical resistance of binary and ternary coatings based on cobalt is caused by the increased tendency to passivity and high resistance to pitting corrosion in the presence of molybdenum and zirconium, as well as the acid nature of their oxides. Binary coating with molybdenum content not less than 20 at.% and ternary ones with zirconium content in terms of corrosion deep index are in a group ;very proof;. It was shown that Co-Mo-Zr alloys exhibits the greatest level of catalytic properties as cathode material for hydrogen electrolytic production from acidic media which is not inferior a platinum electrode. The deposits Co-Mo-Zr with zirconium content 2-4 at.% demonstrate high catalytic properties in the carbon(II) oxide conversion. This confirms the efficiency of materials as catalysts for the gaseous wastes purification and gives the reason to recommend them as catalysts for red-ox processes activating by oxygen as well as electrode materials for red-ox batteries.

  14. Influence of dosage, pH and contact time in stabilized landfill leachate treatment using ozone/zirconium tetrachloride catalytic oxidation

    NASA Astrophysics Data System (ADS)

    Zakaria, Siti Nor Farhana; Aziz, Hamidi Abdul

    2017-10-01

    Leachate is a critical problem of sanitary landfills because it contains high organic matter and hazardous compounds that can generate negative environmental effects. The high chemical oxygen demand (COD) and color of the leachate necessitates its treatment before it can be released to the water body. Thus, an investigation into the performance of advanced oxidation processes (AOPs) was conducted using a combination of ozone (O3) with zirconium tetrachloride (ZrCl4) as catalyst in stabilized landfill leachate treatment. Such leachate was collected from the Alor Pongsu Landfill site (APLS), Perak, Malaysia. COD and color parameter were used as indicators to examine the effect of O3/ZrCl4 dosage, pH, and contact time. The experiment was run under gas flow rate of 1,000 mL/min±10% and temperature below 15 °C. The maximum removal obtained for COD and color were 88% and 100%, respectively. This outcome was achieved at 27 g/m3 ozone dosage, pH 6, 90 min reaction time, and dosage ratio of 1:2 (COD g: ZrCl4 g). The reaction rate constant (k) was 0.2364 min-1 and followed pseudo first order. Thus, given the efficiency of the O3/ZrCl4 mixture for the remediation of stabilized landfill leachate, a new alternative method in leachate industrial treatment was identified.

  15. Effect of zirconium addition on welding of aluminum grain refined by titanium plus boron

    NASA Astrophysics Data System (ADS)

    Zaid, A. I. O.

    2014-06-01

    Aluminum oxidizes freely in ordinary atmosphere which makes its welding difficult and weak, particularly it solidifies in columnar structure with large grains. Therefore, it is anticipated that the effect of addition of some grain refiners to its melt before solidification is worth while investigating as it may enhance its weldabilty and improve its mechanical strength. In this paper, the effect of addition of zirconium at a weight of 0.1% (which corresponds to the peretictic limit on the aluminum-zirconium base phase diagram) to commercially pure aluminum, grain refined by Ti+B on its weldability, using gas tungsten arc welding, GTAW, method which was formerly known as TIG. A constant current level of 30 AC Ampere was used because it removes the oxides during the welding process. Metallographic examination of the weldments of the different combinations of Al with Al and Al with its microalloys: in the heat affected zone, HAZ, and away from it was carried out and examined for HAZ width, porosity, cracks and microhardness. It was found that grain refining by Ti+B or Zr resulted in enhancement of the weldment.

  16. Corrosion-electrochemical behavior of zirconium in molten alkali metal carbonates

    NASA Astrophysics Data System (ADS)

    Nikitina, E. V.

    2016-08-01

    The corrosion and electrochemical characteristics of zirconium during its interaction with molten lithium, sodium, and potassium carbonates containing from 1 to 5 wt % additives to the salt phase are studied in a temperature range of 500-800°C using gravimetry, corrosion potential measurement, and anodic polarization. The substances decreasing the corrosion losses due to the strengthening and thickening of an oxide film (lithium, sodium, potassium hydroxides) are used as passivators. Sodium chloride, fluoride, and sulfate serve as corrosion stimulators (activators).

  17. Fluorometric determination of zirconium in minerals

    USGS Publications Warehouse

    Alford, W.C.; Shapiro, L.; White, C.E.

    1951-01-01

    The increasing use of zirconium in alloys and in the ceramics industry has created renewed interest in methods for its determination. It is a common constituent of many minerals, but is usually present in very small amounts. Published methods tend to be tedious, time-consuming, and uncertain as to accuracy. A new fluorometric procedure, which overcomes these objections to a large extent, is based on the blue fluorescence given by zirconium and flavonol in sulfuric acid solution. Hafnium is the only element that interferes. The sample is fused with borax glass and sodium carbonate and extracted with water. The residue is dissolved in sulfuric acid, made alkaline with sodium hydroxide to separate aluminum, and filtered. The precipitate is dissolved in sulfuric acid and electrolysed in a Melaven cell to remove iron. Flavonol is then added and the fluorescence intensity is measured with a photo-fluorometer. Analysis of seven standard mineral samples shows excellent results. The method is especially useful for minerals containing less than 0.25% zirconium oxide.

  18. Fischer-Tropsch Cobalt Catalyst Improvements with the Presence of TiO2, La2O3, and ZrO2 on an Alumina Support

    NASA Technical Reports Server (NTRS)

    Klettlinger, Jennifer Lindsey Suder

    2012-01-01

    The objective of this study was to evaluate the effect of titanium oxide, lanthanum oxide, and zirconium oxide on alumina supported cobalt catalysts. The hypothesis was that the presence of lanthanum oxide, titanium oxide, and zirconium oxide would reduce the interaction between cobalt and the alumina support. This was of interest because an optimized weakened interaction could lead to the most advantageous cobalt dispersion, particle size, and reducibility. The presence of these oxides on the support were investigated using a wide range of characterization techniques such as SEM, nitrogen adsorption, x-ray diffraction (XRD), temperature programmed reduction (TPR), temperature programmed reduction after reduction (TPR-AR), and hydrogen chemisorptions/pulse reoxidation. Results indicated that both La2O3 and TiO2 doped supports facilitated the reduction of cobalt oxide species in reference to pure alumina supported cobalt catalysts, however further investigation is needed to determine the effect of ZrO2 on the reduction profile. Results showed an increased corrected cluster size for all three doped supported catalysts in comparison to their reference catalysts. The increase in reduction and an increase in the cluster size led to the conclusion that the support-metal interaction weakened by the addition of TiO2 and La2O3. It is also likely that the interaction decreased upon presence of ZrO2 on the alumina, but further research is necessary. Preliminary results have indicated that the alumina-supported catalysts with titanium oxide and lanthanum oxide present are of interest because of the weakened cobalt support interaction. These catalysts showed an increased extent of reduction, therefore more metallic cobalt is present on the support. However, whether or not there is more cobalt available to participate in the Fischer-Tropsch synthesis reaction (cobalt surface atoms) depends also on the cluster size. On one hand, increasing cluster size alone tends to decrease the active site density; on the other hand, by increasing the size of the cobalt clusters, there is less likelihood of forming oxidized cobalt complexes (cobalt aluminate) during Fischer-Tropsch synthesis. Thus, from the standpoint of stability, improving the extent of reduction while increasing the particle size slightly may be beneficial for maintaining the sites, even if there is a slight decrease in overall initial active site density.

  19. NADH Electrooxidation Using Bis(1,10-phenanthroline-5,6-dione) (2,2′-bipyridine)ruthenium(II)-Exchanged Zirconium Phosphate Modified Carbon Paste Electrodes

    PubMed Central

    Santiago, Mitk’El B.; Vélez, Meredith M.; Borrero, Solmarie; Díaz, Agustín; Casillas, Craig A.; Hofmann, Cristina; Guadalupe, Ana R.; Colón, Jorge L.

    2007-01-01

    We present a carbon paste electrode (CPE) modified using the electron mediator bis(1,10-phenanthroline-5,6-dione) (2,2′-bipyridine)ruthenium(II) ([Ru(phend)2bpy]2+) exchanged into the inorganic layered material zirconium phosphate (ZrP). X-Ray powder diffraction showed that the interlayer distance of ZrP increases upon [Ru(phend)2bpy]2+ intercalation from 10.3 Å to 14.2 Å. The UV-vis and IR spectroscopies results showed the characteristic peaks expected for [Ru(phend)2bpy]2+. The UV-vis spectrophotometric results indicate that the [Ru(phend)2bpy]2+ concentration inside the ZrP layers increased as a function of the loading level. The exchanged [Ru(phend)2bpy]2+ exhibited luminescence even at low concentration. Modified CPEs were constructed and analyzed using cyclic voltammetry. The intercalated mediator remained electroactive within the layers (E°′ = −38.5 mV vs. Ag/AgCl, 3.5 M NaCl) and electrocatalysis of NADH oxidation was observed. The kinetics of the modified CPE shows a Michaelis –Menten behavior. This CPE was used for the oxidation of NADH in the presence of Bakers’ yeast alcohol dehydrogenase. A calibration plot for ethanol is presented. PMID:18516242

  20. A comparative study of zirconium and titanium implants in rat: osseointegration and bone material quality.

    PubMed

    Hoerth, Rebecca M; Katunar, María R; Gomez Sanchez, Andrea; Orellano, Juan C; Ceré, Silvia M; Wagermaier, Wolfgang; Ballarre, Josefina

    2014-02-01

    Permanent metal implants are widely used in human medical treatments and orthopedics, for example as hip joint replacements. They are commonly made of titanium alloys and beyond the optimization of this established material, it is also essential to explore alternative implant materials in view of improved osseointegration. The aim of our study was to characterize the implant performance of zirconium in comparison to titanium implants. Zirconium implants have been characterized in a previous study concerning material properties and surface characteristics in vitro, such as oxide layer thickness and surface roughness. In the present study, we compare bone material quality around zirconium and titanium implants in terms of osseointegration and therefore characterized bone material properties in a rat model using a multi-method approach. We used light and electron microscopy, micro Raman spectroscopy, micro X-ray fluorescence and X-ray scattering techniques to investigate the osseointegration in terms of compositional and structural properties of the newly formed bone. Regarding the mineralization level, the mineral composition, and the alignment and order of the mineral particles, our results show that the maturity of the newly formed bone after 8 weeks of implantation is already very high. In conclusion, the bone material quality obtained for zirconium implants is at least as good as for titanium. It seems that the zirconium implants can be a good candidate for using as permanent metal prosthesis for orthopedic treatments.

  1. An investigation on the preparation of nanocrystalline hydrous zirconia from zirconium tungstate

    NASA Astrophysics Data System (ADS)

    Antunes, M.; Perottoni, C. A.; Gouvêa, D.; Machado, G.; Zorzi, J. E.

    2018-02-01

    Hydrous nanocrystalline zirconia was prepared from an unusual precursor—the bimetallic oxide zirconium tungstate (ZrW2O8)—in alkaline medium. Different experimental conditions (NaOH concentration, time and temperature) were used to investigate the effects on crystallographic, morphological, chemical and thermal characteristics of the products. The resulting materials are composed of particles with a crystal structure similar to that of cubic ZrO2 (or a mixture of tetragonal and cubic phases, depending on the synthesis conditions), with particle size around 5 nm and crystallites around 3 nm in diameter. These particles form high surface area agglomerates, exhibiting mesoporosity and capacity for adsorption of water and carbon dioxide. The synthesis mechanism appears to be constituted, first, by a chemical substitution reaction between the WO4 tetrahedra and hydroxyl ions, with subsequent solubilization of the structure. Indeed, excess hydroxyls in the medium form colloidal zirconium ions which polymerize/condense, generating crystalline nuclei in a process facilitated by heterogeneous nucleation and supersaturation. The presence of residual tungsten in all samples appears to be a key element for stabilizing the size and crystalline structure of the materials produced.

  2. Calcification of MC3T3-E1 cells on titanium and zirconium.

    PubMed

    Umezawa, Takayuki; Chen, Peng; Tsutsumi, Yusuke; Doi, Hisashi; Ashida, Maki; Suzuki, Shoichi; Moriyama, Keiji; Hanawa, Takao

    2015-01-01

    To confirm similarity of hard tissue compatibility between titanium and zirconium, calcification of MC3T3-E1 cells on titanium and zirconium was evaluated in this study. Mirror-polished titanium (Ti) and zirconium (Zr) disks and zirconium-sputter deposited titanium (Zr/Ti) were employed in this study. The surface of specimens were characterized using scanning electron microscopy and X-ray diffraction. Then, the cellular proliferation, differentiation and calcification of MC3T3-E1 cells on specimens were investigated. The surface of Zr/Ti was much smoother and cleaner than those of Ti and Zr. The proliferation of the cell was the same among three specimens, while the differentiation and calcification on Zr/Ti were faster than those on Ti and Zr. Therefore, Ti and Zr showed the identical hard tissue compatibility according to the evaluation with MC3T3-E1 cells. Sputter deposition may improve cytocompatibility.

  3. Preparation and Corrosion Resistance of Trivalent Chromium-Zirconium Composite Coating

    NASA Astrophysics Data System (ADS)

    Huang, J. Z.

    2018-05-01

    Aluminum alloys are widely used in the various industries because of its superior advantages. However there will be a thin oxide layer on the surface of the pure aluminum to inhibit corrosion, when adding some other elements, the obtained aluminum alloy is easy to be corroded. Surface protection is an important means to improve the corrosion resistance of aluminum alloys. The formal research had already confirmed that the trivalent chromium conversion coating can significantly improve the corrosion resistance, and the usage of the zirconium solution can also protect the aluminum alloy from corrosion. In this study, we constructed the binary conversion coating with the Cr2(SO4)3 and the K2ZrF6. The optimum reaction conditions are as follows: 10g/L H3PO4, 2g/L K2ZrF6, 28g/L Cr2(SO4)3, pH=2.5∼3.5, temperature 40°C, and reaction time 10 min. Copper sulfate titration experiment confirmed that the corrosion resistance was significantly improved.

  4. The influence of adding modified zirconium oxide-titanium dioxide nano-particles on mechanical properties of orthodontic adhesive: an in vitro study.

    PubMed

    Felemban, Nayef H; Ebrahim, Mohamed I

    2017-01-13

    The purpose of this in-vitro study was to examine the effect of incorporating different concentrations of Zirconium oxide-Titanium dioxide (ZrO2-TiO2) nanoparticles, which can have antibacterial properties, on the mechanical properties of an orthodontic adhesive. ZrO2-TiO2 (Zirconium oxide, HWNANO, Hongwu International Group Ltd, China) -Titanium dioxide, Nanoshell, USA) nanopowder were incorporated into orthodontic adhesive (Transbond XT, 3 M Unitek, Monrovia, USA) with different concentrations (0.5% weight nonofiller and 1% weight nanofiller). The size of nanoparticle was 70-80 nm for ZrO2 and less than 50 nm for TiO2. For measuring the shear bond strength of the three groups of orthodontic adhesives [Transbond (control), Transbond mixed with 0.5% weight ZrO2-TiO2, and Transbond mixed with 1% weight ZrO2-TiO2], 30 freshly extracted human first premolars were used and bonded with stainless steel metal brackets (Dentaurum®, Discovery®, Deutschland), using the 3 orthodontic adhesives and 3 M Unitek; Transbond TM Plus Self-Etching Primer (10 samples in each group). The recorded values of compressive strength and tensile strength (measured separately on 10 samples of orthodontic adhesives (add the 3 D size of sample, light cured for 40 s on both sides) of each orthodontic adhesives), as well as the shear bond strength in Mega Pascal unit (MPa) were collected and exposed to one-way analysis of variance (ANOVA) and Tukey's post-hoc tests. orthodontic adhesive with 1% weight ZrO2-TiO2 showed the highest mean compressive (73.42 ± 1.55 MPa, p: 0.003, F: 12.74), tensile strength (8.65 ± 0.74 MPa, p: 0.001, F: 68.20), and shear bond strength (20.05 ± 0.2 MPa, p: 0.001, F: 0.17). Adding ZrO2-TiO2 nanoparticle to orthodontic adhesive increased compressive strength, tensile strength, and shear bond strength in vitro, but in vivo studies and randomized clinical trials are needed to validate the present findings.

  5. High temperature mechanical properties of a zirconium-modified, precipitation- strengthened nickel, 30 percent copper alloy

    NASA Technical Reports Server (NTRS)

    Whittenberger, J. D.

    1974-01-01

    A precipitation-strengthened Monel-type alloy has been developed through minor alloying additions of zirconium to a base Ni-30Cu alloy. The results of this exploratory study indicate that thermomechanical processing of a solution-treated Ni-30Cu-0.2Zr alloy produced a dispersion of precipitates. The precipitates have been tentatively identified as a Ni5Zr compound. A comparison of the mechanical properties, as determined by testing in air, of the zirconium-modified alloy to those of a Ni-30Cu alloy reveals that the precipitation-strengthened alloy has improved tensile properties to 1200 K and improved stress-rupture properties to 1100 K. The oxidation characteristics of the modified alloy appeared to be equivalent to those of the base Ni-30Cu alloy.

  6. In situ electrochemical synthesis of highly loaded zirconium nanoparticles decorated reduced graphene oxide for the selective determination of dopamine and paracetamol in presence of ascorbic acid.

    PubMed

    Ezhil Vilian, A T; Rajkumar, Muniyandi; Chen, Shen-Ming

    2014-03-01

    Highly loaded zirconium oxide (ZrO2) nanoparticles were supported on graphene oxide (ERGO/ZrO2) via an in situ, simple and clean strategy on the basis of the electrochemical redox reaction between zirconyl chloride and graphene oxide (ZrOCl2 and GO). The electrochemical measurements and surface morphology of the as prepared nanocomposite were studied using cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and field emission scanning electron microscopy (FESEM). This ZrO2 decorated reduced graphene oxide nanocomposite modified GCE (ERGO/ZrO2) exhibits a prominent electrocatalytic activity toward the selective detection and determination of dopamine (DA) and paracetamol (PA) in presence of ascorbic acid (AA). The peaks of linear sweep voltammetry (LSV) for DA and PA oxidation at ERGO/ZrO2 modified electrode surface were clearly separated from each other when they co-existed in the physiological pH (pH 7.0) with a potential value of 140 mV (between AA and DA) and 330 mV (between AA and PA). It was, therefore, possible to simultaneously determine DA and PA in the samples at ERGO/ZrO2 nanocomposite modified GCE. Linear calibration curves were obtained for 9-237 μM of PA and DA. The ERGO/ZrO2 nanocomposite electrode has been satisfactorily used for the determination of DA and PA in the presence of AA at pharmaceutical formulations in human urine samples with a linear range of 3-174 μM. The proposed biosensor shows a wide linear range, low detection limit, good reproducibility and acceptable stability, providing a biocompatible platform for bio sensing and bio catalysis. Copyright © 2013 Elsevier B.V. All rights reserved.

  7. The Deformation Mechanism of Fatigue Behaviour in a N36 Zirconium Alloy

    NASA Astrophysics Data System (ADS)

    Wang, Yingzhu

    2018-05-01

    Zirconium alloys are widely used as claddings in nuclear reactor. A N36 zirconium alloy has been deformed into a sheet with highly texture according to the result of electron back scatter diffraction test. Then this N36 zirconium alloy sheet has been cut into small beam samples with 12 x 3 x 3 mm3 in size. In this experiment, a three-point bending test was carried out to investigate the fatigue behaviour of N36 zirconium alloy. Cyclic loadings were applied on the top middle of the beam samples. The region of interest (ROI) is located at the middle bottom of the front face of the beam sample where slip band was observed in deformed beam sample due to strain concentration by using scanning electron microscopy. Twinning also plays an important role to accommodate the plastic deformation of N36 zirconium alloy in fatigue, which displays competition with slip.

  8. Bond strength of selected composite resin-cements to zirconium-oxide ceramic

    PubMed Central

    Fons-Font, Antonio; Amigó-Borrás, Vicente; Granell-Ruiz, María; Busquets-Mataix, David; Panadero, Rubén A.; Solá-Ruiz, Maria F.

    2013-01-01

    Objectives: The aim of this study was to evaluate bond strengths of zirconium-oxide (zirconia) ceramic and a selection of different composite resin cements. Study Design: 130 Lava TM cylinders were fabricated. The cylinders were sandblasted with 80 µm aluminium oxide or silica coated with CoJet Sand. Silane, and bonding agent and/or Clearfil Ceramic Primer were applied. One hundred thirty composite cement cylinders, comprising two dual-polymerizing (Variolink II and Panavia F) and two autopolymerizing (Rely X and Multilink) resins were bonded to the ceramic samples. A shear test was conducted, followed by an optical microscopy study to identify the location and type of failure, an electron microscopy study (SEM and TEM) and statistical analysis using the Kruskal-Wallis test for more than two independent samples and Mann-Whitney for two independent samples. Given the large number of combinations, Bonferroni correction was applied (α=0.001). Results: Dual-polymerizing cements provided better adhesion values (11.7 MPa) than the autopolymerizing (7.47 MPa) (p-value M-W<0.001). The worst techniques were Lava TM + sandblasting + Silane + Rely X; Lava TM + sandblasting + Silane + Multilink and Lava TM + CoJet + silane + Multilink. Adhesive failure (separation of cement and ceramic) was produced at a lesser force than cohesive failure (fracture of cement) (p-value M-W<0.001). Electron microscopy confirmed that the surface treatments modified the zirconium-oxide ceramic, creating a more rough and retentive surface, thus providing an improved micromechanical interlocking between the cement and the ceramic. Key words:Shear bond strength, silica coating, surface treatment, zirconia ceramics, phosphate monomer. PMID:22926485

  9. Studies on Acetone Powder and Purified Rhus Laccase Immobilized on Zirconium Chloride for Oxidation of Phenols

    PubMed Central

    Lu, Rong; Miyakoshi, Tetsuo

    2012-01-01

    Rhus laccase was isolated and purified from acetone powder obtained from the exudates of Chinese lacquer trees (Rhus vernicifera) from the Jianshi region, Hubei province of China. There are two blue bands appearing on CM-sephadex C-50 chromatography column, and each band corresponding to Rhus laccase 1 and 2, the former being the major constituent, and each had an average molecular weight of approximately 110 kDa. The purified and crude Rhus laccases were immobilized on zirconium chloride in ammonium chloride solution, and the kinetic properties of free and immobilized Rhus laccase, such as activity, molecular weight, optimum pH, and thermostability, were examined. In addition, the behaviors on catalytic oxidation of phenols also were conducted. PMID:22545205

  10. Effect of oxidation on transport properties of zirconium-1% niobium alloy

    NASA Astrophysics Data System (ADS)

    Peletsky, V. E.; Musayeva, Z. A.

    1995-11-01

    The thermal conductivity and electrical resistivity of zirconium-1 wt% niobium samples were measured before and after the process of their oxidation in air. A special procedure was used to dissolve the gas and to smooth out its concentration in the alloy. The basic experiments were performed under high vacuum under steady-state temperature conditions. The temperature range was 300 1600 K. for the pure alloy and 300 1100 K for the samples containing oxygen. It was found that the thermal conductivity—oxygen concentration relation reverses its sign from negative at low and middle temperatures to positive at temperatures above 900 K. The relation between the electrical resistivity and the oxygen content does not show this feature. The Lorenz function was found to have an anomalous temperature dependence.

  11. Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility.

    PubMed

    Li, H F; Zhou, F Y; Li, L; Zheng, Y F

    2016-04-19

    In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are <1%, much lower than 5%, the safe value for biomaterials according to ISO 10993-4 standard. Compared with conventional biomedical 316L stainless steel, Co-Cr alloys and Ti-based alloys, the magnetic susceptibilities of the zirconium-ruthenium alloys (1.25 × 10(-6) cm(3)·g(-1)-1.29 × 10(-6) cm(3)·g(-1) for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti-6Al-4V, ~3.5 × 10(-6) cm(3)·g(-1), CP Ti and Ti-6Al-7Nb, ~3.0 × 10(-6) cm(3)·g(-1)), and one-sixth that of Co-Cr alloys (Co-Cr-Mo, ~7.7 × 10(-6) cm(3)·g(-1)). Among the Zr-Ru alloy series, Zr-1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr-Ru alloy system as therapeutic devices under MRI diagnostics environments.

  12. Sorbents and Mechanisms of Removal

    DTIC Science & Technology

    2010-08-21

    Interactions of Ammonia with Pillared Graphite Oxide Intercalated with Aluminium and Zirconium Polyoxycations Mykola Seredych and T. J. Bandosz ,J...Adsorbents Containing Silver Nanoparticles M. Seredych, S. Bashkova, R. Pietrzak, T.J. Bandosz Langmuir, 26 (2010) 9457-9464 35. Graphite Oxide /Zr(OH)4...Small Molecule Toxic Gases on Graphite Oxide Based Adsorbents Adorbent Wokshop Camille Petit, Roberts Pietrzak and T.J. Bandosz Seattle, WA, July 12-14

  13. Isomerization of Cyclooctadiene to Cyclooctyne with a Zinc/Zirconium Heterobimetallic Complex.

    PubMed

    Butler, Michael J; White, Andrew J P; Crimmin, Mark R

    2016-06-06

    Reaction of a zinc/zirconium heterobimetallic complex with 1,5-cyclooctadiene (1,5-COD) results in slow isomerization to 1,3-cyclooctadiene (1,3-COD), along with the formation of a new complex that includes a cyclooctyne ligand bridging two metal centers. While analogous magnesium/zirconium and aluminum/zirconium heterobimetallic complexes are competent for the catalytic isomerization of 1,5-COD to 1,3-COD, only in the case of the zinc species is the cyclooctyne adduct observed. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Isomerization of Cyclooctadiene to Cyclooctyne with a Zinc/Zirconium Heterobimetallic Complex

    PubMed Central

    Butler, Michael J.; White, Andrew J. P.

    2016-01-01

    Abstract Reaction of a zinc/zirconium heterobimetallic complex with 1,5‐cyclooctadiene (1,5‐COD) results in slow isomerization to 1,3‐cyclooctadiene (1,3‐COD), along with the formation of a new complex that includes a cyclooctyne ligand bridging two metal centers. While analogous magnesium/zirconium and aluminum/zirconium heterobimetallic complexes are competent for the catalytic isomerization of 1,5‐COD to 1,3‐COD, only in the case of the zinc species is the cyclooctyne adduct observed. PMID:27071992

  15. Fracture strength and fatigue resistance of all-ceramic molar crowns manufactured with CAD/CAM technology.

    PubMed

    Zahran, Mohammed; El-Mowafy, Omar; Tam, Laura; Watson, Philip A; Finer, Yoav

    2008-07-01

    All-ceramic crowns are subject to fracture during function, especially in the posterior area. The use of yttrium-stabilized zirconium-oxide ceramic as a substructure for all-ceramic crowns to improve fracture resistance is unproven. The aim of this study was to compare fracture strength and fatigue resistance of new zirconium-oxide and feldspathic all-ceramic crowns made with computer-aided design/computer-aided manufacturing (CAD/CAM). An ivorine molar was prepared to receive an all-ceramic crown. Using epoxy resin, 40 replication dies were made of the prepared tooth. Twenty feldspathic all-ceramic crowns (Vita Mark II) (VMII) and 20 zirconium-oxide crown copings (In-Ceram YZ) (YZ) were made using CAD/CAM technique (CEREC-3D). The YZ copings were sintered and veneered manually with a fine-particle ceramic (VM9). All crowns were cemented to their respective dies using resin cement (Panavia F 2.0). Ten crowns in each group were subjected to compressive fatigue loading in a universal testing machine (instron). The other ten crowns from each group were loaded to fracture at a crosshead speed of 1 mm/min. Data were statistically analyzed using independent t-test and Fisher's exact test at alpha= 0.05. There was a significant difference between the survival rates of the two materials during the fatigue test (p < 0.001). All VMII crowns survived without any crack formation, while all YZ crowns fractured (40%) or developed cracks (60%). All the YZ crown fractures occurred within the veneering layer during the fatigue test. There was no significant difference in mean fracture load between the two materials (p= 0.268). Mean fracture loads (standard deviation) in N were: 1459 (492) for YZ crowns and 1272 (109) for VMII crowns. The performance of VMII crowns was superior to YZ crowns in the fatigue test. The premature fractures and cracks of the YZ crowns were attributed to weakness in the YZ veneer layer or in the core/veneer bond.

  16. Coordination behavior of bis-phenolate saturated and unsaturated N-heterocyclic carbene ligands to zirconium: reactivity and activity in the copolymerization of cyclohexene oxide with CO2.

    PubMed

    Lalrempuia, Ralte; Breivik, Frida; Törnroos, Karl W; Le Roux, Erwan

    2017-06-27

    Tetravalent zirconium complexes supported by tridentate bis-phenolate imidazolidin-2-ylidene (L1), imidazol-2-ylidene (L2) and benzimidazol-2-ylidene (L3) NHC ligands were synthesized and evaluated as precursors for the copolymerization of cyclohexene oxide (CHO) with CO 2 . While the reactivity of the imidazolidinium [H 3 L1] chloride salt with Zr(OiPr) 4 (HOiPr), and subsequent ligand exchanges with either (CH 3 ) 3 SiCl or LiOiPr lead to a series of heteroleptic compounds (κ 3 -O,C,O-L1)Zr(X) 2 (THF) (X = Cl, OiPr), both imidazolium [H 3 L2] and benzimidazolium [H 3 L3] chloride salts give a mixture of homoleptic (κ 3 -O,C,O-NHC) 2 Zr and zwitterionic (κ 2 -O,O-HL)ZrCl 2 (OiPr) compounds along with traces or the absence of the heteroleptic intermediate (κ 3 -O,C,O-NHC)Zr(Cl)(OiPr)(THF). Such dissimilar reactivity between the unsaturated and saturated NHC ligands is predominantly ascribed to the increased acidity of azolium salts along with the π-donor strength of the C carbene in L2 and L3-Zr moieties. The reactivity with the more acidic azolium salts (H 3 L2/3) and the destabilized Zr-X trans to NHC carbene bond results in a significant increase in the amount of homoleptic compounds generating HCl. The released HCl reacts preferentially with the heteroleptic intermediates having non-planar NHC ligands (i.e. L2/3) promoting the formation of zwitterionic complexes. The in situ deprotonation of the isolated zwitterionic (κ 2 -O,O-HL3)ZrCl 2 (OiPr) compound by using Ag 2 O gives the homoleptic complex as the major component along with a bimetallic hydroxo-bridged [(κ 3 -O,C,O-L3)Zr(μ-OH)(OiPr)] 2 compound. Of particular interest is that only the heteroleptic NHC-Zr(iv) complexes were identified to be active and highly selective towards the copolymerization of CHO with CO 2 independently of the co-catalysts used (both anionic and neutral) under mild conditions (P CO 2 < 1 bar, T = 60 °C), and gave atactic and completely alternating copolymers in a controlled manner (M w /M n ≈ 1.3-1.8). In contrast, the isolated homoleptic, zwitterionic and bimetallic zirconium species were found to be inactive under similar reaction conditions. Although the activity found for NHC-Zr(iv) complexes is nearly of the same order of magnitude as that of the NHC-Ti(iv) analogues, these results are the first examples of tetravalent zirconium complexes achieving high selectivity (99% in PCHC) in the catalyzed copolymerization of CHO with CO 2 .

  17. Chlorination of UO 2, PuO 2 and rare earth oxides using ZrCl 4 in LiCl-KCl eutectic melt

    NASA Astrophysics Data System (ADS)

    Sakamura, Yoshiharu; Inoue, Tadashi; Iwai, Takashi; Moriyama, Hirotake

    2005-04-01

    A new chlorination method using ZrCl 4 in a molten salt bath has been investigated for the pyrometallurgical reprocessing of nuclear fuels. ZrCl 4 has a high reactivity with oxygen but is not corrosive to refractory metals such as steel. Rare earth oxides (La 2O 3, CeO 2, Nd 2O 3 and Y 2O 3) and actinide oxides (UO 2 and PuO 2) were allowed to react with ZrCl 4 in a LiCl-KCl eutectic salt at 773 K to give a metal chloride solution and a precipitate of ZrO 2. An addition of zirconium metal as a reductant was effective in chlorinating the dioxides. When the oxides were in powder form, the reaction was observed to progress rapidly. Cyclic voltammetry provided a convenient way of establishing when the reaction was completed. It was demonstrated that the ZrCl 4 chlorination method, free from corrosive gas, was very simple and useful.

  18. Phase separation of metal-added corium and its effect on a steam explosion

    NASA Astrophysics Data System (ADS)

    Min, B. T.; Kim, J. H.; Hong, S. W.; Hong, S. H.; Park, I. K.; Song, J. H.; Kim, H. D.

    2008-07-01

    To simulate a relocation of molten core material and its interaction phenomenon with water during a severe accident in a nuclear reactor, a typical corium of UO 2/ZrO 2/Zr/Stainless steel mixed at a 62 wt%, 15 wt%, 12 wt% and 11 wt%, respectively, was melted and then cooled down to become a solidified ingot. It was shown that the molten corium was separated into two layers, of which the upper layer was oxide mixtures and the lower layer was metal alloys. The upper layer was UO 2 and ZrO 2 and the lower layer mostly consisted of metal mixtures such as uranium, zirconium and stainless steel. Iron content varied with the positions and about a half of it existed as an alloy such as Fe 2U. Uranium metal was produced by reduction of UO 2 by zirconium metal. The average densities of the upper oxide layer and the lower metal layer were 8.802 and 9.411 g/cm 3, respectively. In another test, metal-added molten corium was poured into water and it showed that a steam explosion could occur by applying an external trigger.

  19. Development and property evaluation of nuclear grade wrought FeCrAl fuel cladding for light water reactors

    DOE PAGES

    Yamamoto, Yukinori; Pint, Bruce A.; Terrani, Kurt A.; ...

    2015-10-19

    Development of nuclear grade, iron-based wrought FeCrAl alloys has been initiated for light water reactor (LWR) fuel cladding to serve as a substitute for zirconium-based alloys with enhanced accident tolerance. Ferritic alloys with sufficient chromium and aluminum additions can exhibit significantly improved oxidation kinetics in high-temperature steam environments when compared to zirconium-based alloys. In the first phase, a set of model FeCrAl alloys containing 10–20Cr, 3–5Al, and 0–0.12Y in weight percent, were prepared by conventional arc-melting and hot-working processes to explore the effect of composition on the properties of FeCrAlY alloys. It was found that the tensile properties were insensitivemore » to the alloy compositions studied; however, the steam oxidation resistance strongly depended on both the chromium and the aluminum contents. The second phase development focused on strengthening Fe-13Cr-5Al with minor alloying additions of molybdenum, niobium, and silicon. Combined with an optimized thermo-mechanical treatment, a thermally stable microstructure was produced with improved tensile properties at temperatures up to 741°C.« less

  20. 40 CFR 721.10601 - Lanthanum lead titanium zirconium oxide.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ... systems). (iii) Release to water. Requirements as specified in § 721.90 (a)(4), (b)(4), and (c)(4) (Where N=8, and 8 is an aggregate of releases for the following substances: Lead strontium titanium...-271; CAS No. 1262279-31-1); Calcium cobalt lead strontium titanium tungsten oxide (PMN P-11-272; CAS...

  1. 40 CFR 721.10601 - Lanthanum lead titanium zirconium oxide.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ... systems). (iii) Release to water. Requirements as specified in § 721.90 (a)(4), (b)(4), and (c)(4) (Where N=8, and 8 is an aggregate of releases for the following substances: Lead strontium titanium...-271; CAS No. 1262279-31-1); Calcium cobalt lead strontium titanium tungsten oxide (PMN P-11-272; CAS...

  2. Preferable removal of phosphate from water using hydrous zirconium oxide-based nanocomposite of high stability.

    PubMed

    Chen, Liang; Zhao, Xin; Pan, Bingcai; Zhang, Weixian; Hua, Ming; Lv, Lu; Zhang, Weiming

    2015-03-02

    In this study, we employed a new nanocomposite adsorbent HZO-201, which featured high stability under varying solution chemistry, for preferable removal of phosphate from synthetic solution and a real effluent. An anion exchange resin (D-201) was employed as the host of HZO-201, where nano-hydrous zirconium oxide (HZO) was encapsulated as the active species. D-201 binds phosphate through nonspecific electrostatic affinity, whereas the loaded HZO nanoparticles capture phosphate through formation of the inner-sphere complexes. Quantitative contribution of both species to phosphate adsorption was predicted based on the double-Langmuir model. Preferable removal of phosphate by HZO-201 was observed in the presence of the competing anions at higher levels (Cl(-), NO3(-), SO4(2-), HCO3(-)). Fixed-bed adsorption indicated that the effective volume capacity of a synthetic water (2.0 mg P-PO4(3-)/L) by using HZO-201 was ∼1600 BV in the first run (<0.5mg P-PO4(3-)/L), comparable to Fe(III)-based nanocomposite HFO-201 (∼1500 BV) and much larger than D-201 (<250 BV). The exhausted HZO-201 can be in situ regenerated by using a binary NaOH-NaCl solution for cyclic runs, whether fed with the synthetic solution or real effluent. In general, HZO-201 is a promising alternative to Fe(III)-based adsorbents for trace phosphate removal from effluent particularly at acidic pH. Copyright © 2014 Elsevier B.V. All rights reserved.

  3. Preliminary investigation of zirconium boride ceramals for gas-turbine blade applications

    NASA Technical Reports Server (NTRS)

    Hoffman, Charles A

    1953-01-01

    Zirconium boride ZrB2 ceramals were investigated for possible gas-turbine-blade application. Included in the study were thermal shock evaluations of disks, preliminary turbine-blade operation, and observations of oxidation resistance. Thermal shock disks of the following three compositions were studied: (a) 97.5 percent ZrB2 plus 2.5 percent B by weight; (b) 92.5 percent ZrB2 plus 7.5 percent B by weight; and (c) 100 percent ZrB2. Thermal shock disks were quenched from temperatures of 1800 degrees, 2000 degrees, 2200 degrees, and 2400 degrees F. The life of turbine blades containing 93 percent ZrB2 plus 7 percent B by weight was determined in gas-turbine tests. The blades were run at approximately 1600 degrees F and 15,000 to 26,000 rpm. The thermal shock resistance of the 97.5 percent ZrB2 plus 2.5 percent boron ceramals compares favorably with that of TiC plus Co and TiC plus Ni ceramals. Oxidation of the disks during the thermal shock evaluation was slight for the comparatively short time (8.3 hr) up through 2000 degrees F. Oxidation of a specimen was severe, however, after 100 hours at 2000 degrees F. The turbine blade performance evaluation of the 93 percent ZrB2 plus 7 percent B composition was preliminary in scope ; no conclusions can be drawn.

  4. Electrospinning of ceramic nanofibers

    NASA Astrophysics Data System (ADS)

    Eick, Benjamin M.

    Silicon Carbide (SiC) nanofibers of diameters as low as 20 nm are fabricated. The fibers were produced through the electrostatic spinning of the preceramic poly(carbomethylsilane) with pyrolysis to ceramic. A new technique was used where the preceramic was blended with polystyrene (PS) and, subsequent to electrospinning, was exposed to UV to crosslink the PS and prevent fibers flowing during pyrolysis. Electrospun SiC fibers were characterized by FTIR, TGA-DTA, SEM, TEM, XRD, and SAED. Fibers were shown to be polycrystalline and nanograined with alpha-SiC 15R polytype being dominant, where commercial fiber production methods form beta-SiC 3C. Pyrolysis of the bulk polymer blend to SiC produced alpha-SiC 15R as the dominant polytype with larger grains showing that electrospinning nanofibers affects resultant crystallinity. Fibers produced were shown to have a core-shell structure of an oxide scale that was variable by pyrolysis conditions. Metal oxide powders (chromium oxide, cobalt oxide, iron oxide, silicon oxide, tantalum oxide, titanium oxide, tungsten oxide, vanadium oxide, and zirconium oxide), were converted to metal carbide powders and metal nitride powders by the process of carbothermal reduction (CTR). Synthetic pitch was explored as an alternative to graphite which is a common carbon source for CTR. It was shown via characterization with XRD that pitch performs as well and in some cases better than graphite and is therefore a viable alternative in CTR. Conversion of metal oxide powders with pitch led to conversion of sol-gel based metal oxide nanofibers produced by electrospinning. Pitch was soluble in the solutions xv that were electrospun allowing for intimate contact between the sol-gel and the carbon source for CTR. This method became a two step processing method to produce metal carbide and nitride nanofibers: first electrospin sol-gel based metal oxide nanofibers and subsequently pyrolize them in the manner of CTR to transform them. Results indicate that this method was capable of transforming hafnium, niobium, tantalum, titanium, vanadium, and zirconium sol-gel nanofibers to metal carbides and nitrides.

  5. Fine-grained zirconium-base material

    DOEpatents

    Van Houten, G.R.

    1974-01-01

    A method is described for making zirconium with inhibited grain growth characteristics, by the process of vacuum melting the zirconium, adding 0.3 to 0.5% carbon, stirring, homogenizing, and cooling. (Official Gazette)

  6. Sample environment for in situ synchrotron corrosion studies of materials in extreme environments

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

    Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Motta, Arthur T.

    A new in situ sample environment has been designed and developed to study the interfacial interactions of nuclear cladding alloys with high temperature steam. The sample environment is particularly optimized for synchrotron X-ray diffraction (XRD) studies for in situ structural analysis. The sample environment is highly corrosion resistant and can be readily adapted for steam environments. The in situ sample environment design complies with G2 ASTM standards for studying corrosion in zirconium and its alloys and offers remote temperature and pressure monitoring during the in situ data collection. The use of the in situ sample environment is exemplified by monitoringmore » the oxidation of metallic zirconium during exposure to steam at 350°C. Finally, the in situ sample environment provides a powerful tool for fundamental understanding of corrosion mechanisms by elucidating the substoichiometric oxide phases formed during early stages of corrosion, which can provide a better understanding the oxidation process.« less

  7. Semimicrodetermination of combined tantalum and niobium with selenous acid

    USGS Publications Warehouse

    Grimaldi, F.S.; Schnepfe, M.

    1959-01-01

    Tantalum and niobium are separated and determined gravimetrically by precipitation with selenous acid from highly acidic solutions in the absence of complexing agents. Hydrogen peroxide is used in the preparation of the solution and later catalytically destroyed during digestion of the precipitate. From 0.2 to 30 mg., separately or in mixtures, of niobium or tantalum pentoxide can be separated from mixtures containing 100 mg. each of the oxides of scandium, yttrium, cerium, vanadium, molybdenum, iron, aluminum, tin, lead, and bismuth with a single precipitation; and from 30 mg. of titanium dioxide, and 50 mg. each of the oxides of antimony and thorium, when present separately, with three precipitations. At least 50 mg. of uranium(VI) oxide can be separated with a single precipitation when present alone; otherwise, three precipitations may be needed. Zirconium does not interfere when the tantalum and niobium contents of the sample are small, but in general, zirconium as well as tungsten interfere. The method is applied to the determination of the earth acids in tantaloniobate ores.

  8. Sample environment for in situ synchrotron corrosion studies of materials in extreme environments

    DOE PAGES

    Elbakhshwan, Mohamed S.; Gill, Simerjeet K.; Motta, Arthur T.; ...

    2016-10-25

    A new in situ sample environment has been designed and developed to study the interfacial interactions of nuclear cladding alloys with high temperature steam. The sample environment is particularly optimized for synchrotron X-ray diffraction (XRD) studies for in situ structural analysis. The sample environment is highly corrosion resistant and can be readily adapted for steam environments. The in situ sample environment design complies with G2 ASTM standards for studying corrosion in zirconium and its alloys and offers remote temperature and pressure monitoring during the in situ data collection. The use of the in situ sample environment is exemplified by monitoringmore » the oxidation of metallic zirconium during exposure to steam at 350°C. Finally, the in situ sample environment provides a powerful tool for fundamental understanding of corrosion mechanisms by elucidating the substoichiometric oxide phases formed during early stages of corrosion, which can provide a better understanding the oxidation process.« less

  9. In vitro assessment of artifacts induced by titanium, titanium-zirconium and zirconium dioxide implants in cone-beam computed tomography.

    PubMed

    Sancho-Puchades, Manuel; Hämmerle, Christoph H F; Benic, Goran I

    2015-10-01

    The aim of this study was to test whether or not the intensity of artifacts around implants in cone-beam computed tomography (CBCT) differs between titanium, titanium-zirconium and zirconium dioxide implants. Twenty models of a human mandible, each containing one implant in the single-tooth gap position 45, were cast in dental stone. Five test models were produced for each of the following implant types: titanium 4.1 mm diameter (Ti4.1 ), titanium 3.3 mm diameter (Ti3.3 ), titanium-zirconium 3.3 mm diameter (TiZr3.3 ) and zirconium dioxide 3.5-4.5 mm diameter (ZrO3.5-4.5 ) implants. For control purposes, three models without implants were produced. Each model was scanned using a CBCT device. Gray values (GV) were recorded at eight circumferential positions around the implants at 0.5 mm, 1 mm and 2 mm from the implant surface (GVT est ). GV were assessed in the corresponding volumes of interest (VOI) in the control models without implants (GVC ontrol ). Differences of gray values (ΔGV) between GVT est and GVC ontrol were calculated as percentages. One-way ANOVA and post hoc tests were applied to detect differences between implant types. Mean ΔGV for ZrO3.5-4.5 presented the highest absolute values, generally followed by TiZr3.3 , Ti4.1 and Ti3.3 implants. The differences of ΔGV between ZrO3.5-4.5 and the remaining groups were statistically significant in the majority of the VOI (P ≤ 0.0167). ΔGV for TiZr3.3 , Ti4.1 and Ti3.3 implants did not differ significantly in the most VOI. For all implant types, ΔGV showed positive values buccally, mesio-buccally, lingually and disto-lingually, whereas negative values were detected mesially and distally. Zirconium dioxide implants generate significantly more artifacts as compared to titanium and titanium-zirconium implants. The intensity of artifacts around zirconium dioxide implants exhibited in average the threefold in comparison with titanium implants. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

  10. Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility

    PubMed Central

    Li, H.F.; Zhou, F.Y.; Li, L.; Zheng, Y.F.

    2016-01-01

    In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are <1%, much lower than 5%, the safe value for biomaterials according to ISO 10993-4 standard. Compared with conventional biomedical 316L stainless steel, Co–Cr alloys and Ti-based alloys, the magnetic susceptibilities of the zirconium-ruthenium alloys (1.25 × 10−6 cm3·g−1–1.29 × 10−6 cm3·g−1 for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti–6Al–4V, ~3.5 × 10−6 cm3·g−1, CP Ti and Ti–6Al–7Nb, ~3.0 × 10−6 cm3·g−1), and one-sixth that of Co–Cr alloys (Co–Cr–Mo, ~7.7 × 10−6 cm3·g−1). Among the Zr–Ru alloy series, Zr–1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr–Ru alloy system as therapeutic devices under MRI diagnostics environments. PMID:27090955

  11. Overcoming the crystallization and designability issues in the ultrastable zirconium phosphonate framework system

    DOE PAGES

    Zheng, Tao; Yang, Zaixing; Gui, Daxiang; ...

    2017-05-30

    Metal-organic frameworks (MOFs) based on zirconium phosphonates exhibit superior chemical stability suitable for applications under harsh conditions. These compounds mostly exist as poorly crystallized precipitates, and precise structural information has therefore remained elusive. Furthermore, a zero-dimensional zirconium phosphonate cluster acting as secondary building unit has been lacking, leading to poor designability in this system. We overcome these challenges and obtain single crystals of three zirconium phosphonates that are suitable for structural analysis. Furthermore, these compounds are built by previously unknown isolated zirconium phosphonate clusters and exhibit combined high porosity and ultrastability even in fuming acids. SZ-2 possesses the largest voidmore » volume recorded in zirconium phosphonates and SZ-3 represents the most porous crystalline zirconium phosphonate and the only porous MOF material reported to survive in aqua regia. SZ-2 and SZ-3 can effectively remove uranyl ions from aqueous solutions over a wide pH range, and we have elucidated the removal mechanism.« less

  12. Overcoming the crystallization and designability issues in the ultrastable zirconium phosphonate framework system

    PubMed Central

    Zheng, Tao; Yang, Zaixing; Gui, Daxiang; Liu, Zhiyong; Wang, Xiangxiang; Dai, Xing; Liu, Shengtang; Zhang, Linjuan; Gao, Yang; Chen, Lanhua; Sheng, Daopeng; Wang, Yanlong; Diwu, Juan; Wang, Jianqiang; Zhou, Ruhong; Chai, Zhifang; Albrecht-Schmitt, Thomas E.; Wang, Shuao

    2017-01-01

    Metal-organic frameworks (MOFs) based on zirconium phosphonates exhibit superior chemical stability suitable for applications under harsh conditions. These compounds mostly exist as poorly crystallized precipitates, and precise structural information has therefore remained elusive. Furthermore, a zero-dimensional zirconium phosphonate cluster acting as secondary building unit has been lacking, leading to poor designability in this system. Herein, we overcome these challenges and obtain single crystals of three zirconium phosphonates that are suitable for structural analysis. These compounds are built by previously unknown isolated zirconium phosphonate clusters and exhibit combined high porosity and ultrastability even in fuming acids. SZ-2 possesses the largest void volume recorded in zirconium phosphonates and SZ-3 represents the most porous crystalline zirconium phosphonate and the only porous MOF material reported to survive in aqua regia. SZ-2 and SZ-3 can effectively remove uranyl ions from aqueous solutions over a wide pH range, and we have elucidated the removal mechanism. PMID:28555656

  13. Overcoming the crystallization and designability issues in the ultrastable zirconium phosphonate framework system

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

    Zheng, Tao; Yang, Zaixing; Gui, Daxiang

    Metal-organic frameworks (MOFs) based on zirconium phosphonates exhibit superior chemical stability suitable for applications under harsh conditions. These compounds mostly exist as poorly crystallized precipitates, and precise structural information has therefore remained elusive. Furthermore, a zero-dimensional zirconium phosphonate cluster acting as secondary building unit has been lacking, leading to poor designability in this system. We overcome these challenges and obtain single crystals of three zirconium phosphonates that are suitable for structural analysis. Furthermore, these compounds are built by previously unknown isolated zirconium phosphonate clusters and exhibit combined high porosity and ultrastability even in fuming acids. SZ-2 possesses the largest voidmore » volume recorded in zirconium phosphonates and SZ-3 represents the most porous crystalline zirconium phosphonate and the only porous MOF material reported to survive in aqua regia. SZ-2 and SZ-3 can effectively remove uranyl ions from aqueous solutions over a wide pH range, and we have elucidated the removal mechanism.« less

  14. Process for the manufacture of an attrition resistant sorbent used for gas desulfurization

    DOEpatents

    Venkataramani, Venkat S.; Ayala, Raul E.

    2003-09-16

    This process produces a sorbent for use in desulfurization of coal gas. A zinc titanate compound and a metal oxide are mixed by milling the compounds in an aqueous medium, the resulting mixture is dried and then calcined, crushed, sleved and formed into pellets for use in a moving-bed reactor. Metal oxides suitable for use as an additive in this process include: magnesium oxide, magnesium oxide plus molybdenum oxide, calcium oxide, yttrium oxide, hafnium oxide, zirconium oxide, cupric oxide, and tin oxide. The resulting sorbent has a percentage of the original zinc or titanium ions substituted for the oxide metal of the chosen additive.

  15. Hip Dislocation Increases Roughness of Oxidized Zirconium Femoral Heads in Total Hip Arthroplasty: An Analysis of 59 Retrievals

    PubMed Central

    Moussa, Mohamed E.; Esposito, Christina I.; Elpers, Marcella E.; Wright, Timothy M.; Padgett, Douglas E.

    2014-01-01

    The aims of this study were to assess damage on the surface of retrieved oxidized zirconium metal (OxZr) femoral heads, to measure surface roughness of scratches, and to evaluate the extent of surface effacement using scanning electron microscopy (SEM). Ceramic zirconia-toughened alumina (ZTA) heads were analyzed for comparison. OxZr femoral heads explanted for recurrent dislocation had the most severe damage (p<0.001). The median surface roughness of damaged OxZr femoral heads was 1.49μm, compared to 0.084μm for damaged ZTA heads and 0.052μm for undamaged OxZr (p<0.001). This may be of clinical concern because increased surface roughness has the potential to increase the wear of polyethylene liners articulating against these OxZr heads in THA. PMID:25443362

  16. Analysis of Operating Strategies Using Different Target Designs For 238Pu Production

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

    Thomas, Tomcy; Sherman, Steven R; Sawhney, Dr. Rapinder

    2017-01-01

    An engineering effort is underway to re-establish capability to produce 238Pu oxide at the kilogram scale in the United States. A multi-step batch process is being developed to produce this important material. Recently, a portion of this process was studied using discrete-event simulation tools to determine whether the conceptual process might achieve its yearly production goal. The study showed the conceptual process can meet the yearly production goal under some circumstances, but process improvements would be needed to ensure greater likelihood of success. This study extends the work performed previously by examining the effects of changing the reactor target designmore » on the yearly process output. Two new reactor target configurations are considered an aluminum-clad reactor target containing 50% greater 237Np oxide content than the original target, and a zirconium alloy-clad target using no aluminum. The results indicate that use of the new aluminum-clad target configuration may allow the process to achieve the same yearly production goal in less time using fewer targets. If the zirconium alloy-clad target is used, then even fewer targets would be needed to reach the production goal, but some process changes would be required to handle the zirconium cladding. The number of days needed to process a target batch to completion, and the steady state 238Pu oxide production rate, for each configuration are compared to the results from the initial simulation study.« less

  17. Dispersion toughened silicon carbon ceramics

    DOEpatents

    Wei, G.C.

    1984-01-01

    Fracture resistant silicon carbide ceramics are provided by incorporating therein a particulate dispersoid selected from the group consisting of (a) a mixture of boron, carbon and tungsten, (b) a mixture of boron, carbon and molybdenum, (c) a mixture of boron, carbon and titanium carbide, (d) a mixture of aluminum oxide and zirconium oxide, and (e) boron nitride. 4 figures.

  18. Environmentally Friendly Zirconium Oxide Pretreatment

    DTIC Science & Technology

    2013-05-01

    during the conversion of the highly soluble hexavalent chromate ions to an inert and relatively insoluble trivalent chromium oxide layer. Depletion of...are being used commercially in automotive and other industrial operations as replacements to hexavalent chromium -based and zinc phosphate...Society for Testing and Materials AVCRAD Aviation Classification Repair Activity Depot Chrome (VI) Hexavalent Chromium CRS Cold Rolled Steel

  19. CONTROL ROD FOR A NUCLEAR REACTOR AND METHOD OF PREPARATION

    DOEpatents

    Hausner, H.H.

    1958-12-30

    BS>An improved control rod is presented for a nuclear reactor. This control rod is comprised of a rare earth metal oxide or rare earth metal carbide such as gadolinium oxide or gadolinium carbide, uniformly distributed in a metal matrix having a low cross sectional area of absorption for thermal neutrons, such as aluminum, beryllium, and zirconium.

  20. Hydrogen pickup mechanism of zirconium alloys

    NASA Astrophysics Data System (ADS)

    Couet, Adrien

    Although the optimization of zirconium based alloys has led to significant improvements in hydrogen pickup and corrosion resistance, the mechanisms by which such alloy improvements occur are still not well understood. In an effort to understand such mechanisms, a systematic study of the alloy effect on hydrogen pickup is conducted, using advanced characterization techniques to rationalize precise measurements of hydrogen pickup. The hydrogen pick-up fraction is accurately measured for a specially designed set of commercial and model alloys to investigate the effects of alloying elements, microstructure and corrosion kinetics on hydrogen uptake. Two different techniques to measure hydrogen concentrations were used: a destructive technique, Vacuum Hot Extraction, and a non-destructive one, Cold Neutron Prompt Gamma Activation Analysis. The results indicate that hydrogen pickup varies not only from alloy to alloy but also during the corrosion process for a given alloy. For instance Zircaloy type alloys show high hydrogen pickup fraction and sub-parabolic oxidation kinetics whereas ZrNb alloys show lower hydrogen pickup fraction and close to parabolic oxidation kinetics. Hypothesis is made that hydrogen pickup result from the need to balance charge during the corrosion reaction, such that the pickup of hydrogen is directly related to (and indivisible of) the corrosion mechanism and decreases when the rate of electron transport or oxide electronic conductivity sigmao xe through the protective oxide increases. According to this hypothesis, alloying elements (either in solid solution or in precipitates) embedded in the oxide as well as space charge variations in the oxide would impact the hydrogen pick-up fraction by modifying sigmaox e, which drives oxidation and hydriding kinetics. Dedicated experiments and modelling were performed to assess and validate these hypotheses. In-situ electrochemical impedance spectroscopy (EIS) experiments were performed on Zircaloy-4 tubes to directly measure the evolution of sigma oxe as function of exposure time. The results show that sigmao xe decreases as function of exposure time and that its variations are directly correlated to the instantaneous hydrogen pickup fraction variations. The electron transport through the oxide layer is thus altered as the oxide grows, reasons for which are yet to be exactly determined. Preliminary results also show that sigma oxe of ZrNb alloys would be much higher compared with Zircaloy-4. Thus, it is confirmed that sigmaox e is a key parameter in the hydrogen and oxidation mechanism. Because the mechanism whereby alloying elements are incorporated into the oxide layer is critical to changing sigmao xe, the evolution of the oxidation state of two common alloying elements, Fe and Nb, when incorporated into the growing oxide layers is investigated using X-Ray Absorption Near-Edge Spectroscopy (XANES) using micro-beam synchrotron radiation on cross sectional oxide samples. The results show that the oxidation of both Fe and Nb is delayed in the oxide layer compared to that of Zr, and that this oxidation delay is related to the variations of the instantaneous hydrogen pick-up fraction with exposure time. The evolution of Nb oxidation as function of oxide depth is also compatible with space charge compensation in the oxide and with an increase in sigmaox e of ZrNb alloys compared to Zircaloys. Finally, various successively complex models from the well-known Wagner oxidation theory to the more complex effect of space charge on oxidation kinetics have been developed. The general purpose of the modeling effort is to provide a rationale for the sub-parabolic oxidation kinetics and demonstrate the correlation with hydrogen pickup fraction. It is directly demonstrated that parabolic oxidation kinetics is associated with high sigmao xe and low space charges in the oxide whereas sub-parabolic oxidation kinetics is associated with lower sigmaox e and higher space charge in the oxide. All these observations helped us to propose a general corrosion mechanism of zirconium alloys involving both oxidation and hydrogen pickup mechanism to better understand and predict the effect of alloying additions on the behavior of zirconium alloys.

  1. Towards Isotropic Vortex Pinning in YBCO Films with Double-doping BHO-Y2O3 and BZO-Y2O3 Artificial Pining Centers

    NASA Astrophysics Data System (ADS)

    Gautam, Bibek; Sebastian, Mary Ann; Chen, Shihong; Haugan, Timothy; Chen, Yanbin; Xing, Zhongwen; Prestigiacomo, Joseph; Osofsky, Mike; Wu, Judy

    2017-12-01

    Strong and isotropic vortex pinning landscape is demanded for high field applications of YaBa2Cu3O7-x (YBCO) epitaxial thin films. Double-doping (DD) of artificial pinning centers (APCs) of mixed morphologies has been identified as a viable approach for this purpose. This work presents a comparative study on the transport critical current density J c (H, θ) of 3.0 vol.%Y2O3+2.0 (or 6.0) vol.% BaZrO3 (BZO DD) and 3.0 vol.%Y2O3+ 2.0 (or 6.0) vol.% BaHfO3 (BHO DD) films. Based on the elastic strain model, BaHfO3 (BHO) nanorods have lower rigidity than their BaZrO3 (BZO) counterparts, which means their c-axis alignment is more susceptible to the local strain generated by the secondary dopant of Y2O3. Considering the increasing strain field with higher BZO (or BHO doping), the higher susceptibility may result in a large portion of the BHO APCs moving away from perfect c-axis alignment and enhancing isotropic pinning with respect to the H orientation. This is confirmed since the BHO DD films illustrate a less pronounced J c peak at H//c-axis and hence more isotropic J c(θ) than their BZO DD counterparts. At 9.0 T, the variation of the J c across the entire θ range (0-90 degree) is less than 18% for the BHO DD film, in contrast to about 100% for the 2.0 vol.% BZO DD counterpart. At the higher BHO concentration of 6.0 vol.%, this higher tunability of the Y2O3 leads to increased ab-plane aligned BHO APCs and hence enhanced J c at H//ab-plane.

  2. Effect of ZrO2 Source Variations on PbZrO3 - PbTiO3 Piezoelectric Properties.

    DTIC Science & Technology

    1980-01-15

    wfatevalatediohryand wetbnde led/1cn Dipatont aod blNdigohvrywssontoyedP- aeilwt Coe 71 Wsingtongq D roC., e 20390 dnit Z-T ID 5,RM 1473 EDITION OF CAIO NOVGADN...PZ-PT 19 D . Coprecipitation of PZ-PT 26 IV SUMMARY AND CONCLUSIONS 33 V ACKNOWLEDGEMENTS 34 46 0 I 347602V ! _ _ A List of Illustrations Figure Page 1...chloride solution may be processed further to give high-purity zirconium (or zirconyl) compounds, such as the oxide, fluoride, nitrate , sulfate and

  3. First principles study of carbon nanostructures, transition metal dichalcogenides, and magnetoelectric interfaces

    NASA Astrophysics Data System (ADS)

    Hammouri, Mahmoud

    Perovskite oxides such as lead zirconate titanate, lanthanum manganite and two dimensional, atomically thick materials such as graphene, carbon nanotubes, graphene nanoribbon, and transition-metal dichalcogenides (TMDs) received intensive attention due to their electronic, magnetic, and transport properties. Understanding the properties and structure of these materials in solid state is a longstanding scientific challenge, especially for experimentalists. Using state-of-the-art density functional theory, different properties can be explained with an excellent match with experiments. This thesis presents an Ab initio density functional theory study of the electronic, magnetic, and transport properties of nanostructure systems. Nanostructures studied in this thesis include graphene, carbon nanotubes, graphene nanoribbons, zirconium disulfide, and La0.67Sr0.33MnO3/PbZr 02 Ti0.8O3 (LSMO/PZT) (100) interface. I investigated the mechanism of chemical functionalization of the side walls of carbon nanotubes by benzyne molecules. Binding energies, geometries, and electronic structure changes due to this functionalization are examined in detail. The binding energies between benzyne molecules and carbon nanotubes are found to be inversely proportional to nanotube diameter. We also studied the properties of graphene nanoribbons under compressions. Our study showed that the band gaps of graphene nanoribbons were strongly affected by applied compression. In addition, we found that the effect of compression has a strong influence on the IV-characteristic. We also investigated the effect of uniaxial strain on the electronic and magnetic properties of zirconium disulfide nanoribbons. Our calculation showed that the magnetization of zirconium disulfide nanoribbons can be switched on and off by the applied strain. In the last part, we studied the properties of the interface between two perovskite oxides, lead zirconate titanate and lanthanum strontium manganite. Our study demonstrated that the magnetoelectric coupling observed at this interface can be explained by the magnetic reconstruction of lanthanum strontium manganite.

  4. Conversion of NO with a catalytic packed-bed dielectric barrier discharge reactor

    NASA Astrophysics Data System (ADS)

    Xu, CAO; Weixuan, ZHAO; Renxi, ZHANG; Huiqi, HOU; Shanping, CHEN; Ruina, ZHANG

    2017-11-01

    This paper discusses the conversion of nitric oxide (NO) with a low-temperature plasma induced by a catalytic packed-bed dielectric barrier discharge (DBD) reactor. Alumina oxide (Al2O3), glass (SiO2) and zirconium oxide (ZrO2), three different spherical packed materials of the same size, were each present in the DBD reactor. The NO conversion under varying input voltage and specific energy density, and the effects of catalysts (titanium dioxide (TiO2) and manganese oxide (MnO x ) coated on Al2O3) on NO conversion were investigated. The experimental results showed that NO conversion was greatly enhanced in the presence of packed materials in the reactor, and the catalytic packed bed of MnO x /Al2O3 showed better performance than that of TiO2/Al2O3. The surface and crystal structures of the materials and catalysts were characterized through scanning electron microscopy analysis. The final products were clearly observed by a Fourier transform infrared spectrometer and provided a better understanding of NO conversion.

  5. Enhanced removal of arsenic from a highly laden industrial effluent using a combined coprecipitation/nano-adsorption process.

    PubMed

    Jiang, Yingnan; Hua, Ming; Wu, Bian; Ma, Hongrui; Pan, Bingcai; Zhang, Quanxing

    2014-05-01

    Effective arsenic removal from highly laden industrial wastewater is an important but challenging task. Here, a combined coprecipitation/nano-adsorption process, with ferric chloride and calcium chloride as coprecipitation agents and polymer-based nanocomposite as selective adsorbent, has been validated for arsenic removal from tungsten-smelting wastewater. On the basis of operating optimization, a binary FeCl3 (520 mg/L)-CaCl2 (300 mg/L) coprecipitation agent could remove more than 93% arsenic from the wastewater. The resulting precipitate has proved environmental safety based on leaching toxicity test. Fixed-bed column packed with zirconium or ferric-oxide-loaded nanocomposite was employed for further elimination of arsenic in coprecipitated effluent, resulting in a significant decrease of arsenic (from 0.96 to less than 0.5 mg/L). The working capacity of zirconium-loaded nanocomposite was 220 bed volumes per run, much higher than that of ferric-loaded nanocomposite (40 bed volumes per run). The exhausted zirconium-loaded nanocomposite could be efficiently in situ regenerated with a binary NaOH-NaCl solution for reuse without any significant capacity loss. The results validated the combinational coprecipitation/nano-adsorption process to be a potential alternative for effective arsenic removal from highly laden industrial effluent.

  6. Adsorption of phosphate from aqueous solution using iron-zirconium modified activated carbon nanofiber: Performance and mechanism.

    PubMed

    Xiong, Weiping; Tong, Jing; Yang, Zhaohui; Zeng, Guangming; Zhou, Yaoyu; Wang, Dongbo; Song, Peipei; Xu, Rui; Zhang, Chen; Cheng, Min

    2017-05-01

    Phosphate (P) removal is significant for the prevention of eutrophication in natural waters. In this paper, a novel adsorbent for the removal of P from aqueous solution was synthesized by loading zirconium oxide and iron oxide onto activated carbon nanofiber (ACF-ZrFe) simultaneously. The adsorbent was characterized by scanning electron microscopy (SEM), Fourier transform infrared (FT-IR) spectroscopy and X-ray photoelectron spectroscopy (XPS). The results showed that P adsorption was highly pH dependent and the optimum pH was found to be 4.0. The isotherm of adsorption could be well described by the Langmuir model and the maximum P adsorption capacity was estimated to be 26.3mgP/g at 25°C. The kinetic data were well fitted to the pseudo-second-order equation, indicating that chemical sorption was the rate-limiting step. Moreover, co-existing ions including sulfate (SO 4 2- ), chloride (Cl - ), nitrate (NO 3 - ) and fluoride (F - ) exhibited a distinct effect on P adsorption with the order of F - >NO 3 - >Cl - >SO 4 2- . Further investigations by FT-IR spectroscopy and pH variations associated with the adsorption process revealed that ligands exchange and electrostatic interactions were the dominant mechanisms for P adsorption. The findings reported in this work highlight the potential of using ACF-ZrFe as an effective adsorbent for the removal of P in natural waters. Copyright © 2017 Elsevier Inc. All rights reserved.

  7. Development of a 30 kW Inductively Coupled Plasma Torch Facility for Advanced Aerospace Material Investigations

    DTIC Science & Technology

    2012-02-21

    passive oxidation of zirconium diboride forms zirconia and boron oxide, and the passive oxidation of silicon carbide forms silica and carbon monoxide: ZrB2... silicon carbide composites in the ICP wind tunnels. However, this concept has never been explored as an in situ diagnostic for UHTC materials systems...Process- ing, properties, and arc jet oxidation of hafnium diboride/ silicon carbide ultra high temperature ceramics. J Mater Sci 2004;39:5925–37. 12

  8. Highly regioselective terminal alkynes hydroformylation and Pauson-Khand reaction catalysed by mesoporous organised zirconium oxide based powders.

    PubMed

    Goettmann, Frédéric; Le Floch, Pascal; Sanchez, Clément

    2006-01-14

    Zirconia-silica mesoporous powders act as very efficient heterogeneous catalysts for both alkyne hydroformylation and Pauson-Khand reaction and yield regioselectivities opposite to those usually observed.

  9. Effect of zirconium nitride physical vapor deposition coating on preosteoblast cell adhesion and proliferation onto titanium screws.

    PubMed

    Rizzi, Manuela; Gatti, Giorgio; Migliario, Mario; Marchese, Leonardo; Rocchetti, Vincenzo; Renò, Filippo

    2014-11-01

    Titanium has long been used to produce dental implants. Problems related to its manufacturing, casting, welding, and ceramic application for dental prostheses still limit its use, which highlights the need for technologic improvements. The aim of this in vitro study was to evaluate the biologic performance of titanium dental implants coated with zirconium nitride in a murine preosteoblast cellular model. The purpose of this study was to evaluate the chemical and morphologic characteristics of titanium implants coated with zirconium nitride by means of physical vapor deposition. Chemical and morphologic characterizations were performed by scanning electron microscopy and energy dispersive x-ray spectroscopy, and the bioactivity of the implants was evaluated by cell-counting experiments. Scanning electron microscopy and energy dispersive x-ray spectroscopy analysis found that physical vapor deposition was effective in covering titanium surfaces with zirconium nitride. Murine MC-3T3 preosteoblasts were seeded onto titanium-coated and zirconium nitride-coated screws to evaluate their adhesion and proliferation. These experiments found a significantly higher number of cells adhering and spreading onto zirconium nitride-coated surfaces (P<.05) after 24 hours; after 7 days, both titanium and zirconium nitride surfaces were completely covered with MC-3T3 cells. Analysis of these data indicates that the proposed zirconium nitride coating of titanium implants could make the surface of the titanium more bioactive than uncoated titanium surfaces. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  10. A zirconium dioxide ammonia microsensor integrated with a readout circuit manufactured using the 0.18 μm CMOS process.

    PubMed

    Lin, Guan-Ming; Dai, Ching-Liang; Yang, Ming-Zhi

    2013-03-15

    The study presents an ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated sensor chip consists of a heater, an ammonia sensor and a readout circuit. The ammonia sensor is constructed by a sensitive film and the interdigitated electrodes. The sensitive film is zirconium dioxide that is coated on the interdigitated electrodes. The heater is used to provide a working temperature to the sensitive film. A post-process is employed to remove the sacrificial layer and to coat zirconium dioxide on the sensor. When the sensitive film adsorbs or desorbs ammonia gas, the sensor produces a change in resistance. The readout circuit converts the resistance variation of the sensor into the output voltage. The experiments show that the integrated ammonia sensor has a sensitivity of 4.1 mV/ppm.

  11. Zirconium doped TiO{sub 2} thin films: A promising dielectric layer

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

    Kumar, Arvind; Mondal, Sandip, E-mail: sandipmondal@physics.iisc.ernet.in; Rao, K. S. R. Koteswara

    2016-05-06

    In the present work, we have fabricated the zirconium doped TiO{sub 2} thin (ZTO) films from a facile spin – coating method. The addition of Zirconium in TiO{sub 2} offers conduction band offset to Si and consequently decreased the leakage current density by approximately two orders as compared to pure TiO{sub 2} thin (TO) films. The ZTO thin film shows a high dielectric constant 27 with a very low leakage current density ∼10{sup −8} A/cm{sup 2}. The oxide capacitate, flat band voltage and change in flat band voltage are 172 pF, -1.19 V and 54 mV. The AFM analysis confirmed the compactmore » and pore free flat surface. The RMS surface roughness is found to be 1.5 Å. The ellipsometry analysis also verified the fact with a high refractive index 2.21.« less

  12. Accident tolerant fuel cladding development: Promise, status, and challenges

    NASA Astrophysics Data System (ADS)

    Terrani, Kurt A.

    2018-04-01

    The motivation for transitioning away from zirconium-based fuel cladding in light water reactors to significantly more oxidation-resistant materials, thereby enhancing safety margins during severe accidents, is laid out. A review of the development status for three accident tolerant fuel cladding technologies, namely coated zirconium-based cladding, ferritic alumina-forming alloy cladding, and silicon carbide fiber-reinforced silicon carbide matrix composite cladding, is offered. Technical challenges and data gaps for each of these cladding technologies are highlighted. Full development towards commercial deployment of these technologies is identified as a high priority for the nuclear industry.

  13. Composite catalyst for carbon monoxide and hydrocarbon oxidation

    DOEpatents

    Liu, W.; Flytzani-Stephanopoulos, M.

    1996-03-19

    A method and composition are disclosed for the complete oxidation of carbon monoxide and/or hydrocarbon compounds. The method involves reacting the carbon monoxide and/or hydrocarbons with an oxidizing agent in the presence of a metal oxide composite catalyst. The catalyst is prepared by combining fluorite-type oxygen ion conductors with active transition metals. The fluorite oxide, selected from the group consisting of cerium oxide, zirconium oxide, thorium oxide, hafnium oxide, and uranium oxide, and may be doped by alkaline earth and rare earth oxides. The transition metals, selected from the group consisting of molybdenum, copper, cobalt, manganese, nickel, and silver, are used as additives. The atomic ratio of transition metal to fluorite oxide is less than one.

  14. Composite catalyst for carbon monoxide and hydrocarbon oxidation

    DOEpatents

    Liu, Wei; Flytzani-Stephanopoulos, Maria

    1996-01-01

    A method and composition for the complete oxidation of carbon monoxide and/or hydrocarbon compounds. The method involves reacting the carbon monoxide and/or hydrocarbons with an oxidizing agent in the presence of a metal oxide composite catalyst. The catalyst is prepared by combining fluorite-type oxygen ion conductors with active transition metals. The fluorite oxide, selected from the group consisting of cerium oxide, zirconium oxide, thorium oxide, hafnium oxide, and uranium oxide, and may be doped by alkaline earth and rare earth oxides. The transition metals, selected from the group consisting of molybdnum, copper, cobalt, maganese, nickel, and silver, are used as additives. The atomic ratio of transition metal to fluorite oxide is less than one.

  15. Phase stability and photocatalytic activity of Zr-doped anatase synthesized in miniemulsion

    NASA Astrophysics Data System (ADS)

    Schiller, Renate; Weiss, Clemens K.; Landfester, Katharina

    2010-10-01

    A series of mesoporous anatase-type TiO2 doped with zirconium (0-50 mol% Zr) was synthesized by combining the sol-gel process with the inverse miniemulsion technique. Nanoparticles between 100 and 300 nm were directly prepared from acidic precursor solutions of titanium glycolate (EGMT) and zirconium isopropoxide. The miniemulsion technique is a simple and convenient method to synthesize nanoparticles of homogeneous size because the reactions (here hydrolysis and condensation) take place in the confined space of nanodroplets (several hundreds of nanometres) and therefore in a highly controlled manner. For low doping levels (0-7.1 mol% Zr), ZrxTi1 - xO2 solid solutions were formed where Zr was uniformly dispersed into the anatase framework. For higher amounts of zirconium (Zr >= 7.1 mol%), the crystallization of zirconium titanate (ZrTiO4) occurred at a low temperature of 650 °C and it was obtained as a pure material for 47.4 mol% <= Zr <= 50 mol%. The influence of the amount of zirconium on the crystallinity, crystallite size, phase composition and stability, morphology and specific surface area was investigated. For the characterization transmission electron microscopy (TEM), x-ray diffraction (XRD), nitrogen sorption (BET) and inductively coupled plasma-optical emission spectrometry (ICP-OES) were used. The photocatalytic activity of the crystalline mixed oxides (0-9.4 mol% Zr) was examined for the degradation of methylene blue under UV irradiation.

  16. Adsorption of As(III), As(V) and Cu(II) on zirconium oxide immobilized alginate beads in aqueous phase.

    PubMed

    Kwon, Oh-Hun; Kim, Jong-Oh; Cho, Dong-Wan; Kumar, Rahul; Baek, Seung Han; Kurade, Mayur B; Jeon, Byong-Hun

    2016-10-01

    A composite adsorbent to remove arsenite [As(III)], arsenate [As(V)], and copper [Cu(II)] from aqueous phase was synthesized by immobilizing zirconium oxide on alginate beads (ZOAB). The composition (wt%) of ZOAB (Zr-34.0; O-32.7; C-21.3; Ca-1.0) was confirmed by energy dispersive X-ray (EDX) analysis. Sorption studies were conducted on single and binary sorbate systems, and the effects of contact time, initial adsorbate concentration, and pH on the adsorption performance of ZOAB (pHPZC = 4.3) were monitored. The sorption process for As(III)/As(V) and Cu(II) reached an equilibrium state within 240 h and 24 h, respectively, with maximum sorption capacities of 32.3, 28.5, and 69.9 mg g(-1), respectively. The addition of Cu(II) was favorable for As(V) sorption in contrast to As(III). In the presence of 48.6 mg L(-1) Cu(II), the sorption capacity of As(V) increased from 1.5 to 3.8 mg g(-1) after 240 h. The sorption data for As(III)/As(V) and Cu(II) conformed the Freundlich and Langmuir isotherm models, respectively. The adsorption of As(III), As(V), and Cu(II) followed pseudo second order kinetics. The effect of arsenic species on Cu(II) sorption was insignificant. The results of present study demonstrated that the synthesized sorbent could be useful for the simultaneous removal of both anionic and cationic contaminants from wastewaters. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. On the mechanism of zirconium nitride formation by zirconium, zirconia and yttria burning in air

    NASA Astrophysics Data System (ADS)

    Malikova, Ekaterina; Pautova, Julia; Gromov, Alexander; Monogarov, Konstantin; Larionov, Kirill; Teipel, Ulrich

    2015-10-01

    The combustion of Zr and (Zr+ZrO2) powdery mixtures in air was accompanied by major ZrN stabilization. The synthesis of cheap ZrN with the high yield in air was facile and utile. The influence of Y2O3 additive on the content of ZrN the solid combustion products (SCP) was investigated. The reagents and SCP were analyzed by BET, DTA-TGA, XRD, SEM and EDS. Burning temperature was measured by thermal imager. The yield of ZrN in the SCP has been varied by the time regulation of the combustion process. The burning samples were quenched at a certain time to avoid the re-oxidation of the obtained ZrN by oxygen. The quenching of the burned (Zr+ZrO2) samples with the Y2O3 additive was allowed increasing the ZrN yield in SCP up to 66 wt%. The chemical mechanism of ZrN formation in air was discussed and the probable source of ZrN massive formation is suggested.

  18. Modified zirconium-eriochrome cyanine R determination of fluoride

    USGS Publications Warehouse

    Thatcher, L.L.

    1957-01-01

    The Eriochrome Cyanine R method for determining fluoride in natural water has been modified to provide a single, stable reagent solution, eliminate interference from oxidizing agents, extend the concentration range to 3 p.p.m., and extend the phosphate tolerance. Temperature effect was minimized; sulfate error was eliminated by precipitation. The procedure is sufficiently tolerant to interferences found in natural and polluted waters to permit the elimination of prior distillation for most samples. The method has been applied to 500 samples.

  19. Atom economy and green elimination of nitric oxide using ZrN powders.

    PubMed

    Chen, Ning; Wang, Jigang; Yin, Wenyan; Li, Zhen; Li, Peishen; Guo, Ming; Wang, Qiang; Li, Chunlei; Wang, Changzheng; Chen, Shaowei

    2018-05-01

    Nitric oxide (NO) may cause serious environmental problems, such as acid rain, haze weather, global warming and even death. Herein, a new low-cost, highly efficient and green method for the elimination of NO using zirconium nitride (ZrN) is reported for the first time, which does not produce any waste or any by-product. Relevant experimental parameters, such as reaction temperature and gas concentration, were investigated to explore the reaction mechanism. Interestingly, NO can be easily decomposed into nitrogen (N 2 ) by ZrN powders at 600°C with ZrN simultaneously transformed into zirconium dioxide (ZrO 2 ) gradually. The time for the complete conversion of NO into N 2 was approximately 14 h over 0.5 g of ZrN at a NO concentration of 500 ppm. This green elimination process of NO demonstrated good atom economy and practical significance in mitigating environmental problems.

  20. 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.

  1. In Vivo Wear Performance of Cobalt-Chromium Versus Oxidized Zirconium Femoral Total Knee Replacements.

    PubMed

    Gascoyne, Trevor C; Teeter, Matthew G; Guenther, Leah E; Burnell, Colin D; Bohm, Eric R; Naudie, Douglas R

    2016-01-01

    This study examines the damage and wear on the polyethylene (PE) inserts from 52 retrieved Genesis II total knee replacements to identify differences in tribological performance between matched pairs of cobalt-chromium (CoCr) and oxidized zirconium (OxZr) femoral components. Observer damage scoring and microcomputed tomography were used to quantify PE damage and wear, respectively. No significant differences were found between CoCr and OxZr groups in terms of PE insert damage, surface penetration, or wear. No severe damage such as cracking or delamination was noted on any of the 52 PE inserts. Observer damage scoring did not correlate with penetrative or volumetric PE wear. The more costly OxZr femoral component does not demonstrate clear tribological benefit over the standard CoCr component in the short term with this total knee replacement design. Copyright © 2016 Elsevier Inc. All rights reserved.

  2. Adsorption of phosphate in water using one-step synthesized zirconium-loaded reduced graphene oxide

    NASA Astrophysics Data System (ADS)

    Luo, Xin; Wang, Xiurong; Bao, Shaopan; Liu, Xiawei; Zhang, Weicheng; Fang, Tao

    2016-12-01

    In this account, a one-step green hydrothermal method for zirconium-loaded reduced graphene oxide (RGO-Zr) adsorbent was developed in pure water. It is based on the formation of initially strong-coupling RGO-Zr nanocomposites followed by in situ reduction of GO to RGO during the hydrothermal treatment. The phosphate adsorption performance of the as-prepared nanocomposites was investigated in aqueous environment under various conditions. The characterization results of RGO-Zr nanocomposites showed that ZrO2 was successfully integrated onto the RGO sheets in amorphous. The data from equilibrium phosphate adsorption on RGO-Zr revealed that the adsorption kinetics followed a pseudo-second-order kinetic model, where the adsorption isotherm fitted the Langmuir isotherm model with a maximum adsorption capacity of 27.71 mg P/g at pH 5 and 298 K. The improved phosphate adsorption on RGO-Zr was caused by the dispersion of ZrO2 on the RGO surface. Furthermore, the phosphate adsorption was found insensitive to the increase in pH while it was sensitive to the increase in temperature. The coexisting anions of SO42-, F-, Cl-, NO3- and CO32- affected the phosphate adsorption in a different way. Results suggest that the present RGO-Zr adsorbent has the potential for controlling phosphorus pollution in water.

  3. Single-Crystalline UiO-67-Type Porous Network Stable to Boiling Water, Solvent Loss, and Oxidation.

    PubMed

    Wong, Yan-Lung; Yee, Ka-Kit; Hou, Yun-Long; Li, Jiaqian; Wang, Zuankai; Zeller, Matthias; Hunter, Allen D; Xu, Zhengtao

    2018-06-04

    With methylthio groups flanking the carboxyl groups, the 3,3',5,5'-tetrakis(methylthio)biphenyl dicarboxylate (TMBPD) linker forms a zirconium(IV) carboxylate porous framework featuring the topology of the UiO-67 prototype, i.e., with a face-centered-cubic array of the Zr 6 O 4 (OH) 4 clusters. Thioether functionalization proves valuable because the ZrTMBPD crystal is found to be exceptionally stable not only upon long-term exposure to air but also in boiling water and a broad range of pH conditions. The hydrophobicity of the metal-organic framework can also be tuned by simple H 2 O 2 oxidation, as illustrated in the water contact-angle measurement of the pristine and H 2 O 2 -treated ZrTMBPD solid.

  4. Thermo-luminescence and neutron absorption cross section evaluations of compounds of Lithium based oxide ceramic breeders in Li-Zr-O system

    NASA Astrophysics Data System (ADS)

    Mukherjee, Sumanta; Naik, Yeshwant

    2018-04-01

    Lithium-zirconium based oxides were prepared by combustion route. Thermal analysis (TG and DTA) was used to study the combustion process. The nucleation and growth stages were identified and their activation energies were predicted. The suitability of these oxide breeders was evaluated based on their radiation stability, variation in thermal behavior upon γ irradiation, neutron absorption and tritium breeding characteristics. Nuclear properties of these oxide ceramics were evaluated with a view to use them as efficient neutron absorbers and simultaneously breed tritium. Total neutron absorption cross sections were evaluated as a function of neutron energy in the range of 0 to 20 MeV. Resonant absorption is predicted for the neutron of energy 2.3 keV manly due to contribution from neutron induced nuclear reactions of 7Li in this energy range.

  5. Influence of oxide microstructure on corrosion behavior of zirconium-based model alloys

    NASA Astrophysics Data System (ADS)

    Silva, Marcelo Jose Gomes Da

    The extensive utilization of zirconium-based alloys in fuel cladding and other reactor internal components in the nuclear power industry has led to the continuous improvement of these alloys. At the present moment, demands for better performing nuclear fuel cladding materials are increasing. Also, new reactor designs have been proposed that would require the materials to withstand even more rigorous conditions. One of the factors that limit s fuel cladding utilization in nuclear reactors is uniform corrosion and the consequent hydriding of the fuel. In an attempt to develop mechanistic understanding of the role of alloying elements in the growth of a stable protective oxide, a series of model zirconium-based alloys was prepared (Zr-xFe-yCr, Zr-xCu-yMo, Zr-xNb-ySn, for various x and y, pure Zr and Zircaloy-4) and examined with advanced characterization techniques. The alloys were corrosion tested in autoclaves under three different conditions: 360°C water, 500°C steam and 500°C supercritical water in excess of 400 days. These autoclave testing conditions simulate nuclear reactor environment for both current designs (360°C water) and the new supercritical water reactor (500°C steam and 500°C supercritical water) proposed by the generation-IV initiative. The oxide films formed were systematically examined at the Advanced Photon Source using microbeam synchrotron radiation diffraction and fluorescence of cross-sectional samples to determine the oxide phases present and their crystallographic texture as a function of distance from the metal/oxide interface. Also, the overall texture of the oxide layers was investigated using synchrotron radiation diffraction in frontal geometry. The corrosion kinetics is a function of the alloy system and showed a wide range of behaviors, from immediately unstable oxide growth to stable behavior. The corrosion weight gains from testing at high temperature are a factor of five higher than those measured at 360°C but the protectiveness ranking of the alloys is similar. Measured pole figures from different oxides in different corrosion regimes showed that monoclinic oxides grow in slightly distinct directions: protective oxides grow along the (-904)m pole, whether non-protective oxides grow along or close to the (-302)m pole. The angle in between these two directions ((-904)m and (-302)m) is about 6°. Microbeam synchrotron radiation diffraction and fluorescence was performed in the oxide layers and systematic differences are observed in protective and non-protective oxides, both near the oxide/metal interface and in the bulk of the oxide layers. The non-protective oxide interfaces show a smooth transition from metal to oxide with metal diffraction peaks disappearing as the monoclinic oxide peaks appear. In contrast, in a protective oxide, a complex structure near the oxide/metal interface was seen, showing peaks from Zr 3O suboxide and a highly oriented tetragonal oxide phase with specific orientation relationships with the monoclinic oxide and the base metal. The highly oriented tetragonal phase, only present in protective oxides, is believed to be a precursor to the formation of monoclinic oxide found in the bulk of the oxide layer. This plane may promote stable growth by causing the oxide to form in a manner that maximizes occupation of the substrate surface and minimizes stress accumulation, leading to more stable oxide growth. The association seen in this work of the precursor oxide phase with protective oxides and its orientation relationship with the monoclinic oxide, combined with the difference in oxide growth direction seen between protective and non-protective oxides, is interpreted as evidence that this phase allows a more properly oriented oxide to grow, in a way that minimizes stress accumulation and therefore delays the oxide transition to larger oxide thicknesses.

  6. A regenerable potassium and phosphate sorbent system to enhance dialysis efficacy and device portability: an in vitro study.

    PubMed

    Wester, Maarten; Simonis, Frank; Gerritsen, Karin G; Boer, Walther H; Wodzig, Will K; Kooman, Jeroen P; Joles, Jaap A

    2013-09-01

    Continuous dialysis could provide benefit by constant removal of potassium and phosphate. This study investigates the suitability of specific potassium and phosphate sorbents for incorporation in an extracorporeal device by capacity and regenerability testing. Capacity testing was performed in uraemic plasma. Regenerability was tested for potassium sorbents, with adsorption based on cationic exchange for sodium, with 0.1 M and 1.0 M NaCl. To regenerate phosphate sorbents, with adsorption based on anionic exchange, 0.1 M and 1.0 M NaHCO3 and NaOH were used. Subsequently, sodium polystyrene divinylbenzene sulphonate (RES-A) and iron oxide hydroxide (FeOOH) beads were incorporated in a cartridge for testing in bovine blood using a recirculating blood circuit and a dialysis circuit separated by a high-flux dialyzer (dynamic setup). Preloading was tested to assess whether this could limit calcium and magnesium adsorption. In the batch-binding assays, zirconium phosphate most potently adsorbed potassium (0.44 ± 0.05 mmol/g) and RES-A was the best regenerable potassium sorbent (92.9 ± 5.7% with 0.1 M NaCl). Zirconium oxide hydroxide (ZIR-hydr) most potently adsorbed phosphate (0.23 ± 0.05 mmol/g) and the polymeric amine sevelamer carbonate was the best regenerable sorbent (85.7 ± 5.2% with 0.1 M NaHCO3). In the dynamic setup, a potassium adsorption of 10.72 ± 2.06 mmol in 3 h was achieved using 111 g of RES-A and a phosphate adsorption of 4.73 ± 0.53 mmol in 3 h using 55 g of FeOOH. Calcium and magnesium preloading was shown to reduce the net adsorption in 3 h from 3.57 ± 0.91 to -0.29 ± 1.85 and 1.02 ± 0.05 to -0.31 ± 0.18 mmol, respectively. RES-A and FeOOH are suitable, regenerizable sorbents for potassium and phosphate removal in dialysate regeneration. Use of zirconium carbonate and ZIR-hydr may further increase phosphate adsorption, but may compromise sorbent regenerability. Use of polymeric amines for phosphate adsorption may enhance sorbent regenerability. Calcium and magnesium preloading considerably reduced net adsorption of these ions.

  7. Cation vacancies in ferroelectric PbTiO3 and Pb(Zr,Ti)O3 : A positron annihilation lifetime spectroscopy study

    NASA Astrophysics Data System (ADS)

    Keeble, D. J.; Singh, S.; Mackie, R. A.; Morozov, M.; McGuire, S.; Damjanovic, D.

    2007-10-01

    Positron annihilation lifetime spectroscopy measurements identify A - and B -site cation vacancies in ferroelectric perovskite oxides (ABO3) . Crystal PbTiO3 and ceramic lead zirconium titanate (PZT) were studied and gave consistent values for the lifetime resulting from positron localization at lead vacancies VPb . Positron trapping to B -site vacancies was inferred in PZT. Temperature dependent studies showed that the defect specific trapping rate was higher for VB compared to VPb , consistent with the larger negative charge. Doping PZT with Fe increased the fraction positron trapping to VB compared to VPb -type defects.

  8. Effect of sodium zirconium cyclosilicate on potassium lowering for 28 days among outpatients with hyperkalemia: the HARMONIZE randomized clinical trial.

    PubMed

    Kosiborod, Mikhail; Rasmussen, Henrik S; Lavin, Philip; Qunibi, Wajeh Y; Spinowitz, Bruce; Packham, David; Roger, Simon D; Yang, Alex; Lerma, Edgar; Singh, Bhupinder

    2014-12-03

    Hyperkalemia is a common electrolyte abnormality that may be difficult to manage because of a lack of effective therapies. Sodium zirconium cyclosilicate is a nonabsorbed cation exchanger that selectively binds potassium in the intestine. To evaluate the efficacy and safety of zirconium cyclosilicate for 28 days in patients with hyperkalemia. HARMONIZE was a phase 3, multicenter, randomized, double-blind, placebo-controlled trial evaluating zirconium cyclosilicate in outpatients with hyperkalemia (serum potassium ≥5.1 mEq/L) recruited from 44 sites in the United States, Australia, and South Africa (March-August 2014). Patients (n = 258) received 10 g of zirconium cyclosilicate 3 times daily in the initial 48-hour open-label phase. Patients (n = 237) achieving normokalemia (3.5-5.0 mEq/L) were then randomized to receive zirconium cyclosilicate, 5 g (n = 45 patients), 10 g (n = 51), or 15 g (n = 56), or placebo (n = 85) daily for 28 days. The primary end point was mean serum potassium level in each zirconium cyclosilicate group vs placebo during days 8-29 of the randomized phase. In the open-label phase, serum potassium levels declined from 5.6 mEq/L at baseline to 4.5 mEq/L at 48 hours. Median time to normalization was 2.2 hours, with 84% of patients (95% CI, 79%-88%) achieving normokalemia by 24 hours and 98% (95% CI, 96%-99%) by 48 hours. In the randomized phase, serum potassium was significantly lower during days 8-29 with all 3 zirconium cyclosilicate doses vs placebo (4.8 mEq/L [95% CI, 4.6-4.9], 4.5 mEq/L [95% CI, 4.4-4.6], and 4.4 mEq/L [95% CI, 4.3-4.5] for 5 g, 10 g, and 15 g; 5.1 mEq/L [95% CI, 5.0-5.2] for placebo; P < .001 for all comparisons). The proportion of patients with mean potassium <5.1 mEq/L during days 8-29 was significantly higher in all zirconium cyclosilicate groups vs placebo (36/45 [80%], 45/50 [90%], and 51/54 [94%] for the 5-g, 10-g, and 15-g groups, vs 38/82 [46%] with placebo; P < .001 for each dose vs placebo). Adverse events were comparable between zirconium cyclosilicate and placebo, although edema was more common in the 15-g group (edema incidence: 2/85 [2%], 1/45 [2%], 3/51 [6%], and 8/56 [14%] patients in the placebo, 5-g, 10-g, and 15-g groups). Hypokalemia developed in 5/51 (10%) and 6/56 patients (11%) in the 10-g and 15-g zirconium cyclosilicate groups, vs none in the 5-g or placebo groups. Among outpatients with hyperkalemia, open-label sodium zirconium cyclosilicate reduced serum potassium to normal levels within 48 hours; compared with placebo, all 3 doses of zirconium cyclosilicate resulted in lower potassium levels and a higher proportion of patients with normal potassium levels for up to 28 days. Further studies are needed to evaluate the efficacy and safety of zirconium cyclosilicate beyond 4 weeks and to assess long-term clinical outcomes. clinicaltrials.gov Identifier: NCT02088073.

  9. Electrophoretic fabrication of chitosan-zirconium-oxide nanobiocomposite platform for nucleic acid detection.

    PubMed

    Das, Maumita; Dhand, Chetna; Sumana, Gajjala; Srivastava, A K; Nagarajan, R; Nain, Lata; Iwamoto, M; Manaka, Takaaki; Malhotra, B D

    2011-03-14

    The present work describes electrophoretic fabrication of nanostructured chitosan-zirconium-oxide composite (CHIT-NanoZrO(2)) film (180 nm) onto indium-tin-oxide (ITO)-coated glass plate. This nanobiocomposite film has been explored as immobilization platform for probe DNA specific to M. Tuberculosis as model biomolecule to investigate its sensing characteristics. It is revealed that pH-responsive behavior of CHIT and its cationic skeleton is responsible for the movement of CHIT-NanoZrO(2) colloids toward cathode during electrophoretic deposition. The FT-IR, SEM, TEM, and EDX techniques have been employed for the structural, morphological, and composition analysis of the fabricated electrodes. The morphological studies clearly reveal uniform inter-linking and dispersion of hexagonal nanograins of ZrO(2) (30-50 nm) into the chitosan matrix, resulting in homogeneous nanobiocomposite formation. Electrochemical response measurements of DNA/CHIT-NanoZrO(2)/ITO bioelectrode, carried out using cyclic voltammetry and differential pulse voltammetry, reveal that this bioelectrode can specifically detect complementary target DNA up to 0.00078 μM with sensitivity of 6.38 × 10(-6) AμM(-1).

  10. A simple spectrophotometric method for determination of zirconium or hafnium in selected molybdenum-base alloys

    NASA Technical Reports Server (NTRS)

    Dupraw, W. A.

    1972-01-01

    A simple analytical procedure is described for accurately and precisely determining the zirconium or hafnium content of molybdenum-base alloys. The procedure is based on the reaction of the reagent Arsenazo III with zirconium or hafnium in strong hydrochloric acid solution. The colored complexes of zirconium or hafnium are formed in the presence of molybdenum. Titanium or rhenium in the alloy have no adverse effect on the zirconium or hafnium complex at the following levels in the selected aliquot: Mo, 10 mg; Re, 10 mg; Ti, 1 mg. The spectrophotometric measurement of the zirconium or hafnium complex is accomplished without prior separation with a relative standard deviation of 1.3 to 2.7 percent.

  11. The effect of 0.1 atomic percent zirconium on the cyclic oxidation behavior of beta-NiAl for 300 hours at 1200 C

    NASA Technical Reports Server (NTRS)

    Barrett, C. A.

    1988-01-01

    The long time effect of 0.1 at percent Zr (0.2 wt percent Zr) on the cyclic oxidation behavior of hipped beta-NiAl was studied. Oxidation testing was performed in static air at 1200 C for up to 3000 one-hour exposure cycles. Specific weight change versus time data was modeled with the COSP computer program to analyze cyclic oxidation behavior. The Zr-free stoichiometric alloy oxidized and spalled randomly to bare metal between cycles at a rate high enough to deplete Al to a low enough level that oxidation breakaway took place as nonprotective NiO replaced the alpha-Al2O3/NiAl2O4 scale as the controlling oxide. The Zr minimized this severe type of spalling maintaining the protective alpha-Al2O3 scale even out to 3000 hours for the stoichiometric alloy with no significant Al depletion. A third beta-NiAl alloy containing 0.1 at percent Zr but with 10 percent less Al than the stoichiometric alloy was also tested and showed some depletion of Al, but the protective Al2O3/NiAl2O4 was still maintained to close to 2700 hours.

  12. Thermodynamic and kinetic studies of As(V) removal from water by zirconium oxide-coated marine sand.

    PubMed

    Khan, Tabrez Alam; Chaudhry, Saif Ali; Ali, Imran

    2013-08-01

    Arsenic contamination of groundwater is a major threat to human beings globally. Among various methods available for arsenic removal, adsorption is fast, inexpensive, selective, accurate, reproducible and eco-friendly in nature. The present paper describes removal of arsenate from water on zirconium oxide-coated sand (novel adsorbent). In the present work, zirconium oxide-coated sand was prepared and characterised by infrared and X-ray diffraction techniques. Batch experiments were performed to optimise different adsorption parameters such as initial arsenate concentration (100-1,000 μg/L), dose (1-8 g/L), pH of the solution (2-14), contact time (15-150 min.), and temperature (20, 30, 35 and 40 °C). The experimental data were analysed by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich isotherm models. Furthermore, thermodynamic and kinetic parameters were evaluated to know the mode of adsorption between ZrOCMS and As(V). The maximum removal of arsenic, 97 %, was achieved at initial arsenic concentration of 200 μg/L, after 75 min at dosage of 5.0 g/L, pH 7.0 and 27 ± 2 °C. For 600 μg/L concentration, the maximum Langmuir monolayer adsorption capacity was found to be 270 μg/g at 35 °C. Kinetic modelling data indicated that adsorption process followed pseudo-second-order kinetics. The mechanism is controlled by liquid film diffusion model. Thermodynamic parameter, ΔH°, was -57.782, while the values of ΔG° were -9.460, -12.183, -13.343 and -13.905 kJ/mol at 20, 30, 35 and 40 °C, respectively, suggesting exothermic and spontaneous nature of the process. The change in entropy, ΔS°= -0.23 kJ/mol indicated that the entropy decreased due to adsorption of arsenate ion onto the solid adsorbent. The results indicated that the reported zirconium oxide-coated marine sand (ZrOCMS) was good adsorbent with 97 % removal capacity at 200 μg/L concentration. It is interesting to note that the permissible limit of arsenic as per World Health Organization is 10 μg/L, and in real situation, this low concentration can be achieved through this adsorbent. Besides, the adsorption capacity showed that this adsorbent may be used for the removal of arsenic from any natural water resource.

  13. Thermal conductivity of self-ion irradiated nanocrystalline zirconium thin films

    DOE PAGES

    Pulavarthy, Raghu; Wang, Baoming; Hattar, Khalid; ...

    2017-07-15

    Thermomechanical stability and high thermal conductivity are important for nuclear cladding material performance and reliability, which degrade over time under irradiation. The literature suggests nanocrystalline materials as radiation tolerant, but little or no evidence is present from thermal transport perspective. In this study, we irradiated 10 nm grain size zirconium thin films with 800 keV Zr + beam from a 6 MV HVE Tandem accelerator to achieve various doses of 3 × 10 10 to 3.26 × 10 14 ions/cm 2, corresponding to displacement per atom (dpa) of 2.1 × 10 –4 to 2.28. Transmission electron microscopy showed significant grainmore » growth, texture evolution and oxidation in addition to the creation of displacement defects due to the irradiation. The specimens were co-fabricated with micro-heaters to establish thermal gradients that were mapped using infrared thermometry. An energy balance approach was used to estimate the thermal conductivity of the specimens, as function of irradiation dosage. As a result, up to 32% reduction of thermal conductivity was measured for the sample exposed to a dose of 2.1 dpa (3 × 10 14 ions/cm 2).« less

  14. Thermal conductivity of self-ion irradiated nanocrystalline zirconium thin films

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

    Pulavarthy, Raghu; Wang, Baoming; Hattar, Khalid

    Thermomechanical stability and high thermal conductivity are important for nuclear cladding material performance and reliability, which degrade over time under irradiation. The literature suggests nanocrystalline materials as radiation tolerant, but little or no evidence is present from thermal transport perspective. In this study, we irradiated 10 nm grain size zirconium thin films with 800 keV Zr + beam from a 6 MV HVE Tandem accelerator to achieve various doses of 3 × 10 10 to 3.26 × 10 14 ions/cm 2, corresponding to displacement per atom (dpa) of 2.1 × 10 –4 to 2.28. Transmission electron microscopy showed significant grainmore » growth, texture evolution and oxidation in addition to the creation of displacement defects due to the irradiation. The specimens were co-fabricated with micro-heaters to establish thermal gradients that were mapped using infrared thermometry. An energy balance approach was used to estimate the thermal conductivity of the specimens, as function of irradiation dosage. As a result, up to 32% reduction of thermal conductivity was measured for the sample exposed to a dose of 2.1 dpa (3 × 10 14 ions/cm 2).« less

  15. Effect of different surface treatments on shear bond strength of zirconia to three resin cements

    NASA Astrophysics Data System (ADS)

    Dadjoo, Nisa

    Statement of problem: There are no standard guidelines for material selection to obtain acceptable bonding to high-strength zirconium oxide ceramic. Studies suggest resin cements in combination with MDP-containing primer is a reasonable choice, however, the other cements cannot be rejected and need further investigation. Objective: The purpose of this in vitro study was the evaluation of the shear bond strength of three composite resin cements to zirconia ceramic after using different surface conditioning methods. Materials and methods: One hundred and twenty sintered Y-TZP ceramic (IPS e.max ZirCAD) squares (8 x 8 x 4 mm) were embedded in acrylic molds, then divided into three groups (n=40) based on the type of cement used. Within each group, the specimens were divided into four subgroups (n=10) and treated as follows: (1) Air abrasion with 50microm aluminum oxide (Al2O 3) particles (ALO); (2) Air abrasion + Scotchbond Universal adhesive (SBU); (3) Air abrasion + Monobond Plus (MBP); (4) Air abrasion + Z-Prime Plus (ZPP). Composite cylinders were used as carriers to bond to conditioned ceramic using (1) RelyX Ultimate adhesive resin cement (RX); (2) Panavia SA self-adhesive resin cement (PSA); (3) Calibra esthetic cement (CAL). The bonded specimens were submerged in distilled water and subjected to 24-hour incubation period at 37°C. All specimens were stressed in shear at a constant crosshead speed of 0.5 mm/min until failure. Statistical analysis was performed by ANOVA. The bond strength values (MPa), means and standard deviations were calculated and data were analyzed using analysis of variance with Fisher's PLSD multiple comparison test at the 0.05 level of significance. The nature of failure was recorded. Results: The two-way ANOVA showed Panavia SA to have the highest strength at 44.3 +/- 16.9 MPa (p<0.05). The combination of Scotchbond Universal surface treatment with Panavia SA cement showed statistically higher bond strength (p=0.0054). The highest bond strengths for all three cements were observed with Scotchbond Universal surface treatment (p=0.0041). Calibra in combination with aluminum oxide air abrasion resulted in statistically lowest bond strength at 12.0 +/- 3.9 MPa. The predominant mode of failure was cohesive with cement remaining principally on the zirconium oxide samples in 57.5% of the specimens, followed by cement found on both the zirconium oxide samples and composite rods (mixed) in 32.5% of the samples. Only 10% of the specimens were found with cement on the composite rods (adhesive failure). Conclusions: Within the limitations of this in vitro study, the MDP-containing resin cement, Panavia SA, yielded the strongest bond to Y-TZP ceramic when compared to adhesive (RelyX Ultimate) or esthetic (Calibra) resin cements. Air abrasion particle + Scotchbond Universal surface treatment demonstrated the highest bond strength regardless of the cement. Significance: The variation of surface conditioning methods yielded different results in accordance with the cement types. Overall, Scotchbond Universal adhesive + air abrasion yielded the highest bond strengths among all three surface treatments. The phosphate monomer-containing luting system, Panavia SA, is acceptable for bonding to zirconia ceramics.

  16. Performance of granular zirconium-iron oxide in the removal of fluoride from drinking water.

    PubMed

    Dou, Xiaomin; Zhang, Yansu; Wang, Hongjie; Wang, Tingjie; Wang, Yili

    2011-06-01

    In this study, a granular zirconium-iron oxide (GZI) was successfully prepared using the extrusion method, and its defluoridation performance was systematically evaluated. The GZI was composed of amorphous and nano-scale oxide particles. The Zr and Fe were evenly distributed on its surface, with a Zr/Fe molar ratio of ∼2.3. The granular adsorbent was porous with high permeability potential. Moreover, it had excellent mechanical stability and high crushing strength, which ensured less material breakage and mass loss in practical use. In batch tests, the GZI showed a high adsorption capacity of 9.80 mg/g under an equilibrium concentration of 10 mg/L at pH 7.0, which outperformed many other reported granular adsorbents. The GZI performed well over a wide pH range, of 3.5-8.0, and especially well at pH 6.0-8.0, which was the preferred range for actual application. Fluoride adsorption on GZI followed pseudo-second-order kinetics and could be well described by the Freundlich equilibrium model. With the exception of HCO(3)(-), other co-existing anions and HA did not evidently inhibit fluoride removal by GZI when considering their real concentrations in natural groundwater, which showed that GZI had a high selectivity for fluoride. In column tests using real groundwater as influent, about 370, 239 and 128 bed volumes (BVs) of groundwater were treated before breakthrough was reached under space velocities (SVs) of 0.5, 1 and 3 h(-1), respectively. Additionally, the toxicity characteristic leaching procedure (TCLP) results suggested that the spent GZI was inert and could be safely disposed of in landfill. In conclusion, this granular adsorbent showed high potential for fluoride removal from real groundwater, due to its high performance and physical-chemical properties. Copyright © 2011 Elsevier Ltd. All rights reserved.

  17. SPM oxidation and parallel writing on zirconium nitride thin films

    NASA Astrophysics Data System (ADS)

    Farkas, N.; Comer, J. R.; Zhang, G.; Evans, E. A.; Ramsier, R. D.; Dagata, J. A.

    2005-07-01

    Systematic investigation of the SPM oxidation process of sputter-deposited ZrN thin films is reported. During the intrinsic part of the oxidation, the density of the oxide increases until the total oxide thickness is approximately twice the feature height. Further oxide growth is sustainable as the system undergoes plastic flow followed by delamination from the ZrN-silicon interface keeping the oxide density constant. ZrN exhibits superdiffusive oxidation kinetics in these single tip SPM studies. We extend this work to the fabrication of parallel oxide patterns 70 nm in height covering areas in the square centimeter range. This simple, quick, and well-controlled parallel nanolithographic technique has great potential for biomedical template fabrication.

  18. Mixed oxide solid solutions

    DOEpatents

    Magno, Scott; Wang, Ruiping; Derouane, Eric

    2003-01-01

    The present invention is a mixed oxide solid solution containing a tetravalent and a pentavalent cation that can be used as a support for a metal combustion catalyst. The invention is furthermore a combustion catalyst containing the mixed oxide solid solution and a method of making the mixed oxide solid solution. The tetravalent cation is zirconium(+4), hafnium(+4) or thorium(+4). In one embodiment, the pentavalent cation is tantalum(+5), niobium(+5) or bismuth(+5). Mixed oxide solid solutions of the present invention exhibit enhanced thermal stability, maintaining relatively high surface areas at high temperatures in the presence of water vapor.

  19. A sensitive determination of terbutaline in pharmaceuticals and urine samples using a composite electrode based on zirconium oxide nanoparticles.

    PubMed

    Baytak, Aysegul Kutluay; Teker, Tugce; Duzmen, Sehriban; Aslanoglu, Mehmet

    2016-10-01

    An accurate and precise determination of terbutaline has been carried out using a glassy carbon electrode (GCE) modified with a composite of multi-walled carbon nanotubes (MWCNTs) and nanoparticles of zirconium oxide (ZrO2NPs). Energy dispersive X-ray and scanning electron microscopic techniques were utilized for the characterization of the composite layer. Terbutaline exhibited a broad oxidation peak at 770mV on a GCE. However, MWCNTs/GCE presented an electrocatalytic effect toward the oxidation of terbutaline with a better anodic peak at 660mV. Furthermore, the electrochemical behavior of terbutaline has greatly been improved at a GCE modified with a composite of MWCNTs and nanoparticles of ZrO2. The ZrO2NPs/MWCNTs/GCE exhibited a sharp anodic wave at 645mV with a large enhancement of the current response for terbutaline. Square wave voltammetry (SWV) was performed for the determination of terbutaline at ZrO2NPs/MWCNTs/GCE. A linear plot was obtained for the current responses of terbutaline against concentrations in the range of 10-160nM yielding a detection limit of 2.25nM (based on 3Sb/m). Improved voltammetric behavior, long-time stability and good reproducibility were obtained for terbutaline at the proposed electrode. A mean recovery of 101.2% with an RSD% of 1.9 was obtained for the analysis of the drug formulation. The accurate and precise quantification of terbutaline makes the ZrO2NPs/MWCNTs/GCE system of great interest for monitoring its therapeutic use. Copyright © 2016 Elsevier B.V. All rights reserved.

  20. Development of bone-like zirconium oxide nanoceramic modified chitosan based porous nanocomposites for biomedical application.

    PubMed

    Bhowmick, Arundhati; Pramanik, Nilkamal; Jana, Piyali; Mitra, Tapas; Gnanamani, Arumugam; Das, Manas; Kundu, Patit Paban

    2017-02-01

    Here, zirconium oxide nanoparticles (ZrO 2 NPs) were incorporated for the first time in organic-inorganic hybrid composites containing chitosan, poly(ethylene glycol) and nano-hydroxypatite (CS-PEG-HA) to develop bone-like nanocomposites for bone tissue engineering application. These nanocomposites were characterized by FT-IR, XRD, TEM combined with SAED. SEM images and porosity measurements revealed highly porous structure having pore size of less than 1μm to 10μm. Enhanced water absorption capacity and mechanical strengths were obtained compared to previously reported CS-PEG-HA composite after addition of 0.1-0.3wt% of ZrO 2 NPs into these nanocomposites. The mechanical strengths and porosities were similar to that of human spongy bone. Strong antimicrobial effects against gram-negative and gram-positive bacterial strains were also observed. Along with getting low alkalinity pH (7.4) values, similar to the pH of human plasma, hemocompatibility and cytocompatibility with osteoblastic MG-63 cells were also established for these nanocomposites. Addition of 15wt% HA-ZrO 2 (having 0.3wt% ZrO 2 NPs) into CS-PEG (55:30wt%) composite resulted in greatest mechanical strength, porosity, antimicrobial property and cytocompatibility along with suitable water absorption capacity and compatibility with human pH and blood. Thus, this nanocomposite could serve as a potential candidate to be used for bone tissue engineering. Copyright © 2016 Elsevier B.V. All rights reserved.

  1. Performance of magnetic zirconium-iron oxide nanoparticle in the removal of phosphate from aqueous solution

    NASA Astrophysics Data System (ADS)

    Zhang, Chang; Li, Yongqiu; Wang, Fenghua; Yu, Zhigang; Wei, Jingjing; Yang, Zhongzhu; Ma, Chi; Li, Zihao; Xu, ZiYi; Zeng, Guangming

    2017-02-01

    In this study, magnetic zirconium-iron oxide nanoparticles (MZION) of different Fe/Zr molar ratios were successfully prepared using the co-precipitation method, and their performance for phosphate removal was systematically evaluated. The as-obtained adsorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential analyzer, Fourier transform infrared spectroscopy (FT-IR) and Brunauer Emmett Teller (BET) specific surface area analysis. The effects of pH, ionic strength, and co-existing ions (including Cl-, SO42-, NO3- and HCO3-) were measured to evaluate the adsorption performance in batch experiments. The results showed that decreasing the Fe/Zr molar ratios increased the specific surface area that was propitious to adsorption process, but the adsorption capacity enhanced with the decrease of Fe/Zr molar ratios. Phosphate adsorption on MZION could be well described by the Freundlich equilibrium model and pseudo-second-order kinetics. The adsorption of phosphate was highly pH dependent and decreased with increasing pH from 1.5 to 10.0. The adsorption was slightly affected by ionic strength. With the exception of HCO3-, co-existing anions showed minimum or no effect on their adsorption performance. After adsorption, phosphate on these MZION could be easily desorbed by 0.1 M NaOH solution. The phosphate adsorption mechanism of MZION followed the inner-sphere complexing mechanism, and the surface sbnd OH groups played a significant role in the phosphate adsorption. Additionally, the main advantages of MZION consisted in its separation convenience and highly adsorption capacity compared to other adsorbents.

  2. 21 CFR 82.1051 - Lakes (D&C).

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ..., gloss white, clay, titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or... radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium; or (ii) a salt prepared... subpart, by combining such color with the basic radical sodium, potassium, aluminum, barium, calcium...

  3. 21 CFR 82.1051 - Lakes (D&C).

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ..., gloss white, clay, titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or... radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium; or (ii) a salt prepared... subpart, by combining such color with the basic radical sodium, potassium, aluminum, barium, calcium...

  4. 21 CFR 82.1051 - Lakes (D&C).

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ..., gloss white, clay, titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or... radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium; or (ii) a salt prepared... subpart, by combining such color with the basic radical sodium, potassium, aluminum, barium, calcium...

  5. 21 CFR 82.1051 - Lakes (D&C).

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ..., gloss white, clay, titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or... radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium; or (ii) a salt prepared... subpart, by combining such color with the basic radical sodium, potassium, aluminum, barium, calcium...

  6. 21 CFR 82.1051 - Lakes (D&C).

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ..., gloss white, clay, titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or... radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium; or (ii) a salt prepared... subpart, by combining such color with the basic radical sodium, potassium, aluminum, barium, calcium...

  7. Catalyst support of mixed cerium zirconium titanium oxide, including use and method of making

    DOEpatents

    Willigan, Rhonda R [Manchester, CT; Vanderspurt, Thomas Henry [Glastonbury, CT; Tulyani, Sonia [Manchester, CT; Radhakrishnan, Rakesh [Vernon, CT; Opalka, Susanne Marie [Glastonbury, CT; Emerson, Sean C [Broad Brook, CT

    2011-01-18

    A durable catalyst support/catalyst is capable of extended water gas shift operation under conditions of high temperature, pressure, and sulfur levels. The support is a homogeneous, nanocrystalline, mixed metal oxide of at least three metals, the first being cerium, the second being Zr, and/or Hf, and the third importantly being Ti, the three metals comprising at least 80% of the metal constituents of the mixed metal oxide and the Ti being present in a range of 5% to 45% by metals-only atomic percent of the mixed metal oxide. The mixed metal oxide has an average crystallite size less than 6 nm and forms a skeletal structure with pores whose diameters are in the range of 4-9 nm and normally greater than the average crystallite size. The surface area of the skeletal structure per volume of the material of the structure is greater than about 240 m.sup.2/cm.sup.3. The method of making and use are also described.

  8. Development of a direct patterning method for functional oxide thin films using ultraviolet irradiation and hybrid-cluster gels and its application to thin-film transistor fabrication

    NASA Astrophysics Data System (ADS)

    Yoshimoto, Yuuki; Li, Jinwang; Shimoda, Tatsuya

    2018-04-01

    A gel state exists in the solution-solid conversion process. We found that solidification can be promoted by irradiating the gel with ultraviolet (UV) light. In this study, a patterning method without using a vacuum system or employing photoresist materials has been proposed wherein solidification was applied to a gel by UV irradiation. Indium oxide gel, indium gallium oxide gel, lanthanum zirconium oxide gel, and lanthanum ruthenium oxide gels were successfully patterned by using our technique. Moreover, an oxide thin-film transistor was fabricated by our novel patterning method and was successfully operated.

  9. Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications?

    PubMed Central

    Spijksma, Gerald I.; Blank, Dave H. A.; Bouwmeester, Henny J. M.; Kessler, Vadim G.

    2009-01-01

    Modification of different zirconium propoxide precursors with H2dea was investigated by characterization of the isolated modified species. Upon modification of zirconium n-propoxide and [Zr(OnPr)(OiPr)3(iPrOH)]2 with ½ a mol equivalent of H2dea the complexes [Zr2(OnPr)6(OCH2CH2)2NH]2 (1) and [Zr2(OnPr)2(OiPr)4(OCH2CH2)2NH]2 (2) were obtained. However, 1H-NMR studies of these tetranuclear compounds showed that these are not time-stable either in solution or solid form. The effect of this time instability on material properties is demonstrated by light scattering and TEM experiments. Modification of zirconium isopropoxide with either ½ or 1 equivalent mol of H2dea results in formation of the trinuclear complex, Zr{η3μ2-NH(C2H4O)2}3[Zr(OiPr)3]2(iPrOH)2 (3) countering a unique nona-coordinated central zirconium atom. This complex 3 is one of the first modified zirconium propoxide precursors shown to be stable in solution for long periods of time. The particle size and morphology of the products of sol-gel synthesis are strongly dependent on the time factor and eventual heat treatment of the precursor solution. Reproducible sol-gel synthesis requires the use of solution stable precursors. PMID:20087472

  10. Abrasion resistant heat pipe

    DOEpatents

    Ernst, D.M.

    1984-10-23

    A specially constructed heat pipe is described for use in fluidized bed combustors. Two distinct coatings are spray coated onto a heat pipe casing constructed of low thermal expansion metal, each coating serving a different purpose. The first coating forms aluminum oxide to prevent hydrogen permeation into the heat pipe casing, and the second coating contains stabilized zirconium oxide to provide abrasion resistance while not substantially affecting the heat transfer characteristics of the system.

  11. Oxygen Migration and Local Structural Changes with Schottky Defects in Pure Zirconium Oxide Crystals

    NASA Astrophysics Data System (ADS)

    Terada, Yayoi; Mohri, Tetsuo

    2018-05-01

    By employing the Buckingham potential, we performed classical molecular-dynamics computer simulations at constant pressure and temperature for a pure ZrO2 crystal without any vacancies and for a pure ZrO2 crystal containing zirconium vacancies and oxygen vacancies. We examined the positions of atoms and vacancies in the steady state, and we investigated the migration behavior of atoms and the local structure of vacancies of the pure ZrO2 crystal. We found that Schottky defects (aggregates consisting of one zirconium vacancy with an effective charge of -4 and two oxygen vacancies each with an effective charge of +2 to maintain charge neutrality) are the main defects formed in the steady state in cubic ZrO2, and that oxygen migration occurs through a mechanism involving vacancies on the oxygen sublattice near such defects. We also found that several oxygen atoms near each defect are displaced far from the sublattice site and induce oxygen migration.

  12. 5A Zirconium Dioxide Ammonia Microsensor Integrated with a Readout Circuit Manufactured Using the 0.18 μm CMOS Process

    PubMed Central

    Lin, Guan-Ming; Dai, Ching-Liang; Yang, Ming-Zhi

    2013-01-01

    The study presents an ammonia microsensor integrated with a readout circuit on-a-chip fabricated using the commercial 0.18 μm complementary metal oxide semiconductor (CMOS) process. The integrated sensor chip consists of a heater, an ammonia sensor and a readout circuit. The ammonia sensor is constructed by a sensitive film and the interdigitated electrodes. The sensitive film is zirconium dioxide that is coated on the interdigitated electrodes. The heater is used to provide a working temperature to the sensitive film. A post-process is employed to remove the sacrificial layer and to coat zirconium dioxide on the sensor. When the sensitive film adsorbs or desorbs ammonia gas, the sensor produces a change in resistance. The readout circuit converts the resistance variation of the sensor into the output voltage. The experiments show that the integrated ammonia sensor has a sensitivity of 4.1 mV/ppm. PMID:23503294

  13. Nanoindentation study of bulk zirconium hydrides at elevated temperatures

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

    Cinbiz, Mahmut Nedim; Balooch, Mehdi; Hu, Xunxiang

    Here, the mechanical properties of zirconium hydrides was studied using nano-indentation technique at a temperature range of 25 – 400 °C. Temperature dependency of reduced elastic modulus and hardness of δ- and ε-zirconium hydrides were obtained by conducting nanoindentation experiments on the bulk hydride samples with independently heating capability of indenter and heating stage. The reduced elastic modulus of δ-zirconium hydride (H/Zr ratio =1.61) decreased from ~113 GPa to ~109 GPa while temperature increased from room temperature to 400°C. For ε-zirconium hydrides (H/Zr ratio=1.79), the reduced elastic modulus decreased from 61 GPa to 54 GPa as temperature increased from roommore » temperature to 300 °C. Whereas, hardness of δ-zirconium hydride significantly decreased from 4.1 GPa to 2.41 GPa when temperature increased from room temperature to 400 °C. Similarly, hardness of ε-zirconium hydride decreased from 3.06 GPa to 2.19 GPa with temperature increase from room temperature to 300°C.« less

  14. Nanoindentation study of bulk zirconium hydrides at elevated temperatures

    DOE PAGES

    Cinbiz, Mahmut Nedim; Balooch, Mehdi; Hu, Xunxiang; ...

    2017-08-02

    Here, the mechanical properties of zirconium hydrides was studied using nano-indentation technique at a temperature range of 25 – 400 °C. Temperature dependency of reduced elastic modulus and hardness of δ- and ε-zirconium hydrides were obtained by conducting nanoindentation experiments on the bulk hydride samples with independently heating capability of indenter and heating stage. The reduced elastic modulus of δ-zirconium hydride (H/Zr ratio =1.61) decreased from ~113 GPa to ~109 GPa while temperature increased from room temperature to 400°C. For ε-zirconium hydrides (H/Zr ratio=1.79), the reduced elastic modulus decreased from 61 GPa to 54 GPa as temperature increased from roommore » temperature to 300 °C. Whereas, hardness of δ-zirconium hydride significantly decreased from 4.1 GPa to 2.41 GPa when temperature increased from room temperature to 400 °C. Similarly, hardness of ε-zirconium hydride decreased from 3.06 GPa to 2.19 GPa with temperature increase from room temperature to 300°C.« less

  15. A study on recovery of uranium in the anode basket residues delivered from the pyrochemical process of used nuclear fuel

    NASA Astrophysics Data System (ADS)

    Eun, H. C.; Kim, T. J.; Jang, J. H.; Kim, G. Y.; Park, S. B.; Yoon, D. S.; Kim, S. H.; Paek, S. W.; Lee, S. J.

    2018-04-01

    In this study, the chlorination of uranium oxide (UO2) using ammonium chloride and zirconium as chemical agents was conducted to recover the uranium in the anode basket residues from the pyrochemical process of used nuclear fuel. The chlorination of UO2 was predicted using thermodynamic equilibrium calculations. The experimental conditions for the chlorination were determined using a chlorination test with cerium oxide (CeO2). In the chlorination test, it was confirmed that UO2 was chlorinated into UCl3 at 320 °C, some UO2 remained without changes in the chemical form, and ZrO2, Zr2O, and ZrCl2 were generated as byproducts.

  16. In vivo genotoxicity assessment of titanium, zirconium and aluminium nanoparticles, and their microparticulated forms, in Drosophila.

    PubMed

    Demir, Eşref; Turna, Fatma; Vales, Gerard; Kaya, Bülent; Creus, Amadeu; Marcos, Ricard

    2013-11-01

    As in vivo system, we propose Drosophila melanogaster as a useful model for study the genotoxic risks associated with nanoparticle exposure. In this study we have carried out a genotoxic evaluation of titanium dioxide (TiO2), zirconium oxide (ZrO2) and aluminium oxide (Al2O3) nanoparticles and their microparticulated forms in D. melanogaster by using the wing somatic mutation and recombination assay. This assay is based on the principle that loss of heterozygosis and the corresponding expression of the suitable recessive markers, multiple wing hairs and flare-3, can lead to the formation of mutant clones in treated larvae, which are expressed as mutant spots on the wings of adult flies. Third instar larvae were feed with TiO2, ZrO2 and Al2O3 nanoparticles, and their microparticulated forms, at concentrations ranging from 0.1 to 10mM. Although a certain level of aggregation/agglomeration was observed in solution, it must be noted than the constant digging activity of larvae ensures that treated medium pass constantly through the digestive tract ensuring exposure. The results showed that no significant increases in the frequency of all spots (e.g. small single, large single, twin, total mwh and total spots) were observed, indicating that these nanoparticles were not able to induce genotoxic activity in the wing spot assay of D. melanogaster. Negative data were also obtained with the microparticulated forms. This indicates that the nanoparticulated form of the selected nanomaterials does not modify the potential genotoxicity of their microparticulated versions. These in vivo results contribute to increase the genotoxicity database on the TiO2, ZrO2 and Al2O3 nanoparticles. Copyright © 2013 Elsevier Ltd. All rights reserved.

  17. Dental discoloration caused by bismuth oxide in MTA in the presence of sodium hypochlorite.

    PubMed

    Marciano, Marina Angélica; Duarte, Marco Antonio Hungaro; Camilleri, Josette

    2015-12-01

    The aim of this research was to analyse the dental discolouration caused by mineral trioxide aggregate (MTA) induced by bismuth oxide and also assess the colour stability of other dental cements. Bismuth oxide, calcium tungstate and zirconium oxide were placed in contact with sodium hypochlorite for 24 h after which they were dried and photographed. Phase analyses were performed by X-ray diffraction (XRD) of radiopacifiers before and after immersion in sodium hypochlorite. Furthermore, teeth previously immersed in water or sodium hypochlorite were filled with MTA Angelus, Portland cement (PC), PC with 20 % zirconium oxide, PC with 20 % calcium tungstate and Biodentine. Teeth were immersed for 28 days in Hank's balanced salt solution after which they were sectioned and characterized using scanning electron microscopy (SEM) with energy-dispersive mapping and stereomicroscopy. Bismuth oxide in contact with sodium hypochlorite exhibited a change in colour from light yellow to dark brown. XRD analysis demonstrated peaks for radiopacifier and sodium chloride in samples immersed in sodium hypochlorite. The SEM images of the dentine to material interface showed alteration in material microstructure for MTA Angelus and Biodentine with depletion in calcium content in the material. The energy-dispersive maps showed migration of radiopacifier and silicon in dentine. MTA Angelus in contact with a tooth previously immersed in sodium hypochlorite resulted in colour alteration at the cement/dentine interface. MTA Angelus should not be used after irrigation with sodium hypochlorite as this will result in tooth discoloration.

  18. Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels.

    PubMed

    Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

    2018-01-12

    Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening.

  19. Effects of Zr Addition on Strengthening Mechanisms of Al-Alloyed High-Cr ODS Steels

    PubMed Central

    Ren, Jian; Yu, Liming; Liu, Yongchang; Liu, Chenxi; Li, Huijun; Wu, Jiefeng

    2018-01-01

    Oxide dispersion strengthened (ODS) steels with different contents of zirconium (denoted as 16Cr ODS, 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS) were fabricated to investigate the effects of Zr on strengthening mechanism of Al-alloyed 16Cr ODS steel. Electron backscatter diffraction (EBSD) results show that the mean grain size of ODS steels could be decreased by Zr addition. Transmission electron microscope (TEM) results indicate that Zr addition could increase the number density but decrease the mean diameter and inter-particle spacing of oxide particles. Furthermore, it is also found that in addition to Y-Al-O nanoparticles, Y-Zr-O oxides with finer size were observed in 16Cr-0.3Zr ODS and 16Cr-0.6Zr ODS steels. These changes in microstructure significantly increase the yield strength (YS) and ultimate tensile strength (UTS) of ODS steels through mechanisms of grain boundary strengthening and dispersion strengthening. PMID:29329260

  20. Effect of DC Plasma Electrolytic Oxidation on Surface Characteristics and Corrosion Resistance of Zirconium

    PubMed Central

    Sowa, Maciej

    2018-01-01

    Zr is a valve metal, the biocompatibility of which is at least on par with Ti. Recently, numerous attempts of the formation of bioactive coatings on Zr by plasma electrolytic oxidation (PEO) in solutions that were based on calcium acetate and calcium β-glycerophosphate were made. In this study, the direct current (DC) PEO of commercially pure zirconium in the solutions that contained Ca(H2PO2)2, Ca(HCOO)2, and Mg(CH3COO)2 was investigated. The treatment was conducted at 75 mA/cm2 up to 200, 300, or 400 V. Five process stages were discerned. The treatment at higher voltages resulted in the formation of oxide layers that had Ca/P or (Mg+Ca)/P ratios that were close to that of hydroxyapatite (Ca/P = 1.67), determined by SEM/EDX. The corrosion resistance studies were performed using electrochemical impedance spectroscopy (EIS) and DC polarization methods. R(Q[R(QR)]) circuit model was used to fit the EIS data. In general, the coatings that were obtained at 200 V were the most corrosion resistant, however, they lacked the porous structure, which is typical for PEO coatings, and is sought after in the biomedical applications. The treatment at 400 V resulted in the formation of the coatings that were more corrosion resistant than those that were obtained at 300 V. This was determined mainly by the prevailing plasma regime at the given process voltage. The pitting resistance of Zr was also improved by the treatment, regardless of the applied process conditions. PMID:29751530

  1. Mechanically activated synthesis of PZT and its electromechanical properties

    NASA Astrophysics Data System (ADS)

    Liu, X.; Akdogan, E. K.; Safari, A.; Riman, R. E.

    2005-08-01

    Mechanical activation was successfully used to synthesize nanostructured phase-pure Pb(Zr0.7Ti0.3)O3 (PZT) powders. Lead zirconium titanium (PbZrTi) hydrous oxide precursor, synthesized from chemical co-precipitation, was mechanically activated in a NaCl matrix. The synthesized PZT particles were characterized by using X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy, laser-light diffraction, and nitrogen adsorption. Thermogravimetric analysis and differential thermal analysis were used to monitor dehydration and phase transformation of PbZrTi hydrous oxide precursor during mechanical activation. The best mechanical activation conditions corresponded to mechanically activating PbZrTi hydrous oxide precursor in a NaCl matrix with a NaCl/precursor weight ratio of 4:1 for 8 h. These conditions resulted in a dispersible phase-pure PZT powder with a median secondary-particle size of ˜110 nm. The properties of PZT 70/30 from mechanically activated powder, as measured on discs sintered at 1150 °C for 2 h, were found to be in close conformity to those obtained by a conventional mixed oxide solid state reaction route.

  2. From Zirconium Nanograins to Zirconia Nanoneedles

    PubMed Central

    Zalnezhad, E.; Hamouda, A. M. S.; Jaworski, J.; Do Kim, Young

    2016-01-01

    Combinations of three simple techniques were utilized to gradually form zirconia nanoneedles from zirconium nanograins. First, a physical vapor deposition magnetron sputtering technique was used to deposit pure zirconium nanograins on top of a substrate. Second, an anodic oxidation was applied to fabricate zirconia nanotubular arrays. Finally, heat treatment was used at different annealing temperatures in order to change the structure and morphology from nanotubes to nanowires and subsequently to nanoneedles in the presence of argon gas. The size of the pure zirconium nanograins was estimated to be approximately 200–300 nm. ZrO2 nanotubular arrays with diameters of 70–120 nm were obtained. Both tetragonal and monoclinic ZrO2 were observed after annealing at 450 °C and 650 °C. Only a few tetragonal peaks appeared at 850 °C, while monoclinic ZrO2 was obtained at 900 °C and 950 °C. In assessing the biocompatibility of the ZrO2 surface, the human cell line MDA-MB-231 was found to attach and proliferate well on surfaces annealed at 850 °C and 450 °C; however, the amorphous ZrO2 surface, which was not heat treated, did not permit extensive cell growth, presumably due to remaining fluoride. PMID:27623486

  3. Protective interlayer for high temperature solid electrolyte electrochemical cells

    DOEpatents

    Singh, P.; Vasilow, T.R.; Richards, V.L.

    1996-05-14

    The invention is comprised of an electrically conducting doped or admixed cerium oxide composition with niobium oxide and/or tantalum oxide for electrochemical devices, characterized by the general formula: Nb{sub x}Ta{sub y}Ce{sub 1{minus}x{minus}y}O{sub 2} where x is about 0.0 to 0.05, y is about 0.0 to 0.05, and x+y is about 0.02 to 0.05, and where x is preferably about 0.02 to 0.05 and y is 0, and a method of making the same is also described. This novel composition is particularly applicable in forming a protective interlayer of a high temperature, solid electrolyte electrochemical cell, characterized by a first electrode; an electrically conductive interlayer of niobium and/or tantalum doped cerium oxide deposited over at least a first portion of the first electrode; an interconnect deposited over the interlayer; a solid electrolyte deposited over a second portion of the first electrode, the first portion being discontinuous from the second portion; and, a second electrode deposited over the solid electrolyte. The interlayer is characterized as being porous and selected from the group consisting of niobium doped cerium oxide, tantalum doped cerium oxide, and niobium and tantalum doped cerium oxide or admixtures of the same. The first electrode, an air electrode, is a porous layer of doped lanthanum manganite, the solid electrolyte layer is a dense yttria stabilized zirconium oxide, the interconnect layer is a dense, doped lanthanum chromite, and the second electrode, a fuel electrode, is a porous layer of nickel-zirconium oxide cermet. The electrochemical cell can take on a plurality of shapes such as annular, planar, etc. and can be connected to a plurality of electrochemical cells in series and/or in parallel to generate electrical energy. 5 figs.

  4. PHYSICAL PROPERTIES OF ZIRCONIUM NITRIDE IN THE HOMOGENEITY REGION (in Ukrainian)

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

    Samsonov, G.V.; Verkhoglyadova, T.S.

    1962-01-01

    The x-ray method was used to determine the homogeneity region of zirconium nitride as 40 to 50 at.% (9.5 to 13.3% by weight) of nitrogen. It is also shown that part of the ionic bond in the zirconium nitride lattice increases with a decrease in the nitrogen content in this region, this increase being higher than in the homogeneity region of titunium nitride due to the smaller degree of unfilling of the electron d-shell of the zirconium atom in comparison with that of the titanium atom. (auth)

  5. Zirconium(IV) oxide: New coating material for nanoresonators for shell-isolated nanoparticle-enhanced Raman spectroscopy

    NASA Astrophysics Data System (ADS)

    Krajczewski, Jan; Abdulrahman, Heman Burhanalden; Kołątaj, Karol; Kudelski, Andrzej

    2018-03-01

    One tool that can be used for determining the structure and composition of surfaces of various materials (even in in situ conditions) is shell-isolated nanoparticle-enhanced Raman spectroscopy (SHINERS). In SHINERS measurements, the surface under investigation is covered with a layer of surface-protected plasmonic nanoparticles, and then the Raman spectrum of the surface analysed is recorded. The plasmonic cores of the used core-shell structures act as electromagnetic nanoresonators, significantly locally enhancing the intensity of the electric field of the incident radiation, leading to a large increase in the efficiency of the generation of the Raman signal from molecules in the close proximity to the deposited SHINERS nanoresonators. A protective layer (from transparent dielectrics such as SiO2, Al2O3 or TiO2) prevents direct interaction between the plasmonic metal and the analysed surface (such interactions may lead to changes in the structure of the surface) and, in the case of plasmonic cores other than gold cores, the dielectric layer increases the chemical stability of the metal core. In this contribution, we show for the first time that core-shell nanoparticles having a silver core (both a solid and hollow one) and a shell of zirconium(IV) oxide are very efficient SHINERS nanoresonators that are significantly more stable in acidic and alkaline media than the silver-silica core-shell structures typically used for SHINERS experiments.

  6. The Retentive Strength of Cemented Zirconium Oxide Crowns after Dentin Pretreatment with Desensitizing Paste Containing 8% Arginine and Calcium Carbonate

    PubMed Central

    Pilo, Raphael; Harel, Noga; Nissan, Joseph; Levartovsky, Shifra

    2016-01-01

    The effect of dentin pretreatment with Desensitizing Paste containing 8% arginine and calcium carbonate on the retention of zirconium oxide (Y-TZP) crowns was tested. Forty molar teeth were mounted and prepared using a standardized protocol. Y-TZP crowns were produced using computer-aided design and computer-aided manufacturing (CAD-CAM) technology. The 40 prepared teeth were either pretreated with Desensitizing Paste or not pretreated. After two weeks, each group was subdivided into two groups, cemented with either Resin Modified Glass Ionomer Cement (RMGIC) or Self Adhesive Resin Cement (SARC)). Prior to cementation, the surface areas of the prepared teeth were measured. After aging, the cemented crown-tooth assemblies were tested for retentive strength using a universal testing machine. The debonded surfaces of the teeth and crowns were examined microscopically at 10× magnification. Pretreating the dentin surfaces with Desensitizing Paste prior to cementation did not affect the retention of the Y-TZP crowns. The retentive values for RMGIC (3.04 ± 0.77 MPa) were significantly higher than those for SARC (2.28 ± 0.58 MPa). The predominant failure modes for the RMGIC and SARC were adhesive cement-dentin and adhesive cement-crown, respectively. An 8.0% arginine and calcium carbonate in-office desensitizing paste can be safely used to reduce post-cementation sensitivity without reducing the retentive strength of Y-TZP crowns. PMID:27023532

  7. The Retentive Strength of Cemented Zirconium Oxide Crowns after Dentin Pretreatment with Desensitizing Paste Containing 8% Arginine and Calcium Carbonate.

    PubMed

    Pilo, Raphael; Harel, Noga; Nissan, Joseph; Levartovsky, Shifra

    2016-03-25

    The effect of dentin pretreatment with Desensitizing Paste containing 8% arginine and calcium carbonate on the retention of zirconium oxide (Y-TZP) crowns was tested. Forty molar teeth were mounted and prepared using a standardized protocol. Y-TZP crowns were produced using computer-aided design and computer-aided manufacturing (CAD-CAM) technology. The 40 prepared teeth were either pretreated with Desensitizing Paste or not pretreated. After two weeks, each group was subdivided into two groups, cemented with either Resin Modified Glass Ionomer Cement (RMGIC) or Self Adhesive Resin Cement (SARC)). Prior to cementation, the surface areas of the prepared teeth were measured. After aging, the cemented crown-tooth assemblies were tested for retentive strength using a universal testing machine. The debonded surfaces of the teeth and crowns were examined microscopically at 10× magnification. Pretreating the dentin surfaces with Desensitizing Paste prior to cementation did not affect the retention of the Y-TZP crowns. The retentive values for RMGIC (3.04 ± 0.77 MPa) were significantly higher than those for SARC (2.28 ± 0.58 MPa). The predominant failure modes for the RMGIC and SARC were adhesive cement-dentin and adhesive cement-crown, respectively. An 8.0% arginine and calcium carbonate in-office desensitizing paste can be safely used to reduce post-cementation sensitivity without reducing the retentive strength of Y-TZP crowns.

  8. Zirconium oxide surface passivation of crystalline silicon

    NASA Astrophysics Data System (ADS)

    Wan, Yimao; Bullock, James; Hettick, Mark; Xu, Zhaoran; Yan, Di; Peng, Jun; Javey, Ali; Cuevas, Andres

    2018-05-01

    This letter reports effective passivation of crystalline silicon (c-Si) surfaces by thermal atomic layer deposited zirconium oxide (ZrOx). The optimum layer thickness and activation annealing conditions are determined to be 20 nm and 300 °C for 20 min. Cross-sectional transmission electron microscopy imaging shows an approximately 1.6 nm thick SiOx interfacial layer underneath an 18 nm ZrOx layer, consistent with ellipsometry measurements (˜20 nm). Capacitance-voltage measurements show that the annealed ZrOx film features a low interface defect density of 1.0 × 1011 cm-2 eV-1 and a low negative film charge density of -6 × 1010 cm-2. Effective lifetimes of 673 μs and 1.1 ms are achieved on p-type and n-type 1 Ω cm undiffused c-Si wafers, respectively, corresponding to an implied open circuit voltage above 720 mV in both cases. The results demonstrate that surface passivation quality provided by ALD ZrOx is consistent with the requirements of high efficiency silicon solar cells.

  9. Effect of phase transformation on optical and dielectric properties of zirconium oxide nanoparticles

    NASA Astrophysics Data System (ADS)

    Chintaparty, Rajababu; Palagiri, Bhavani; Reddy Nagireddy, Ramamanohar; subbha Reddy Imma Reddy, Venkata

    2015-09-01

    Zirconium oxide nanoparticle (ZrO2) is synthesized by the hydrothermal method at different calcination temperatures. The structural analysis is carried out by X-ray diffraction and Raman spectra. The sample prepared at 400 °C and 1100 °C showed the cubic and monoclinic phase, respectively, and the sample calcined at 600 °C and 800 °C showed the mixed phase with co-existence of cubic and monoclinic phases. Furthermore, the morphology and particle size of these samples were investigated by scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. The band gap estimated from UV-Vis spectra of ZrO2 (zirconia) nanocrystalline materials calcined at different temperatures from 400 °C to 1100 °C was in the range of 2.6-4.2 eV. The frequency dependence of dielectric constant and dielectric loss was investigated at room temperature. The low frequency region of dielectric constant is attributed to space charge effects.

  10. Synthesis of hydrous zirconium oxide-impregnated chitosan beads and their application for removal of fluoride and lead

    NASA Astrophysics Data System (ADS)

    Cho, Dong-Wan; Jeon, Byong-Hun; Jeong, Yoojin; Nam, In-Hyun; Choi, Ui-Kyu; Kumar, Rahul; Song, Hocheol

    2016-05-01

    A composite adsorbent capable of simultaneous removal of both cationic and anionic contaminants from aqueous solutions was developed by impregnating hydrous zirconium oxide (HZO) into chitosan beads (CB). The optimal mass ratio of chitosan to HZO was 2:2. The composite adsorbent (HZOCB) had the rugged surface (52.74 m2 g-1) with irregular cracks caused by HZO inclusion and amine functional groups. The rate of Pb2+ adsorption by HZOCB was relatively rapid. Most of Pb2+ (89%) was adsorbed within 2.5 h. A binary sorbate system was noticeably favorable for F- adsorption as compared to single sorbate system. Adsorption of F- and Pb2+ followed pseudo-second order kinetics. The maximum sorption capacities obtained from Langmuir isotherm model were 22.1 and 222.2 mg g-1, respectively. The study demonstrates that the developed composite could be a potential adsorbent for the simultaneous remediation of F- and Pb2+ contamination in water.

  11. Superconducting composite with multilayer patterns and multiple buffer layers

    DOEpatents

    Wu, X.D.; Muenchausen, R.E.

    1993-10-12

    An article of manufacture is described including a substrate, a patterned interlayer of a material selected from the group consisting of magnesium oxide, barium-titanium oxide or barium-zirconium oxide, the patterned interlayer material overcoated with a secondary interlayer material of yttria-stabilized zirconia or magnesium-aluminum oxide, upon the surface of the substrate whereby an intermediate article with an exposed surface of both the overcoated patterned interlayer and the substrate is formed, a coating of a buffer layer selected from the group consisting of cerium oxide, yttrium oxide, curium oxide, dysprosium oxide, erbium oxide, europium oxide, iron oxide, gadolinium oxide, holmium oxide, indium oxide, lanthanum oxide, manganese oxide, lutetium oxide, neodymium oxide, praseodymium oxide, plutonium oxide, samarium oxide, terbium oxide, thallium oxide, thulium oxide, yttrium oxide and ytterbium oxide over the entire exposed surface of the intermediate article, and, a ceramic superconductor. 5 figures.

  12. Stabilized tin-oxide-based oxidation/reduction catalysts

    NASA Technical Reports Server (NTRS)

    Watkins, Anthony Neal (Inventor); Oglesby, Donald M. (Inventor); Gulati, Suresh T. (Inventor); Summers, Jerry C. (Inventor); Schryer, David R. (Inventor); Davis, Patricia P. (Inventor); Leighty, Bradley D. (Inventor); Jordan, Jeffrey D. (Inventor); Schryer, Jacqueline L. (Inventor)

    2008-01-01

    The invention described herein involves a novel approach to the production of oxidation/reduction catalytic systems. The present invention serves to stabilize the tin oxide reducible metal-oxide coating by co-incorporating at least another metal-oxide species, such as zirconium. In one embodiment, a third metal-oxide species is incorporated, selected from the group consisting of cerium, lanthanum, hafnium, and ruthenium. The incorporation of the additional metal oxide components serves to stabilize the active tin-oxide layer in the catalytic process during high-temperature operation in a reducing environment (e.g., automobile exhaust). Moreover, the additional metal oxides are active components due to their oxygen-retention capabilities. Together, these features provide a mechanism to extend the range of operation of the tin-oxide-based catalyst system for automotive applications, while maintaining the existing advantages.

  13. Sulfation of ceria-zirconia model automotive emissions control catalysts

    NASA Astrophysics Data System (ADS)

    Nelson, Alan Edwin

    Cerium-zirconium mixed metal oxides are used in automotive emissions control catalysts to regulate the partial pressure of oxygen near the catalyst surface. The near surface oxygen partial pressure is regulated through transfer of atomic oxygen from the ceria-zirconia solid matrix to the platinum group metals to form metal oxides capable of oxidizing carbon monoxide and unburned hydrocarbons. Although the addition of zirconium in the cubic lattice of ceria increases the oxygen storage capacity and thermal stability of the ceria matrix, the cerium-zirconium oxide system remains particularly susceptible to deactivation from sulfur compounds. While the overall effect of sulfur on these systems is understood (partially irreversible deactivation), the fundamental and molecular interaction of sulfur with ceria-zirconia remains a challenging problem. Ceria-zirconia metal oxide solid solutions have been prepared through co-precipitation with nitrate precursors. The prepared powders were calcined and subsequently formed into planer wafers and characterized for chemical and physical attributes. The prepared samples were subsequently exposed to a sulfur dioxide based environment and characterized with spectroscopic techniques to characterize the extent of sulfation and the nature of surface sulfur species. The extent of sulfation of the model ceria-zirconia systems was characterized with Auger electron spectroscopy (AES) prior to and after treatment in a microreactor. Strong dependencies were observed between the atomic ratio of ceria to zirconia and the extent of sulfation. In addition, the partial pressure of sulfur dioxide during treatments also correlated to the extent of sulfation, while temperature only slightly effected the extent of sulfation. The AES data suggests the gas phase sulfur dioxide preferentially chemisorbs on surface ceria atoms and the extent of sulfation is heavily dependent on sulfur dioxide concentrations and only slightly dependent on catalyst temperatures, as confirmed by thermal programmed desorption (TPD). While hydrogen exposure indicated slight sulfur removal, exposure to a redox environment or atmosphere nearly eliminated the quantity of chemisorbed surface sulfur. The nature of sulfur removal is attributed to the inherent redox properties of ceria-zirconia systems. The complete analysis provides mechanistic insight into sulfation dependencies and fundamental information regarding sulfur adsorption on ceria-zirconia model automotive emissions control systems.

  14. Oxygen mobility in CeO{sub 2} and Ce{sub x}Zr({sub 1-x})O{sub 2} compounds: Study by CO transient oxidation and {sup 18}O/{sup 16}O isotopic exchange

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

    Madier, Y.; Descorme, C.; Govic, A.M. Le

    Cerium-zirconium mixed oxides (Ce{sub x}Zr{sub 1{minus}x}O{sub 2}), precalcined at 900 C in dry air, were supplied by Rhodia Terres Rares as monophasic solid solutions. Introduction of some zirconium atoms in the ceria lattice by isomorphous substitution clearly influences the final properties of these materials as long as the cubic structure of ceria is maintained. Modifications in oxygen storage capacity (OSC measurements), redox properties (CO TPR), and oxygen exchange processes (TPIE) were studied. Ce{sub 0.63}Zr{sub 0.37}O{sub 2} was shown to have the most promising properties with the largest OSC at 400 C and the highest reactivity in O{sub 2} exchange. Allmore » mixed oxides are able to exchange very large amounts of oxygen compared to ceria, implying the participation of bulk oxygen. Furthermore, on Ce{sub x}Zr{sub (1{minus}x)}O{sub 2} samples, oxygen is predominantly exchanged via a multiple heteroexchange mechanism involving surface dioxygen species as superoxides or peroxides.« less

  15. Photocatalytic activity against azo dye and cytotoxicity on MCF-7 cell lines of zirconium oxide nanoparticle mediated using leaves of Lagerstroemia speciosa.

    PubMed

    Sai Saraswathi, V; Santhakumar, K

    2017-04-01

    Metal oxide nanoparticles are gaining interest in recent years. The present paper explains about the green synthesis of zirconium oxide nanoparticles (ZrO NPs) mediated from the leaves of Lagerstroemia speciosa. The prepared ZrO NPs were characterized by UV-vis spectroscopy, FT-IR, X-ray diffraction analysis (XRD), Transmission Electron Microscopy (TEM), Scanning Electron Microscopy (SEM), Energy Dispersive X-ray spectroscopy (EDX) and Thermogravimetric Analysis (TGA). The photocatalytic activity of ZrO NPs was studied for azo dye by exposing to sunlight. The azo dye was degraded up to 94.58%. Also the ZrO NPs were studied for in vitro cytotoxicity activity against breast cancer cell lines-MCF-7 and evaluated by MTT assay. The cell morphological changes were recorded by light microscope. The cells viability was seen at 500μg/mL when compared against control. Hence the research highlights, that the method was simple, eco-friendly towards environment by phytoremediation activity of the azo dye and cytotoxicity activity against MCF-7 cell lines. Hence the present paper may help to further explore the metal nanoparticle for its potential applications. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Zirconium and hafnium

    USGS Publications Warehouse

    Jones, James V.; Piatak, Nadine M.; Bedinger, George M.; Schulz, Klaus J.; DeYoung,, John H.; Seal, Robert R.; Bradley, Dwight C.

    2017-12-19

    Zirconium and hafnium are corrosion-resistant metals that are widely used in the chemical and nuclear industries. Most zirconium is consumed in the form of the main ore mineral zircon (ZrSiO4, or as zirconium oxide or other zirconium chemicals. Zirconium and hafnium are both refractory lithophile elements that have nearly identical charge, ionic radii, and ionic potentials. As a result, their geochemical behavior is generally similar. Both elements are classified as incompatible because they have physical and crystallochemical properties that exclude them from the crystal lattices of most rock-forming minerals. Zircon and another, less common, ore mineral, baddeleyite (ZrO2), form primarily as accessory minerals in igneous rocks. The presence and abundance of these ore minerals in igneous rocks are largely controlled by the element concentrations in the magma source and by the processes of melt generation and evolution. The world’s largest primary deposits of zirconium and hafnium are associated with alkaline igneous rocks, and, in one locality on the Kola Peninsula of Murmanskaya Oblast, Russia, baddeleyite is recovered as a byproduct of apatite and magnetite mining. Otherwise, there are few primary igneous deposits of zirconium- and hafnium-bearing minerals with economic value at present. The main ore deposits worldwide are heavy-mineral sands produced by the weathering and erosion of preexisting rocks and the concentration of zircon and other economically important heavy minerals, such as ilmenite and rutile (for titanium), chromite (for chromium), and monazite (for rare-earth elements) in sedimentary systems, particularly in coastal environments. In coastal deposits, heavy-mineral enrichment occurs where sediment is repeatedly reworked by wind, waves, currents, and tidal processes. The resulting heavy-mineral-sand deposits, called placers or paleoplacers, preferentially form at relatively low latitudes on passive continental margins and supply 100 percent of the world’s zircon. Zircon makes up a relatively small percentage of the economic heavy minerals in most deposits and is produced primarily as a byproduct of heavy-mineral-sand mining for titanium minerals.From 2003 to 2012, world zirconium mineral concentrates production increased by more than 40 percent, and Australia and South Africa were the leading producers. Global consumption of zirconium mineral concentrates generally increased during the same time period, largely as a result of increased demand in developing economies in Asia and the Middle East. Global demand weakened in 2012, causing a decrease in world production of zirconium mineral concentrates and delaying the development of several new mining projects. Global consumption is expected to increase in the future, however, as demand from the ceramics, chemicals, and metals industries increases (driven by renewed growth in developing economies) and demand for zirconium and hafnium metal increases (driven by the construction and operation of new nuclear powerplants).The behaviors of zirconium and hafnium in the environment are very similar to one another in that most zirconium- and hafnium-bearing minerals have limited solubility and reactivity. Anthropogenic sources of zirconium, and likely hafnium, are from industrial zirconium-containing byproducts and emissions from the processing of sponge zirconium, and exposure to the general population from these sources is small. Zirconium and hafnium are likely not essential to human health and generally are considered to be of low toxicity to humans. The main exposure risks are associated with industrial inhalation and dermal exposure. Because of the low solubility of zirconium and hafnium, ecological health concerns in the aquatic environment and in soils are minimal. Heavy-mineral-sand mining may lead to increased erosion rates when the mining is managed improperly. In addition, surface mining requires removal of the overlying organic soil layer and produces waste material that includes tailings and slimes. The soil removal and mining activity disturbs the surrounding ecosystem and alters the character of the landscape. Dry mineral separation processes create high amounts of airborne dust, whereas wet mineral separation processes do not. In operations that restore the landscape to pre-mining conditions, the volume of waste and the impact on the landscape may be relatively temporary.

  17. Surface treatment to form a dispersed Y2O3 layer on Zircaloy-4 tubes

    NASA Astrophysics Data System (ADS)

    Jung, Yang-Il; Kim, Hyun-Gil; Guim, Hwan-Uk; Lim, Yoon-Soo; Park, Jung-Hwan; Park, Dong-Jun; Yang, Jae-Ho

    2018-01-01

    Zircaloy-4 is a traditional zirconium-based alloy developed for application in nuclear fuel cladding tubes. The surfaces of Zircaloy-4 tubes were treated using a laser beam to increase their mechanical strength. Laser beam scanning of a tube coated with yttrium oxide (Y2O3) resulted in the formation of a dispersed oxide layer in the tube's surface region. Y2O3 particles penetrated the Zircaloy-4 during the laser treatment and were distributed uniformly in the surface region. The thickness of the dispersed oxide layer varied from 50 to 140 μm depending on the laser beam trajectory. The laser treatment also modified the texture of the tube. The preferred basal orientation along the normal to the tube surface disappeared, and a random structure appeared after laser processing. The most obvious result was an increase in the mechanical strength. The tensile strength of Zircaloy-4 increased by 10-20% with the formation of the dispersed oxide layer. The compressive yield stress also increased, by more than 15%. Brittle fracture was observed in the surface-treated samples during tensile and compressive deformation at room temperature; however, the fracture behavior was changed in ductile at elevated temperatures.

  18. High-Temperature Ceramic Matrix Composite with High Corrosion Resistance

    DTIC Science & Technology

    2010-06-02

    ceramics with silicide additives may be explained in the following ways: 1) metal oxide, for example Ta2O5, formed at oxidation of TaSi2, in the...practically monophase ones, possibly, the additives of corresponding metals in silicide powders were present in insignificant amounts. For...boride with zirconium silicide we prepared the mixtures with 20 vol. % of silicide , the latter being hot pressed in the temperature range of 1600

  19. Tantalum Addition to Zirconium Diboride for Improved Oxidation Resistance

    NASA Technical Reports Server (NTRS)

    Levine, Stanley R.; Opila, Eliizabeth J.

    2003-01-01

    Ultrahigh temperature ceramics have performed unreliably due to material flaws and attachment design. These deficiencies are brought to the fore by the low fracture toughness and thermal shock resistance of UHTCs. If these deficiencies are overcome, we are still faced with poor oxidation resistance as a limitation on UHTC applicability to reusable launch vehicles. We have been addressing the deficiencies of UHTCs with our focus on composite constructions and functional grading to address the mechanical issues, and on composition modification to address the oxidation issue. The approaches and progress toward the latter are reported.

  20. Controlled atmosphere for fabrication of cermet electrodes

    DOEpatents

    Ray, Siba P.; Woods, Robert W.

    1998-01-01

    A process for making an inert electrode composite wherein a metal oxide and a metal are reacted in a gaseous atmosphere at an elevated temperature of at least about 750.degree. C. The metal oxide is at least one of the nickel, iron, tin, zinc and zirconium oxides and the metal is copper, silver, a mixture of copper and silver or a copper-silver alloy. The gaseous atmosphere has an oxygen content that is controlled at about 5-3000 ppm in order to obtain a desired composition in the resulting composite.

  1. Controlled atmosphere for fabrication of cermet electrodes

    DOEpatents

    Ray, S.P.; Woods, R.W.

    1998-08-11

    A process is disclosed for making an inert electrode composite wherein a metal oxide and a metal are reacted in a gaseous atmosphere at an elevated temperature of at least about 750 C. The metal oxide is at least one of the nickel, iron, tin, zinc and zirconium oxides and the metal is copper, silver, a mixture of copper and silver or a copper-silver alloy. The gaseous atmosphere has an oxygen content that is controlled at about 5--3000 ppm in order to obtain a desired composition in the resulting composite. 2 figs.

  2. Investigation of holmium-doped zirconium oxide ceramic phosphor as an ultraviolet wavelength-discriminating laser beam viewer

    NASA Astrophysics Data System (ADS)

    Yamanoi, Kohei; Hori, Tatsuhiro; Minami, Yuki; Empizo, Melvin John F.; Luong, Mui Viet; Shiro, Atsushi; Watanabe, Jun; Iwano, Keisuke; Iwasa, Yuki; Cadatal-Raduban, Marilou; Gabayno, Jacque Lynn; Shimizu, Toshihiko; Sarukura, Nobuhiko; Norimatsu, Takayoshi

    2018-01-01

    We report the fluorescence spectra of ZrO2 and trivalent Ho-doped ZrO2 ceramics under ultraviolet (UV) excitation at 213, 266, and 355 nm wavelengths. The Ho3+-doped ZrO2 ceramics exhibited varying fluorescence color tones depending on the excitation wavelength used. The different color tones match the fluorescence spectrum characteristics at each excitation wavelength. Our results demonstrate that Ho3+-doped ZrO2 ceramics can discriminate between UV light, specifically the third, fourth, and fifth harmonics of a Nd:YAG laser. It can potentially be used for developing UV laser beam viewers to aid laser alignment.

  3. 21 CFR 82.2051 - Lakes (Ext. D&C).

    Code of Federal Regulations, 2010 CFR

    2010-04-01

    ..., titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or on any combination of... is a salt in which is combined the basic radical sodium, potassium, barium, or calcium; or (ii) a... color with the basic radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium. (2...

  4. 21 CFR 82.2051 - Lakes (Ext. D&C).

    Code of Federal Regulations, 2012 CFR

    2012-04-01

    ..., titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or on any combination of... is a salt in which is combined the basic radical sodium, potassium, barium, or calcium; or (ii) a... color with the basic radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium. (2...

  5. 21 CFR 82.2051 - Lakes (Ext. D&C).

    Code of Federal Regulations, 2013 CFR

    2013-04-01

    ..., titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or on any combination of... is a salt in which is combined the basic radical sodium, potassium, barium, or calcium; or (ii) a... color with the basic radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium. (2...

  6. 21 CFR 82.2051 - Lakes (Ext. D&C).

    Code of Federal Regulations, 2014 CFR

    2014-04-01

    ..., titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or on any combination of... is a salt in which is combined the basic radical sodium, potassium, barium, or calcium; or (ii) a... color with the basic radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium. (2...

  7. 21 CFR 82.2051 - Lakes (Ext. D&C).

    Code of Federal Regulations, 2011 CFR

    2011-04-01

    ..., titanium dioxide, zinc oxide, talc, rosin, aluminum benzoate, calcium carbonate, or on any combination of... is a salt in which is combined the basic radical sodium, potassium, barium, or calcium; or (ii) a... color with the basic radical sodium, potassium, aluminum, barium, calcium, strontium, or zirconium. (2...

  8. Quercetin as colorimetric reagent for determination of zirconium

    USGS Publications Warehouse

    Grimaldi, F.S.; White, C.E.

    1953-01-01

    Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50?? of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K1 = 0.33 ?? 10-5 and K2 = 1.3 ?? 10-9. Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

  9. Capabilities of laser ablation mass spectrometry in the differentiation of natural and artificial opal gemstones.

    PubMed

    Erel, Eric; Aubriet, Frédéric; Finqueneisel, Gisèle; Muller, Jean-François

    2003-12-01

    The potentialities of laser ablation coupled to ion cyclotron resonance Fourier transform mass spectrometry are evaluated to distinguish natural and artificial opals. The detection of specific species in both ion detection modes leads us to obtain relevant criteria of differentiation. In positive ions, species including hafnium and large amounts of zirconium atoms are found to be specific for artificial opal. In contrast, aluminum, titanium, iron, and rubidium are systematically detected in the study of natural opals. Moreover, some ions allow us to distinguish between natural opal from Australia and from Mexico. Australian gemstone includes specifically strontium, cesium, and barium. Moreover, it is also found that the yield of (H2O)0-1(SiO2)nX- (X- = O-, OH-, KO-, NaO-, SiO2-, AlO1-2-, FeO2-, ZrO2-, and ZrO3-) and (Al2O3)(SiO2)nAlO2- ions depends on the composition of the sample when opals are laser ablated. Ions, which include zirconium oxide species, are characteristics of artificial gem. In contrast, natural opals lead us, after laser ablation, to the production of ions including H2O, Al2O3 motifs and AlO-, KO-, NaO-, and FeO2- species.

  10. Chitosan /Zeolite Y/Nano ZrO2 nanocomposite as an adsorbent for the removal of nitrate from the aqueous solution.

    PubMed

    Teimouri, Abbas; Nasab, Shima Ghanavati; Vahdatpoor, Niaz; Habibollahi, Saeed; Salavati, Hossein; Chermahini, Alireza Najafi

    2016-12-01

    In the present study, a series of chitosan/Zeolite Y/Nano Zirconium oxide (CTS/ZY/Nano ZrO 2 ) nanocomposites were made by controlling the molar ratio of chitosan (CTS) to Zeolite Y/Nano Zirconium oxide in order to remove nitrate (NO 3 - ) ions in the aqueous solution. The nanocomposite adsorbents were characterized by XRD, FTIR, BET, SEM and TEM. The influence of different molar ratios of CTS to ZY/Nano ZrO 2 , the initial pH value of the nitrate solution, contact time, temperature, the initial concentration of nitrate and adsorbent dose was studied. The adsorption isotherms and kinetics were also analyzed. It was attempted to describe the sorption processes by the Langmuir equation and the theoretical adsorption capacity (Q 0 ) was found to be 23.58mg nitrate per g of the adsorbent. The optimal conditions for nitrate removal were found to be: molar ratio of CTS/ZY/Nano ZrO 2 : 5:1; pH: 3; 0.02g of adsorbent and temperature: 35°C, for 60min. The adsorption capacities of CTS, ZY, Nano ZrO 2 , CTS/Nano ZrO 2 , CTS/ZY and CTS/ZY/Nano ZrO 2 nanocomposites for nitrate removal were compared, showing that the adsorption ability of CTS/ZY/Nano ZrO 2 nanocomposite was higher than the average values of those of CTS (1.95mg/g for nitrate removal), ZY, Nano ZrO 2 , CTS/Nano ZrO 2, and CTS/ZY. Copyright © 2016. Published by Elsevier B.V.

  11. Thermodynamic Analysis and Growth of Zirconium Carbide by Chemical Vapor Deposition

    NASA Astrophysics Data System (ADS)

    Wei, Sun; Hua, Hao Zheng; Xiang, Xiong

    Equilibrium calculations were used to optimize conditions for the chemical vapor deposition of zirconium carbide from zirconium halide + CxHy+H2+Ar system. The results show the CVD-ZrC phase diagram is divided into ZrC+C, ZrC and ZrC+Zr zones by C, Zr generating lines. For the same mole of ZrCl4 reactant, it needs higher concentration of CH4 to generate single ZrC phase than that of C3H6. Using these calculations as a guide, single-phase cubic zirconium carbide coatings were deposited onto graphite substrate.

  12. SEPARATION OF URANIUM FROM ZIRCONIUM AND NIOBIUM BY SOLVENT EXTRACTION

    DOEpatents

    Voiland, E.E.

    1958-05-01

    A process for separation of the uranium from zirconium and/or niobium values contained in 3 to 7M aqueous nitric acid solutions is described. This is accomplished by adding phosphoric acid anions to the nitric acid solution containing the uranium, zirconium, and/or niobium in an amount sufficient to make the solution 0.05 to 0.2M in phosphate ion and contacting the solution with an organic water-immiscible solvent such as MEK, whereby the uranyl values are taken up by the extract phase while the zirconium and niobium preferentially remain in the aqueous raffinate.

  13. 78 FR 40200 - Duke Energy Carolinas, LLC, Oconee Nuclear Station Units 1, 2, and 3; Independent Spent Fuel...

    Federal Register 2010, 2011, 2012, 2013, 2014

    2013-07-03

    ... breaches.'' Zircaloy is a type of zirconium alloy which includes both Zircaloy-2 and Zircaloy-4 cladding, but does not include M5 cladding. The M5 is a different type of zirconium alloy, which does not... ``zirconium alloy'' clad spent fuel assemblies in the 24PHB DSC, which would include both the ``zircaloy clad...

  14. Establishment of the roadmap for chlorination process development for zirconium recovery and recycle

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

    Collins, E.D.; Del Cul, G.D.; Spencer, B.B.

    Process development studies are being conducted to recover, purify, and reuse the zirconium (about 98.5% by mass) in used nuclear fuel (UNF) zirconium alloy cladding. Feasibility studies began in FY 2010 using empty cladding hulls that were left after fuel dissolution or after oxidation to a finely divided oxide powder (voloxidation). In FY 2012, two industrial teams (AREVA and Shaw-Westinghouse) were contracted by the Department of Energy Office of Nuclear Energy (NE) to provide technical assistance to the project. In FY 2013, the NE Fuel Cycle Research and Development Program requested development of a technology development roadmap to guide futuremore » work. The first step in the roadmap development was to assess the starting point, that is, the current state of the technology and the end goal. Based on previous test results, future work is to be focused on first using chlorine as the chlorinating agent and secondly on the use of a process design that utilizes a chlorination reactor and dual ZrCl{sub 4} product salt condensers. The likely need for a secondary purification step was recognized. Completion of feasibility testing required an experiment on the chemical decladding flowsheet option. This was done during April 2013. The roadmap for process development will continue through process chemistry optimization studies, the chlorinated reactor design configuration, product salt condensers, and the off-gas trapping of tritium or other volatile fission products from the off-gas stream. (authors)« less

  15. Exceptional capability of nanosized CeO(2) materials to "dissolve" lanthanide oxides established by time-gated excitation and emission spectroscopy.

    PubMed

    Tiseanu, Carmen; Parvulescu, Vasile; Avram, Daniel; Cojocaru, Bogdan; Sanchez-Dominguez, Margarita

    2014-05-28

    The atomic scale homogeneity of Ce and Zr oxygen bonds represents the main reason for enhanced total oxygen storage capability of CeO2-ZrO2 (Ce/Zr = 1) as compared to that of CeO2. Here, we demonstrate that the addition of 10% Eu(3+) by wet impregnation on preformed nanosized CeO2-ZrO2 (Ce/Zr = 1) followed by calcination induces a remarkable homogeneity of 10% Eu(3+)-CeO2-ZrO2 solid solution. By use of time-resolved emission and excitation spectroscopies, the improvement of the nanoscale chemical and structural homogeneity of 10% Eu(3+)-CeO2-ZrO2 calcined at 1000 as compared to sample calcined at 750 °C is demonstrated. Based on the comparison of luminescence properties of 10% Eu(3+) impregnated on preformed nanosized CeO2-ZrO2 and CeO2, we also show that the presence of zirconium does not only preserve the ability of cerium oxide to "dissolve" lanthanide oxide, but also determines an important stabilization of defects (oxygen vacancies) generated upon Eu(3+) doping.

  16. Capture of Tritium Released from Cladding in the Zirconium Recycle Process

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

    Spencer, Barry B.; Walker, T. B.; Bruffey, S. H.

    2016-08-31

    Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-based cladding and could be released from the cladding when themore » solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using nonradioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.« less

  17. Capture of Tritium Released from Cladding in the Zirconium Recycle Process

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

    Spencer, Barry B.; Walker, T. B.; Bruffey, Stephanie H.

    2016-08-31

    This report is issued as the first revision to FCRD-MRWFD-2016-000297. Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-basedmore » cladding and could be released from the cladding when the solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using non-radioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.« less

  18. Effect of ceramic nanoparticles on the solid-state reaction mechanism of dolomite-zirconium oxide followed by neutron thermodiffraction measurements

    NASA Astrophysics Data System (ADS)

    Serena, S.; Caballero, A.; Turrillas, X.; Martin, D.; Sainz, M. A.

    2009-05-01

    Calcium zirconate-magnesium oxide material was obtained by solid-state reaction from mixed dolomite (CaMg(CO3)2) and zirconia (m-ZrO2) nanopowders. The nanopowders were obtained by high-energy milling, which produced an increase of the superficial free energy of the particles. The role of nanoparticles in the reaction process of monoclinic-zirconia and dolomite was analysed for the first time using neutron thermodiffraction and differential thermal analysis-thermogravimetric techniques. The neutron thermodiffraction of this mixture provides a clear description in situ of the different decomposition and reaction processes that occur in the nanopowders mixture. The results make it possible to analyze the effect of the nanoparticles on the reaction behaviour of these materials.

  19. Composite anion-exchangers modified with nanoparticles of hydrated oxides of multivalent metals

    NASA Astrophysics Data System (ADS)

    Maltseva, T. V.; Kolomiets, E. O.; Dzyazko, Yu. S.; Scherbakov, S.

    2018-02-01

    Organic-inorganic composite ion-exchangers based on anion exchange resins have been obtained. Particles of one-component and two-component modifier were embedded using the approach, which allows us to realize purposeful control of a size of the embedded particles. The approach is based on Ostwald-Freundlich equation, which was adapted to deposition in ion exchange matrix. The equation was obtained experimentally. Hydrated oxides of zirconium and iron were applied to modification, concentration of the reagents were varied. The embedded particles accelerate sorption, the rate of which is fitted by the model equation of chemical reactions of pseudo-second order. When sorption of arsenate ions from very diluted solution (50 µg dm-3) occurs, the composites show higher distribution coefficients comparing with the pristine resin.

  20. Methodology for the effective stabilization of tin-oxide-based oxidation/reduction catalysts

    NASA Technical Reports Server (NTRS)

    Jordan, Jeffrey D. (Inventor); Schryer, David R. (Inventor); Leighty, Bradley D. (Inventor); Watkins, Anthony N. (Inventor); Summers, Jerry C. (Inventor); Davis, Patricia P. (Inventor); Oglesby, Donald M. (Inventor); Schryer, Jacqueline L. (Inventor); Gulati, Suresh T. (Inventor)

    2011-01-01

    The invention described herein involves a novel approach to the production of oxidation/reduction catalytic systems. The present invention serves to stabilize the tin oxide reducible metal-oxide coating by co-incorporating at least another metal-oxide species, such as zirconium. In one embodiment, a third metal-oxide species is incorporated, selected from the group consisting of cerium, lanthanum, hafnium, and ruthenium. The incorporation of the additional metal oxide components serves to stabilize the active tin-oxide layer in the catalytic process during high-temperature operation in a reducing environment (e.g., automobile exhaust). Moreover, the additional metal oxides are active components due to their oxygen-retention capabilities. Together, these features provide a mechanism to extend the range of operation of the tin-oxide-based catalyst system for automotive applications, while maintaining the existing advantages.

  1. Effect of Zirconium Oxide and Zinc Oxide Nanoparticles on Physicochemical Properties and Antibiofilm Activity of a Calcium Silicate-Based Material

    PubMed Central

    Guerreiro-Tanomaru, Juliane Maria; Trindade-Junior, Adinael; Cesar Costa, Bernardo; da Silva, Guilherme Ferreira; Drullis Cifali, Leonardo; Basso Bernardi, Maria Inês

    2014-01-01

    The aim of the present study was to evaluate the antibiofilm activity against Enterococcus faecalis, compressive strength. and radiopacity of Portland cement (PC) added to zirconium oxide (ZrO2), as radiopacifier, with or without nanoparticulated zinc oxide (ZnO). The following experimental materials were evaluated: PC, PC + ZrO2, PC + ZrO2 + ZnO (5%), and PC + ZrO2 + ZnO (10%). Antibiofilm activity was analyzed by using direct contact test (DCT) on Enterococcus faecalis biofilm, for 5 h or 15 h. The analysis was conducted by using the number of colony-forming units (CFU/mL). The compressive strength was performed in a mechanical testing machine. For the radiopacity tests, the specimens were radiographed together with an aluminium stepwedge. The results were submitted to ANOVA and Tukey tests, with level of significance at 5%. The results showed that all materials presented similar antibiofilm activity (P > 0.05). The addition of nanoparticulated ZnO decreased the compressive strength of PC. All materials presented higher radiopacity than pure PC. It can be concluded that the addition of ZrO2 and ZnO does not interfere with the antibiofilm activity and provides radiopacity to Portland cement. However, the presence of ZnO (5% or 10%) significantly decreased the compressive strength of the materials. PMID:25431798

  2. Corrigendum to "Preliminary assessment of accident-tolerant fuels on LWR performance during normal operation and under DB and BDB accident conditions" [J. Nucl. Mater. 448 (2014) 520-533

    NASA Astrophysics Data System (ADS)

    Ott, L. J.; Robb, K. R.; Wang, D.

    2015-06-01

    In Section 5.2, certain material properties for "FeCrAl oxide" were not modeled based on "stainless steel oxide" as indicated in the text. Instead, the "FeCrAl oxide" material properties were modeled using the default properties in MELCOR for "zirconium oxide". The properties affected are the FeCrAl oxide density, specific heat, enthalpy, thermal conductivity, melting point, and latent heat of fusion. Table 5.1 and Figs. 5.1a-d from Section 5.2 have been corrected below. As discussed below, the overall conclusions of the paper remain unchanged.

  3. Synthesis and nonstoichiometry of the zirconium trihalides

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

    Daake, R.L.; Corbett, J.D.

    1978-05-01

    The synthesis of ZrX/sub 3/ (X = Cl, Br, I) by reaction of the corresponding tetrahalides with ZrCl, ZrBr, or ZrI/sub 1.8/ in sealed tantalum tubing gives high-purity, single-phase products, thereby avoiding problems of the relatively low reactivity of and contamination by zirconium powder reductant used previously. Phase limits for the three trihalides established by isopiestic equilibration with the adjoining phases are 2.94 (2) less than or equal to Cl:Zr less than or equal to 3.03 (2) (440/sup 0/C), 2.87 (2) less than or equal to Br:Zr less than or equal to 3.23 (2) (435/sup 0/C), and 2.83 (5) (775/supmore » 0/C) less than or equal to I:Zr less than or equal to 3.43 (5) (475/sup 0/C). The hexagonal lattice constants for the bromide phase (Guinier techniques) decrease linearly with increasing bromide content across the entire range without the development of any additional lines. The variation of the c dimension for ZrI/sub 3/ (and HfI/sub 3/) on oxidation is in the opposite direction, and in this case extra lines from a presumed superlattice structure developed toward the upper limit. The structural implications of these results are considered. The reported structure for ..cap alpha..-ZrCl/sub 3/, an unusual BiI/sub 3/-type variant, was based on a misassigned ZrCl powder pattern and therefore appears to be in error. 25 references.« less

  4. Characterisation of well-adhered ZrO2 layers produced on structured reactors using the sonochemical sol-gel method

    NASA Astrophysics Data System (ADS)

    Jodłowski, Przemysław J.; Chlebda, Damian K.; Jędrzejczyk, Roman J.; Dziedzicka, Anna; Kuterasiński, Łukasz; Sitarz, Maciej

    2018-01-01

    The aim of this study was to obtain thin zirconium dioxide coatings on structured reactors using the sonochemical sol-gel method. The preparation method of metal oxide layers on metallic structures was based on the synergistic combination of three approaches: the application of ultrasonic irradiation during the synthesis of Zr sol-gel based on a precursor solution containing zirconium(IV) n-propoxide, the addition of stabilszing agents, and the deposition of ZrO2 on the metallic structures using the dip-coating method. As a result, dense, uniform zirconium dioxide films were obtained on the FeCrAlloy supports. The structured reactors were characterised by various physicochemical methods, such as BET, AFM, EDX, XRF, XRD, XPS and in situ Raman spectroscopy. The results of the structural analysis by Raman and XPS spectroscopy confirmed that the metallic surface was covered by a ZrO2 layer without any impurities. SEM/EDX mapping revealed that the deposited ZrO2 covered the metallic support uniformly. The mechanical and high temperature tests showed that the developed ultrasound assisted sol-gel method is an efficient way to obtain thin, well-adhered zirconium dioxide layers on the structured reactors. The prepared metallic supports covered with thin ZrO2 layers may be a good alternative to layered structured reactors in several dynamics flow processes, for example for gas exhaust abatement.

  5. SiC Composite for Fuel Structure Applications

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

    Yueh, Ken

    Extensive evaluation was performed to determine the suitability of using SiC composite as a boiling water reactor (BWR) fuel channel material. A thin walled SiC composite box, 10 cm in dimension by approximately 1.5 mm wall thickness was fabricated using chemical vapor deposition (CVD) for testing. Mechanical test results and performance evaluations indicate the material could meet BWR channel mechanical design requirement. However, large mass loss of up to 21% was measured in in-pile corrosion test under BWR-like conditions in under 3 months of irradiation. A fresh sister sample irradiated in a follow-up cycle under PWR conditions showed no measureablemore » weight loss and thus supports the hypothesis that the oxidizing condition of the BWR-like coolant chemistry was responsible for the high corrosion rate. A thermodynamic evaluation showed SiC is not stable and the material may oxidize to form SiO 2 and CO 2. Silica has demonstrated stability in high temperature steam environment and form a protective oxide layer under severe accident conditions. However, it does not form a protective layer in water under normal BWR operational conditions due to its high solubility. Corrosion product stabilization by modifying the SiC CVD surface is an approach evaluated in this study to mitigate the high corrosion rate. Titanium and zirconium have been selected as stabilizing elements since both TiSiO 4 and ZrSiO 4 are insoluble in water. Corrosion test results in oxygenated water autoclave indicate TiSiO4 does not form a protective layer. However, zirconium doped test samples appear to form a stable continuous layer of ZrSiO 4 during the corrosion process. Additional process development is needed to produce a good ZrSiC coating to verify functionality of the mitigation concept.« less

  6. Highly Efficient and Selective Photooxidation of Sulfur Mustard Simulant by a Triazolobenzothiadiazole-Moiety-Functionalized Metal-Organic Framework in Air.

    PubMed

    Zhang, Wen-Qiang; Cheng, Ke; Zhang, He; Li, Qiu-Yan; Ma, Zheng; Wang, Zixuan; Sheng, Jialing; Li, Yinwei; Zhao, Xinsheng; Wang, Xiao-Jun

    2018-04-16

    A photoactive triazolobenzothiadiazole (TBTD)-conjugated terphenyldicarboxylate (TPDC) linker was introduced into a porous and robust UiO-68 isoreticular zirconium metal-organic framework (denoted as UiO-68-TBTD) by the de novo synthetic approach of mixed TPDC struts. Under blue-light-emitting-diode irradiation, UiO-68-TBTD can serve as a heterogeneous photocatalyst for the highly efficient and selective oxidation of a sulfur mustard simulant (2-chloroethyl ethyl sulfide) to the corresponding much less toxic sulfoxide product, with a half-life of only 3 min in the open air atmosphere.

  7. Measurement of the distribution coefficient of neodymium in cubic ZrO 2

    NASA Astrophysics Data System (ADS)

    Römer, H.; Luther, K.-D.; Assmus, W.

    1993-05-01

    The incorporation of solute elements into single crystals has been examined for many years. In this paper we investigate the distribution coefficient of Nd 2O 3 in cubic stabilized zirconiumdioxide crystals. The distribution coefficient is measured as a function of the growth velocity. The validity of the Burton-Prim-Slichter theory [J.A. Burton, R.C. Prim and W.P. Slichter, J. Chem. Phys. 21 (1953) 1987] for the system zirconium dioxide/yttrium oxide is confirmed by the experimental results. The value for the equilibrium distribution coefficient is evaluated as k0 = 0.426.

  8. Mesoporous Silica-Supported Amidozirconium-Catalyzed Carbonyl Hydroboration

    DOE PAGES

    Eedugurala, Naresh; Wang, Zhuoran; Chaudhary, Umesh; ...

    2015-11-04

    The hydroboration of aldehydes and ketones using a silica-supported zirconium catalyst is reported. Reaction of Zr(NMe 2) 4 and mesoporous silica nanoparticles (MSN) provides the catalytic material Zr(NMe 2) n@MSN. Exhaustive characterization of Zr(NMe 2) n@MSN with solid-state (SS)NMR and infrared spectroscopy, as well as through reactivity studies, suggests its surface structure is primarily ≡SiOZr(NMe 2) 3. The presence of these nitrogen-containing zirconium sites is supported by 15N NMR spectroscopy, including natural abundance 15N NMR measurements using dynamic nuclear polarization (DNP) SSNMR. The Zr(NMe 2) n@MSN material reacts with pinacolborane (HBpin) to provide Me 2NBpin and the material ZrH/Bpin@MSN thatmore » is composed of interacting surface-bonded zirconium hydride and surface-bonded borane ≡SiOBpin moieties in an approximately 1:1 ratio, as well as zirconium sites coordinated by dimethylamine. The ZrH/Bpin@MSN is characterized by 1H/ 2H and 11B SSNMR and infrared spectroscopy and through its reactivity with D 2. The zirconium hydride material or the zirconium amide precursor Zr(NMe 2) n@MSN catalyzes the selective hydroboration of aldehydes and ketones with HBpin in the presence of functional groups that are often reduced under hydroboration conditions or are sensitive to metal hydrides, including olefins, alkynes, nitro groups, halides, and ethers. Remarkably, this catalytic material may be recycled without loss of activity at least eight times, and air-exposed materials are catalytically active. These supported zirconium centers are robust catalytic sites for carbonyl reduction and that surface-supported, catalytically reactive zirconium hydride may be generated from zirconium-amide or zirconium alkoxide sites.« less

  9. Mesoporous Silica-Supported Amidozirconium-Catalyzed Carbonyl Hydroboration

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

    Eedugurala, Naresh; Wang, Zhuoran; Chaudhary, Umesh

    The hydroboration of aldehydes and ketones using a silica-supported zirconium catalyst is reported. Reaction of Zr(NMe 2) 4 and mesoporous silica nanoparticles (MSN) provides the catalytic material Zr(NMe 2) n@MSN. Exhaustive characterization of Zr(NMe 2) n@MSN with solid-state (SS)NMR and infrared spectroscopy, as well as through reactivity studies, suggests its surface structure is primarily ≡SiOZr(NMe 2) 3. The presence of these nitrogen-containing zirconium sites is supported by 15N NMR spectroscopy, including natural abundance 15N NMR measurements using dynamic nuclear polarization (DNP) SSNMR. The Zr(NMe 2) n@MSN material reacts with pinacolborane (HBpin) to provide Me 2NBpin and the material ZrH/Bpin@MSN thatmore » is composed of interacting surface-bonded zirconium hydride and surface-bonded borane ≡SiOBpin moieties in an approximately 1:1 ratio, as well as zirconium sites coordinated by dimethylamine. The ZrH/Bpin@MSN is characterized by 1H/ 2H and 11B SSNMR and infrared spectroscopy and through its reactivity with D 2. The zirconium hydride material or the zirconium amide precursor Zr(NMe 2) n@MSN catalyzes the selective hydroboration of aldehydes and ketones with HBpin in the presence of functional groups that are often reduced under hydroboration conditions or are sensitive to metal hydrides, including olefins, alkynes, nitro groups, halides, and ethers. Remarkably, this catalytic material may be recycled without loss of activity at least eight times, and air-exposed materials are catalytically active. These supported zirconium centers are robust catalytic sites for carbonyl reduction and that surface-supported, catalytically reactive zirconium hydride may be generated from zirconium-amide or zirconium alkoxide sites.« less

  10. Effect of additives on the volatility of elements in a DC arc during the atomic emission analysis of nickel(II) oxide

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

    Zolotareva, N.I.; Kuzyakov, Yu.Ya.; Khlystova, A.D.

    1986-10-20

    The authors have studied the effect of traditional halogenating additives, AgCl, CdF/sub 2/, PTFE and that of an effective additive they have selected, ZnF/sub 2/, on the volatility of impurity elements, viz. tungsten, molybdenum, titanium, and zirconium from nickel (II) oxide, and determined the constants for the average relative volatility of the elements by the method of Kantor and Pungor. The results have been used to lower the limits of detection of the impurities cited in nickel(II) oxide.

  11. Development of Enhanced Window layers for CIGS Photovoltaic Devices

    NASA Astrophysics Data System (ADS)

    Alexander, J. Nicholas

    One of the most promising thin film devices right now is the Copper Indium Gallium Selenide (CIGS) solar cell with maximum reported power conversion efficiency of 22.3%. The Transparent Conducting Oxide (TCO) which is the top layer of the CIGS device also known as the window layer, is responsible for collecting the electrons generated in the CIGS device and conducting them to the circuit. Development of a very low resistivity film with a high optical transmission is crucial for optimal performance of devices as well as the ability to be deployed without changes to their properties for several decades. Current TCOs such as indium tin oxide (ITO) and aluminum doped zinc oxide (AZO) are met with limitations with either using large amounts of expensive materials such as indium, often requiring and anneal step to obtain good conductivity, or have shown poor long term reliability. This thesis is focused on development of InZnO and zirconium doped InZnO as a potential replacement TCO to obtain high conductivity and high transmission like the leading TCOs without needing heated depositions, post deposition annealing, and maintain a good film reliability. Zirconium doping was employed to farther enhance both the optical and electrical properties through enhancement of the films high frequency permittivity of InZnO while providing improved reliability to the film. The films were grown through a mix of DC and RF co-sputtering. InZnO films were deposited at varying indium concentration ( 10-30%) and samples were able to achieve low resistivity ( 7x10-4 O-cm), high mobility (>30 cm2/v.s), high carrier concentration (>10 20 cm-3), while maintaining high transmission (> 80%) in the visible and near-infrared region. After zirconium was incorporated into the InZnO films by replacement of the ZnO target with a ZrO2/ZnO (5:95) target, films of Zr:InZnO were deposit through the same method to achieve films that maintained very similar electrical and optical properties. The little change found in the elerical and optical properties has strongly indicated that incorporation of zirconium into the InZnO thin film may not be replacing indium and zinc in the structure of the film and not influence the high frequency permittivity and carrier concentration of InZnO. It is also shown that the incorporation of zirconium does not indicate any detrimental effects on the properties of InZnO. To investigate film reliability, a custom damp-heat chamber was designed in this study to expose samples of InZnO/SLG (soda lime glass), Zr:InZnO/SLG, and AZO up to 5000 hours in approximately 85°C and 85% relative humidity to accelerate the degradation rate of the films. AZO was found to degrade very rapidly and enter MO resistance in approximately 1 week in this damp heat setup, while the majority of InZnO and Zr:InZnO films remained conductive through the entire experiment. It was found films showed improvements to their reliability with increases in film thickness and indium content, decreases in the amount of oxygen present in the films (containing more oxygen vacancies), and films incorporated with zirconium. Zirconium may not have had the desired impact to the electrical and optical properties, but by adding zirconium doping and tailoring oxygen incorporation, films of Zr:InZnO were able to show no significant change in several thousand hours exposed to the damp-heat environment. Films were also investigated by XPS and chemical analysis showed hydroxide formation, which similar to AZO is likely the reason for performance degradation. Even in samples that did not heavily change in electrical properties show indication of diffusion of moisture through the film which is a potential problem for degradation at the interfaces in completed CIGS devices. In Addition to the TCO studies, two other studies are performed in this work on CIGS and photovoltaic related work. First the CdS layer, which is part of the window layers, usually referred to as the n-type buffer layer, had an alternative deposition chemistry investigated. This new chemistry replacing thiourea with N-methylthiourea was used in a chemical bath deposition (CBD). This new chemistry yielded more controlled growth kinetics with a wider processing window. The films grown using this chemistry were more uniform than those grown with the standard process using thiourea. These uniform films were shown to have more complete surface coverage at very thin layers ( 20-30 nm). The second study investigated commercial modules of crystalline silicon, CIGS, and CdTe based technologies with a total system capacity of approximately 100 kW. The system is fitted with current, voltage, temperature, irradiance, and a complete weather station. The purpose of the system is to investigate different panel technologies and monitoring challenges in northeast climates and to track their degradation over time. (Abstract shortened by ProQuest.).

  12. Changes in the state of iron atoms in Zr alloys during corrosion tests in an autoclave

    NASA Astrophysics Data System (ADS)

    Filippov, V. P.; Bateev, A. B.; Lauer, Yu. A.; Kargin, N. I.; Petrov, V. I.

    2014-04-01

    Mössbauerinvestigations were carried out on oxide films formed on specimens of zirconium alloys Zr-1.0 %wtFe-1.2 %wtSn-0.5 %wtCr subjected to corrosion in steam-water environment at a temperature of 360 °C and at a pressure of 16.8 MPa with lithium and boron additions, and on Zr-1.4 %wtFe-0.7 %wtCr corroded in steam-water environment at 350 °C and 16.8 MPa as well as in steam-water environment at 500 °C and 10 MPa. In the metal part of the samples, under the oxide film, the iron atoms are in form of intermetallic precipitates of Zr(Fe, Cr)2. The corrosion process decomposes the intermetallic precipitates and particles are formed of metallic iron with inclusions of chromium atoms -Fe(Cr), α-Fe2O3 and Fe3O4 compounds. Part of the iron ions are in divalent and part in trivalent paramagnetic states. It is proposed that some part of the iron containing oxide precipitates in the oxide film may be in the form of nanoparticles which pass from the superparamagnetic to the ferromagnetic state with decreasing temperature.

  13. Chemically Layered Porous Solids

    NASA Technical Reports Server (NTRS)

    Koontz, Steve

    1991-01-01

    Aerogels and other porous solids in which surfaces of pores have chemical properties varying with depth below macroscopic surfaces prepared by sequences of chemical treatments. Porous glass or silica bead treated to make two depth zones having different chemical properties. Beads dropped along tube filled with flowing gas containing atomic oxygen, generated in microwave discharge. General class of materials treatable include oxides of aluminum, silicon, zirconium, tin, titanium, and nickel, and mixtures of these oxides. Potential uses of treated materials include chromatographic separations, membrane separations, controlled releases of chemicals, and catalysis.

  14. Development of biocomposed material based on zirconium oxide for regeneration of bone tissue

    NASA Astrophysics Data System (ADS)

    Lytkin, Ivan; Buyakov, Ales; Kurzina, Irina

    2017-11-01

    Porous ceramic materials based on magnesium oxide stabilized zirconia were studied. The pore structure and thin crystalline structure were studied. The porosity of some of the materials studied was obtained by conducting a pore-forming additive, UHMWPE. It is shown that after impregnation with polylactide, the residual porosity varies from 22.5 to 5.9%. The average pore size was 2 µm. X-Ray diffraction analysis showed that the fine crystal structure of the ceramic is mainly represented by baddeleyite.

  15. Versatile Oxide Films Protect FeCrAl Alloys Under Normal Operation and Accident Conditions in Light Water Power Reactors

    NASA Astrophysics Data System (ADS)

    Rebak, Raul B.

    2018-02-01

    The US has currently a fleet of 99 nuclear power light water reactors which generate approximately 20% of the electricity consumed in the country. Near 90% of the reactors are at least 30 years old. There are incentives to make the existing reactors safer by using accident tolerant fuels (ATF). Compared to the standard UO2-zirconium-based system, ATF need to tolerate loss of active cooling in the core for a considerably longer time while maintaining or improving the fuel performance during normal operation conditions. Ferritic iron-chromium-aluminum (FeCrAl) alloys have been identified as an alternative to replace current zirconium alloys. They contain Fe (base) + 10-22 Cr + 4-6 Al and may contain smaller amounts of other elements such as molybdenum and traces of others. FeCrAl alloys offer outstanding resistance to attack by superheated steam by developing an alumina oxide on the surface in case of a loss of coolant accident like at Fukushima. FeCrAl alloys also perform well under normal operation conditions both in boiling water reactors and pressurized water reactors because they are protected by a thin oxide rich in chromium. Under normal operation condition, the key element is Cr and under accident conditions it is Al.

  16. Ablation-resistant carbide Zr0.8Ti0.2C0.74B0.26 for oxidizing environments up to 3,000 °C

    NASA Astrophysics Data System (ADS)

    Zeng, Yi; Wang, Dini; Xiong, Xiang; Zhang, Xun; Withers, Philip J.; Sun, Wei; Smith, Matthew; Bai, Mingwen; Xiao, Ping

    2017-06-01

    Ultra-high temperature ceramics are desirable for applications in the hypersonic vehicle, rockets, re-entry spacecraft and defence sectors, but few materials can currently satisfy the associated high temperature ablation requirements. Here we design and fabricate a carbide (Zr0.8Ti0.2C0.74B0.26) coating by reactive melt infiltration and pack cementation onto a C/C composite. It displays superior ablation resistance at temperatures from 2,000-3,000 °C, compared to existing ultra-high temperature ceramics (for example, a rate of material loss over 12 times better than conventional zirconium carbide at 2,500 °C). The carbide is a substitutional solid solution of Zr-Ti containing carbon vacancies that are randomly occupied by boron atoms. The sealing ability of the ceramic's oxides, slow oxygen diffusion and a dense and gradient distribution of ceramic result in much slower loss of protective oxide layers formed during ablation than other ceramic systems, leading to the superior ablation resistance.

  17. Ablation-resistant carbide Zr0.8Ti0.2C0.74B0.26 for oxidizing environments up to 3,000 °C.

    PubMed

    Zeng, Yi; Wang, Dini; Xiong, Xiang; Zhang, Xun; Withers, Philip J; Sun, Wei; Smith, Matthew; Bai, Mingwen; Xiao, Ping

    2017-06-14

    Ultra-high temperature ceramics are desirable for applications in the hypersonic vehicle, rockets, re-entry spacecraft and defence sectors, but few materials can currently satisfy the associated high temperature ablation requirements. Here we design and fabricate a carbide (Zr 0.8 Ti 0.2 C 0.74 B 0.26 ) coating by reactive melt infiltration and pack cementation onto a C/C composite. It displays superior ablation resistance at temperatures from 2,000-3,000 °C, compared to existing ultra-high temperature ceramics (for example, a rate of material loss over 12 times better than conventional zirconium carbide at 2,500 °C). The carbide is a substitutional solid solution of Zr-Ti containing carbon vacancies that are randomly occupied by boron atoms. The sealing ability of the ceramic's oxides, slow oxygen diffusion and a dense and gradient distribution of ceramic result in much slower loss of protective oxide layers formed during ablation than other ceramic systems, leading to the superior ablation resistance.

  18. Ablation-resistant carbide Zr0.8Ti0.2C0.74B0.26 for oxidizing environments up to 3,000 °C

    PubMed Central

    Zeng, Yi; Wang, Dini; Xiong, Xiang; Zhang, Xun; Withers, Philip J.; Sun, Wei; Smith, Matthew; Bai, Mingwen; Xiao, Ping

    2017-01-01

    Ultra-high temperature ceramics are desirable for applications in the hypersonic vehicle, rockets, re-entry spacecraft and defence sectors, but few materials can currently satisfy the associated high temperature ablation requirements. Here we design and fabricate a carbide (Zr0.8Ti0.2C0.74B0.26) coating by reactive melt infiltration and pack cementation onto a C/C composite. It displays superior ablation resistance at temperatures from 2,000–3,000 °C, compared to existing ultra-high temperature ceramics (for example, a rate of material loss over 12 times better than conventional zirconium carbide at 2,500 °C). The carbide is a substitutional solid solution of Zr–Ti containing carbon vacancies that are randomly occupied by boron atoms. The sealing ability of the ceramic’s oxides, slow oxygen diffusion and a dense and gradient distribution of ceramic result in much slower loss of protective oxide layers formed during ablation than other ceramic systems, leading to the superior ablation resistance. PMID:28613275

  19. Standard methods for chemical analysis of steel, cast iron, open-hearth iron, and wrought iron

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

    None

    1973-01-01

    Methods are described for determining manganese, phosphorus, sulfur, selenium, copper, nickel, chromium, vanadium, tungsten, titanium, lead, boron, molybdenum ( alpha -benzoin oxime method), zirconium (cupferron --phosphate method), niobium and tantalum (hydrolysis with perchloric and sulfurous acids (gravimetric, titrimetric, and photometric methods)), and beryllium (oxide method). (DHM)

  20. SEPARATION OF FISSION PRODUCT VALUES FROM THE HEXAVALENT PLUTONIUM BY CARRIER PRECIPITATION

    DOEpatents

    Davies, T.H.

    1959-12-15

    An improved precipitation of fission products on bismuth phosphate from an aqueous mineral acid solution also containing hexavalent plutonium by incorporating, prior to bismuth phosphate precipitation, from 0.05 to 2.5 grams/ liter of zirconium phosphate, niobium oxide. and/or lanthanum fluoride is described. The plutonium remains in solution.

  1. Effect of nano-sized cerium-zirconium oxide solid solution on far-infrared emission properties of tourmaline powders

    NASA Astrophysics Data System (ADS)

    Guo, Bin; Yang, Liqing; Hu, Weijie; Li, Wenlong; Wang, Haojing

    2015-10-01

    Far-infrared functional nanocomposites were prepared by the co-precipitation method using natural tourmaline (XY3Z6Si6O18(BO3)3V3W, where X is Na+, Ca2+, K+, or vacancy; Y is Mg2+, Fe2+, Mn2+, Al3+, Fe3+, Mn3+, Cr3+, Li+, or Ti4+; Z is Al3+, Mg2+, Cr3+, or V3+; V is O2-, OH-; and W is O2-, OH-, or F-) powders, ammonium cerium(IV) nitrate and zirconium(IV) nitrate pentahydrate as raw materials. The reference sample, tourmaline modified with ammonium cerium(IV) nitrate alone was also prepared by a similar precipitation route. The results of Fourier transform infrared spectroscopy show that tourmaline modified with Ce and Zr has a better far-infrared emission property than tourmaline modified with Ce alone. Through characterization by transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), the mechanism for oxygen evolution during the heat process in the two composite materials was systematically studied. The XPS spectra show that Fe3+ ratio inside tourmaline modified with Ce alone can be raised by doping Zr. Moreover, it is showed that there is a higher Ce3+ ratio inside the tourmaline modified with Ce and Zr than tourmaline modified with Ce alone. In addition, XRD results indicate the formation of CeO2 and Ce1-xZrxO2 crystallites during the heat treatment and further TEM observations show they exist as nanoparticles on the surface of tourmaline powders. Based on these results, we attribute the improved far-infrared emission properties of Ce-Zr doped tourmaline to the enhanced unit cell shrinkage of the tourmaline arisen from much more oxidation of Fe2+ to Fe3+ inside the tourmaline caused by the change in the catalyst redox properties of CeO2 brought about by doping with Zr4+. In all samples, tourmaline modified with 7.14 wt.% Ce and 1.86 wt.% Zr calcined at 800∘C for 5 h has the best far-infrared emission property with the maximum emissivity value of 98%.

  2. Electrochemical response of carbon paste electrode modified with mixture of titanium dioxide/zirconium dioxide in the detection of heavy metals: lead and cadmium.

    PubMed

    Nguyen, Phuong Khanh Quoc; Lunsford, Suzanne K

    2012-11-15

    A novel carbon modified electrode was developed by incorporating titanium dioxide/zirconium dioxide into the graphite carbon paste electrode to detect heavy metals-cadmium and lead. In this work, the development of the novel titanium dioxide/zirconium dioxide modified carbon paste electrode was studied to determine the optimum synthesis conditions related to the temperature, heating duration, amount and ratio of titanium dioxide/zirconium dioxide, and amount of surfactant, to create the most reproducible results. Using cyclic voltammetric (CV) analysis, this study has proven that the novel titanium dioxide/zirconium dioxide can be utilized to detect heavy metals-lead and cadmium, at relatively low concentrations (7.6×10(-6) M and 1.1×10(-5) M for Pb and Cd, respectively) at optimum pH value (pH=3). From analyzing CV data the optimal electrodes surface area was estimated to be 0.028 (±0.003) cm(2). Also, under the specific experimental conditions, electron transfer coefficients were estimated to be 0.44 and 0.33 along with the heterogeneous electron transfer rate constants of 5.64×10(-3) and 2.42×10(-3) (cm/s) for Pb and Cd, respectively. Copyright © 2012 Elsevier B.V. All rights reserved.

  3. Selective separation of zirconium from uranium in carbonate solutions by ion flotation

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

    Jdid, E.A.; Blazy, P.; Mahamadou, A.

    1990-05-01

    Separation of zirconium from uranium in carbonate media was undertaken by ion flotation. The collector chosen was octylhydroxamic acid (HOHX). It gave a well-flocculated precipitate with zirconium which floated in less than 5 min. The stoichiometry of the reaction is HOHX/Zr = 3.9/1, and the selectivity in the presence of uranium is very high. In fact, for a ratio {Phi} = (HOHX),M/(Zr),M, which is just stoichiometric and is close to 4, the zirconium removal rate reaches 99%, even in industrial media. The loss of uranium is only 0.5% although its concentration is 37.4 g/L. Mechanisms of separation are not affectedmore » by a variation of pH between 6.7 and 9.8, of temperature up to 60{degree}C, and of carbonate concentration within the 15 to 60 g/L Na{sub 2}CO{sub 3} range.« less

  4. High-voltage SPM oxidation of ZrN: materials for multiscale applications

    NASA Astrophysics Data System (ADS)

    Farkas, N.; Comer, J. R.; Zhang, G.; Evans, E. A.; Ramsier, R. D.; Dagata, J. A.

    2005-02-01

    Scanning probe microscope (SPM) oxidation was used to form zirconium oxide features on 200 nm thick ZrN films. The features exhibit rapid yet controlled growth kinetics, even in contact mode with 70 V dc applied between the probe tip and substrate. The features grown for times longer than 10 s are higher than 200 nm, and reach more than 1000 nm in height after 300 s. Long-time oxidation experiments and selective etching of the oxides and nitrides lead us to propose that as the oxidation reaches the silicon substrate, delamination occurs with the simultaneous formation of a thin layer of new material at the ZrN/Si interface. High-voltage oxide growth on ZrN is fast and sustainable, and the robust oxide features are promising candidates for multiscale (nanometre-to-micrometre) applications.

  5. Ferrier rearrangement promoted by an electrochemically generated zirconium catalyst.

    PubMed

    Stevanović, Dragana; Pejović, Anka; Damljanović, Ivan; Minić, Aleksandra; Bogdanović, Goran A; Vukićević, Mirjana; Radulović, Niko S; Vukićević, Rastko D

    2015-04-30

    In situ generated zirconium catalyst from a sacrificial zirconium anode was successfully applied to promote Ferrier rearrangement of 3,4,5-tri-O-acetyl-D-glucal and 6-deoxy-3,4-di-O-acetyl-L-glucal (3,4-di-O-acetyl-L-rhamnal) in the presence of three thiols and eleven thiophenols as nucleophiles. A simple constant current electrolysis (20 mA, 0.4 F mol(-1)) of an acetonitrile solution of lithium perchlorate (0.1 M) containing the corresponding glycal and S-nucleophiles, using a zirconium anode and a platinum cathode resulted in the successful synthesis of the corresponding 2,3-unsaturated peracetylated thioglycosides (with an average anomer ratio α/β=4.129 in the case of peracetylated D-glucal and 8.740 in the case of L-rhamnal). The same procedure proved to be appropriate in synthesizing dihydropyran derivatives ('C-glycosides') using allyltrimethylsilane as the nucleophile (only 'α-anomers' were obtained). All new compounds were fully characterized by spectral data, whereas single-crystal X-ray analysis was performed for two thioglycosides. Copyright © 2015 Elsevier Ltd. All rights reserved.

  6. Comparison of surface modified zirconia implants with commercially available zirconium and titanium implants: a histological study in pigs.

    PubMed

    Gredes, Tomasz; Kubasiewicz-Ross, Pawel; Gedrange, Tomasz; Dominiak, Marzena; Kunert-Keil, Christiane

    2014-08-01

    New biomaterials and their various surface modifications should undergo in vitro and in vivo evaluation before clinical trials. The objective of our in vivo study was to evaluate the biocompatibility of newly created zirconium implant surfaces after implantation in the lower jaw of pigs and compare the osseointegration of these dental implants with commercially available zirconium and titanium implants. After a healing period of 12 weeks, a histological analysis of the soft and hard tissues and a histomorphometric analysis of the bone-implant contact (BIC) were performed. The implant surfaces showed an intimate connection to the adjacent bone for all tested implants. The 3 newly created zirconium implant surfaces achieved a BIC of 45% on average in comparison with a BIC of 56% from the reference zirconium implants and 35% from titanium implants. Furthermore, the new zirconium implants had a better attachment to gingival and bone tissues in the range of implant necks as compared with the reference implants. The results suggest that the new implants comparably osseointegrate within the healing period, and they have a good in vivo biocompatibility.

  7. Protective interlayer for high temperature solid electrolyte electrochemical cells

    DOEpatents

    Singh, Prabhakar; Vasilow, Theodore R.; Richards, Von L.

    1996-01-01

    The invention comprises of an electrically conducting doped or admixed cerium oxide composition with niobium oxide and/or tantalum oxide for electrochemical devices, characterized by the general formula: Nb.sub.x Ta.sub.y Ce.sub.1-x-y O.sub.2 where x is about 0.0 to 0.05, y is about 0.0 to 0.05, and x+y is about 0.02 to 0.05, and where x is preferably about 0.02 to 0.05 and y is 0, and a method of making the same. This novel composition is particularly applicable in forming a protective interlayer of a high temperature, solid electrolyte electrochemical cell (10), characterized by a first electrode (12); an electrically conductive interlayer (14) of niobium and/or tantalum doped cerium oxide deposited over at least a first portion (R) of the first electrode; an interconnect (16) deposited over the interlayer; a solid electrolyte (18) deposited over a second portion of the first electrode, the first portion being discontinuous from the second portion; and, a second electrode (20) deposited over the solid electrolyte. The interlayer (14) is characterized as being porous and selected from the group consisting of niobium doped cerium oxide, tantalum doped cerium oxide, and niobium and tantalum doped cerium oxide or admixtures of the same. The first electrode (12), an air electrode, is a porous layer of doped lanthanum manganite, the solid electrolyte layer (18) is a dense yttria stabilized zirconium oxide, the interconnect layer (16) is a dense, doped lanthanum chromite, and the second electrode (20), a fuel electrode, is a porous layer of nickel-zirconium oxide cermet. The electrochemical cell (10) can take on a plurality of shapes such as annular, planar, etc. and can be connected to a plurality of electrochemical cells in series and/or in parallel to generate electrical energy.

  8. Differences in the calcification of preosteoblast cultured on sputter-deposited titanium, zirconium, and gold.

    PubMed

    Chen, Peng; Nagai, Akiko; Tsutsumi, Yusuke; Ashida, Maki; Doi, Hisashi; Hanawa, Takao

    2016-03-01

    In this study, osteogenic differentiation and calcification of preosteoblast (MC3T3-E1) cultured on sputter-deposited titanium (Ti), zirconium (Zr), and gold (Au) on cover glasses were evaluated to understand the differences in bone formation ability among these three metals; these metals show the same high corrosion resistance, but Ti and Zr are covered by surface passive oxide film while Au is not covered by the oxide film. Ti and Zr promoted cellular proliferation without osteogenic differentiation. Cells cultured on Ti and Zr expressed higher levels of Runx2, Col1α1, and Akp2 at an earlier stage, which indicated faster promotion of osteogenic differentiation, as compared to those cultured on Au. Moreover, after 21 days of culture, the Bglap1 and Ifitm5 expression peaks in cells cultured on Ti and Zr were higher than those in cells cultured on Au, which indicated faster promotion of calcification. Cells cultured on Ti showed an advantage in osteogenic differentiation at an early stage, while cells on Zr showed better calcification promotion with a long-term culture. The amount of extracellular calcified deposits was in good agreement with the gene expression results. On the other hand, the intracellular calcium content of cells on Au specimens was higher than that of cells on Ti and Zr specimens. The results indicate that preosteoblasts on Ti and Zr showed faster osteogenic differentiation and calcification than those on Au, whereas Au improved the intracellular calcium content. © 2015 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 104A: 639-651, 2016. © 2015 Wiley Periodicals, Inc.

  9. Low temperature route to uranium nitride

    DOEpatents

    Burrell, Anthony K.; Sattelberger, Alfred P.; Yeamans, Charles; Hartmann, Thomas; Silva, G. W. Chinthaka; Cerefice, Gary; Czerwinski, Kenneth R.

    2009-09-01

    A method of preparing an actinide nitride fuel for nuclear reactors is provided. The method comprises the steps of a) providing at least one actinide oxide and optionally zirconium oxide; b) mixing the oxide with a source of hydrogen fluoride for a period of time and at a temperature sufficient to convert the oxide to a fluoride salt; c) heating the fluoride salt to remove water; d) heating the fluoride salt in a nitrogen atmosphere for a period of time and at a temperature sufficient to convert the fluorides to nitrides; and e) heating the nitrides under vacuum and/or inert atmosphere for a period of time sufficient to convert the nitrides to mononitrides.

  10. Aqueous Isolation of 17-Nuclear Zr-/Hf- Oxide Clusters during the Hydrothermal Synthesis of ZrO2/HfO2.

    PubMed

    Sung, Qing; Liu, Caiyun; Zhang, Guanyun; Zhang, Jian; Tung, Chen-Ho; Wang, Yifeng

    2018-06-21

    Novel 17-nuclear Zr-/Hf- oxide clusters ({Zr17} and {Hf17}) are isolated from aqueous systems. In the clusters, Zr/Hf ions are connected via μ3-O, μ3-OH and μ2-OH linkages into a pinwheel core which is wrapped with SO42-, HCOO- and aqua ligands. Octahedral hexanuclear Zr-/Hf- oxide clusters ({Zr6}oct and {Hf6}oct) are also isolated from the same hydrothermal system by decreasing the synthesis temperature. Structural analysis, synthetic conditions, vibrational spectra and ionic conductivity of the clusters are studied. Structural studies and synthesis inspection suggest that formation of {Zr6}oct and {Zr17} involves assembly of the same transferable building blocks, but the condensation degree and thermodynamic stability of the products increase with hydrothermal temperature. The role of {Zr6}oct and {Zr17} in the formation of ZrO2 nanocrystals are then discussed in the scenario of nonclassical nucleation theory. Besides, the Zr-oxide clusters exhibit ionic conductivity due to the mobility of protons. This study not only adds new members to the Zr-/Hf- oxide cluster family, but also establishes a connection from Zr4+ ions to ZrO2 in the hydrothermal preparation of zirconium oxide nanomaterials. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. TERNARY ALLOYS OF URANIUM, COLUMBIUM, AND ZIRCONIUM

    DOEpatents

    Foote, F.G.

    1960-08-01

    Ternary alloys of uranium are described which are useful as neutron- reflecting materials in a fast neutron reactor. They are especially resistant to corrosion caused by oxidative processes of gascous or aqueous origin and comprise uranium as the predominant metal with zirconiunn and niobium wherein the total content of the minor alloying elements is between 2 and 8% by weight.

  12. Effect of ZrB2 addition on the oxidation behavior of Si-SiC-ZrB2 composites exposed at 1500°C in air.

    PubMed

    D'Amico, Claudio; Bianchi, Giovanni; Padovano, Elisa; Biamino, Sara; Aversa, Alberta; Badini, Claudio; Ortona, Alberto

    2018-01-01

    Silicon carbide ceramics obtained by reactive infiltration of silicon (SRI) have many industrial applications especially involving severe and high temperature conditions. In this study, the oxidation behavior in air of Si-SiC-ZrB 2 systems at a high temperature (1500°C) for dwelling times of up to 48 hours was examined. The oxidation process was analyzed on the basis of elemental maps and X-ray diffraction patterns taken, respectively, on the core and on the surface of the specimens, together with weight gains and the average thicknesses of the resulting scale. Further, flexural strength at room temperature was examined as a function of different oxidation times. The main chemical reactions and phase transformations involved in the oxidation process are reported. Several oxides were detected on the surface: zirconia, silica, zircon and 3-zirconium monoxide. All of the samples showed a parabolic oxidation kinetics, suggesting that the controlling mechanism was the diffusion; however, even after 48 hours, the oxidation process was not finished - indeed, all of the samples continued to gain weight. The oxidation of Si-SiC-ZrB 2 material produced via SRI was slower compared with previously investigated ZrB 2 -SiC composites processed with a different techniques and tested in similar conditions. The oxidation mechanism was found to be consistent with the convection cells model.

  13. Conditions affecting the formation of chlorinated carbon compounds during carbochlorination

    NASA Astrophysics Data System (ADS)

    Landsberg, A.; Wilson, R. D.; Burns, W.

    1988-06-01

    The Bureau of Mines, United States Department of the Interior, has conducted an extensive study of the relationship between various metal oxide carbochlorination reactions and carbon compound byproducts. Experiments in which oxides of titanium, zirconium, and aluminum with graphite, charcoal, metallurgical coke, and pctroleum coke were chlorinated at 600° to 1000 °C produced 136 identified and quantified carbon byproduct compounds. The 20 most abundant of these compounds were correlated with reactants and reaction conditions. Experimental results support a proposed carbochlorination reaction with an initial chlorine-carbon step followed by a reaction between the resulting chlorine-carbon products and the metal oxide.

  14. Conducting metal oxide and metal nitride nanoparticles

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

    DiSalvo, Jr., Francis J.; Subban, Chinmayee V.

    Conducting metal oxide and nitride nanoparticles that can be used in fuel cell applications. The metal oxide nanoparticles are comprised of for example, titanium, niobium, tantalum, tungsten and combinations thereof. The metal nitride nanoparticles are comprised of, for example, titanium, niobium, tantalum, tungsten, zirconium, and combinations thereof. The nanoparticles can be sintered to provide conducting porous agglomerates of the nanoparticles which can be used as a catalyst support in fuel cell applications. Further, platinum nanoparticles, for example, can be deposited on the agglomerates to provide a material that can be used as both an anode and a cathode catalyst supportmore » in a fuel cell.« less

  15. Non-noble metal based electro-catalyst compositions for proton exchange membrane based water electrolysis and methods of making

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

    Kumta, Prashant N.; Kadakia, Karan Sandeep; Datta, Moni Kanchan

    The invention provides electro-catalyst compositions for an anode electrode of a proton exchange membrane-based water electrolysis system. The compositions include a noble metal component selected from the group consisting of iridium oxide, ruthenium oxide, rhenium oxide and mixtures thereof, and a non-noble metal component selected from the group consisting of tantalum oxide, tin oxide, niobium oxide, titanium oxide, tungsten oxide, molybdenum oxide, yttrium oxide, scandium oxide, cooper oxide, zirconium oxide, nickel oxide and mixtures thereof. Further, the non-noble metal component can include a dopant. The dopant can be at least one element selected from Groups III, V, VI and VIImore » of the Periodic Table. The compositions can be prepared using a surfactant approach or a sol gel approach. Further, the compositions are prepared using noble metal and non-noble metal precursors. Furthermore, a thin film containing the compositions can be deposited onto a substrate to form the anode electrode.« less

  16. Supported metallocene catalysts by surface organometallic chemistry. Synthesis, characterization, and reactivity in ethylene polymerization of oxide-supported mono- and biscyclopentadienyl zirconium alkyl complexes: establishment of structure/reactivity relationships.

    PubMed

    Jezequel, M; Dufaud, V; Ruiz-Garcia, M J; Carrillo-Hermosilla, F; Neugebauer, U; Niccolai, G P; Lefebvre, F; Bayard, F; Corker, J; Fiddy, S; Evans, J; Broyer, J P; Malinge, J; Basset, J M

    2001-04-18

    The reactions of CpZr(CH(3))(3), 1, and Cp(2)Zr(CH(3))(2), 2, with partially dehydroxylated silica, silica-alumina, and alumina surfaces have been carried out with careful identification of the resulting surface organometallic complexes in order to probe the relationship between catalyst structure and polymerization activity. The characterization of the supported complexes has been achieved in most cases by in situ infrared spectroscopy, surface microanalysis, qualitative and quantitative analysis of evolved gases during surface reactions with labeled surface, solid state (1)H and (13)C NMR using (13)C-enriched compounds, and EXAFS. 1 and 2 react with silica(500) and silica-alumina(500) by simple protonolysis of one Zr-Me bond by surface silanols with formation of a single well-defined neutral compound. In the case of silica-alumina, a fraction of the supported complexes exhibits some interactions with electronically unsaturated surface aluminum sites. 1 and 2 also react with the hydroxyl groups of gamma-alumina(500), leading to several surface structures. Correlation between EXAFS and (13)C NMR data suggests, in short, two main surface structures having different environments for the methyl group: [Al](3)-OZrCp(CH(3))(2) and [Al](2)-OZrCp(CH(3))(mu-CH(3))-[Al] for the monoCp series and [Al](2)-OZrCp(2)(CH(3)) and [Al]-OZrCp(2)(mu-CH(3))-[Al] for the bisCp series. Ethylene polymerization has been carried out with all the supported complexes under various reaction conditions. Silica-supported catalysts in the absence of any cocatalyst exhibited no activity whatsoever for ethylene polymerization. When the oxide contained Lewis acidic sites, the resulting surface species were active. The activity, although improved by the presence of additional cocatalysts, remained very low by comparison with that of the homogeneous metallocene systems. This trend has been interpreted on the basis of various possible parameters, including the (p-pi)-(d-pi) back-donation of surface oxygen atoms to the zirconium center.

  17. Superior removal of arsenic from water with zirconium metal-organic framework UiO-66.

    PubMed

    Wang, Chenghong; Liu, Xinlei; Chen, J Paul; Li, Kang

    2015-11-12

    In this study, water stable zirconium metal-organic framework (UiO-66) has been synthesized and for the first time applied as an adsorbent to remove aquatic arsenic contamination. The as-synthesized UiO-66 adsorbent functions excellently across a broad pH range of 1 to 10, and achieves a remarkable arsenate uptake capacity of 303 mg/g at the optimal pH, i.e., pH = 2. To the best of our knowledge, this is the highest arsenate As(V) adsorption capacity ever reported, much higher than that of currently available adsorbents (5-280 mg/g, generally less than 100 mg/g). The superior arsenic uptake performance of UiO-66 adsorbent could be attributed to the highly porous crystalline structure containing zirconium oxide clusters, which provides a large contact area and plenty of active sites in unit space. Two binding sites within the adsorbent framework are proposed for arsenic species, i.e., hydroxyl group and benzenedicarboxylate ligand. At equilibrium, seven equivalent arsenic species can be captured by one Zr6 cluster through the formation of Zr-O-As coordination bonds.

  18. Superior removal of arsenic from water with zirconium metal-organic framework UiO-66

    PubMed Central

    Wang, Chenghong; Liu, Xinlei; Chen, J. Paul; Li, Kang

    2015-01-01

    In this study, water stable zirconium metal-organic framework (UiO-66) has been synthesized and for the first time applied as an adsorbent to remove aquatic arsenic contamination. The as-synthesized UiO-66 adsorbent functions excellently across a broad pH range of 1 to 10, and achieves a remarkable arsenate uptake capacity of 303 mg/g at the optimal pH, i.e., pH = 2. To the best of our knowledge, this is the highest arsenate As(V) adsorption capacity ever reported, much higher than that of currently available adsorbents (5–280 mg/g, generally less than 100 mg/g). The superior arsenic uptake performance of UiO-66 adsorbent could be attributed to the highly porous crystalline structure containing zirconium oxide clusters, which provides a large contact area and plenty of active sites in unit space. Two binding sites within the adsorbent framework are proposed for arsenic species, i.e., hydroxyl group and benzenedicarboxylate ligand. At equilibrium, seven equivalent arsenic species can be captured by one Zr6 cluster through the formation of Zr-O-As coordination bonds. PMID:26559001

  19. The Effect of Boron and Zirconium on the Structure and Tensile Properties of the Cast Nickel-Based Superalloy ATI 718Plus

    NASA Astrophysics Data System (ADS)

    Hosseini, Seyed Ali; Abbasi, Seyed Mehdi; Madar, Karim Zangeneh

    2018-04-01

    The effects of boron and zirconium on cast structure, hardness, and tensile properties of the nickel-based superalloy 718Plus were investigated. For this purpose, five alloys with different contents of boron and zirconium were cast via vacuum induction melting and then purified via vacuum arc remelting. Microstructural analysis by light-optical microscope and scanning electron microscope equipped with energy-dispersive x-ray spectroscopy and phase studies by x-ray diffraction analysis were performed. The results showed that boron and zirconium tend to significantly reduce dendritic arm spacing and increase the amount of Laves, Laves/gamma eutectic, and carbide phases. It was also found that boron led to the formation of B4C and (Cr, Fe, Mo, Ni, Ti)3B2 phases and zirconium led to the formation of intermetallic phases and ZrC carbide. In the presence of boron and zirconium, the hardness and its difference between dendritic branches and inter-dendritic spaces increased by concentrating such phases as Laves in the inter-dendritic spaces. These elements had a negative effect on tensile properties of the alloy, including ductility and strength, mainly because of the increase in the Laves phase. It should be noted that the largest degradation of the tensile properties occurred in the alloys containing the maximum amount of zirconium.

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

    Beavin, P. Jr.

    A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also addedmore » to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average percent recoveries and standard deviations for spiked samples were 99.8-100.2 and 1.69-2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8-97.4 and 3.09-4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average perent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action.« less

  1. Spectroscopic, thermal, quantum chemical calculations and in vitro biological studies of titanium/zirconium(IV) complexes of mono-and disubstituted aryldithiocarbonates

    NASA Astrophysics Data System (ADS)

    Andotra, Savit; Kumar, Sandeep; Kour, Mandeep; Kalgotra, Nidhi; Vikas; Chayawan; Pandey, Sushil K.

    2018-03-01

    Aryldithiocarbonates of titanium(IV) and zirconium(IV) corresponding to [(ROCS2)2MCl2] (R = o-, m- or p-CH3C6H4 and 4-Cl-3-CH3C6H3; M = Ti or Zr) have been isolated by the reaction of sodium salt of dithiocarbonates with titanium or zirconium tetrachloride in 1:2 M ratio in CHCl3. Donor stabilized addition complexes of titanium/zirconium with aryldithiocarbonates were also successfully isolated in chloroform. These have been characterized by elemental analyses, IR, mass, TGA/DTA, SEM and heteronuclear NMR (1H, 13C and 31P) spectroscopic studies. The antimicrobial test of these complexes has also been conducted against the bacteria Klebsiella pneumonia and Enterococcus faciolus and fungus Fusarium oxysporium, which indicate potential antimicrobial activity. In addition, the antioxidant activities of the complexes were also investigated through their scavenging effect on DPPH radicals. Density Functional Theory (DFT) calculations have been carried out to investigate geometry parameters of the complexes using B3LYP method and LANL2DZ basis set. HOMO (Highest Occupied Molecular Orbital), LUMO (Lowest Unoccupied Molecular Orbital) energies are analyzed. Based on analytical and theoretical results, a hexacoordinate geometry is concluded around the Ti or Zr atom.

  2. All-alkoxide synthesis of strontium-containing metal oxides

    DOEpatents

    Boyle, Timothy J.

    2001-01-01

    A method for making strontium-containing metal-oxide ceramic thin films from a precursor liquid by mixing a strontium neo-pentoxide dissolved in an amine solvent and at least one metal alkoxide dissolved in a solvent, said at least one metal alkoxide selected from the group consisting of alkoxides of calcium, barium, bismuth, cadmium, lead, titanium, tantalum, hafnium, tungsten, niobium, zirconium, yttrium, lanthanum, antimony, chromium and thallium, depositing a thin film of the precursor liquid on a substrate, and heating the thin film in the presence of oxygen at between 550 and 700.degree. C.

  3. In situ DRIFTS investigation of NH3-SCR reaction over CeO2/zirconium phosphate catalyst

    NASA Astrophysics Data System (ADS)

    Zhang, Qiulin; Fan, Jie; Ning, Ping; Song, Zhongxian; Liu, Xin; Wang, Lanying; Wang, Jing; Wang, Huimin; Long, Kaixian

    2018-03-01

    A series of ceria modified zirconium phosphate catalysts were synthesized for selective catalytic reduction of NO with ammonia (NH3-SCR). Over 98% NOx conversion and 98% N2 selectivity were obtained by the CeO2/ZrP catalyst with 20 wt.% CeO2 loading at 250-425 °C. The interaction between CeO2 and zirconium phosphate enhanced the redox abilities and surface acidities of the catalysts, resulting in the improvement of NH3-SCR activity. The in situ DRIFTS results indicated that the NH3-SCR reaction over the catalysts followed both Eley-Rideal and Langmuir-Hinshelwood mechanisms. The amide (sbnd NH2) groups and the NH4+ bonded to Brønsted acid sites were the important intermediates of Eley-Rideal mechanism.

  4. The effect of environmental factors on selected mechanical properties of zirconium dioxide

    NASA Astrophysics Data System (ADS)

    Wirwicki, W.; Andrzejewska, A.; Andryszczyk, M.; Siemianowski, P.

    2018-04-01

    In many centers around the world, research studies are carried out on the mechanical strength of dental materials and glued joints. A literature review shows the variety of testing techniques related to analyzing the strength and durability of the material itself and the glued joints. In dental ceramics, zirconium dioxide is most often used as a base material, and chemically it consists of 97% ZrO2 and 3% Y2O3. This study was to determine the mechanical properties of zirconium dioxide under different environmental conditions. The material is used for the production of dental crowns and tooth bridges in the CAD/CAM technology. This medium is currently one of the most advanced-generation materials used for prosthetic and implant restorations. They were then subjected to a three-point bending test on the Instron ElektroPlus E3000 durability machine. Storage conditions and time have a positive influence on reducing variation in zirconium resistance for active forces and destructive stresses.

  5. Silicon doped hafnium oxide (HSO) and hafnium zirconium oxide (HZO) based FeFET: A material relation to device physics

    NASA Astrophysics Data System (ADS)

    Ali, T.; Polakowski, P.; Riedel, S.; Büttner, T.; Kämpfe, T.; Rudolph, M.; Pätzold, B.; Seidel, K.; Löhr, D.; Hoffmann, R.; Czernohorsky, M.; Kühnel, K.; Thrun, X.; Hanisch, N.; Steinke, P.; Calvo, J.; Müller, J.

    2018-05-01

    The recent discovery of ferroelectricity in thin film HfO2 materials renewed the interest in ferroelectric FET (FeFET) as an emerging nonvolatile memory providing a potential high speed and low power Flash alternative. Here, we report more insight into FeFET performance by integrating two types of ferroelectric (FE) materials and varying their properties. By varying the material type [HfO2 (HSO) versus hafnium zirconium oxide (HZO)], optimum content (Si doping/mixture ratio), and film thickness, a material relation to FeFET device physics is concluded. As for the material type, an improved FeFET performance is observed for HZO integration with memory window (MW) comparable to theoretical values. For different Si contents, the HSO based FeFET exhibited a MW trend with different stabilized phases. Similarly, the HZO FeFET shows MW dependence on the Hf:Zr mixture ratio. A maximized MW is obtained with cycle ratios of 16:1 (HfO2:Si) and 1:1 (Hf:Zr) as measured on HSO and HZO based FeFETs, respectively. The thickness variation shows a trend of increasing MW with the increased FE layer thickness confirming early theoretical predictions. The FeFET material aspects and stack physics are discussed with insight into the interplay factors, while optimum FE material parameters are outlined in relation to performance.

  6. An investigation of the oxidation behaviour of zirconium alloys using isotopic tracers and high resolution SIMS

    NASA Astrophysics Data System (ADS)

    Yardley, Sean S.; Moore, Katie L.; Ni, Na; Wei, Jang Fei; Lyon, Stuart; Preuss, Michael; Lozano-Perez, Sergio; Grovenor, Chris R. M.

    2013-11-01

    High resolution secondary ion mass spectrometry (SIMS) analysis has been used to study the oxidation mechanisms when commercial low tin ZIRLO™Low tin ZIRLO™ is a trademark of Westinghouse Electric Company LLC in the United States and may be registered in other countries throughout the world. Unauthorized use is strictly prohibited.1 and Zircaloy 4 materials are exposed to corroding environments containing both 18O and 2H isotopes. Clear evidence has been shown for different characteristic distributions of 18O before and after the kinetic transitions, and this behaviour has been correlated with the development of porosity in the oxide which allows the corroding medium to penetrate locally to the metal/oxide interface.

  7. Artefacts in multimodal imaging of titanium, zirconium and binary titanium–zirconium alloy dental implants: an in vitro study

    PubMed Central

    Schöllchen, Maximilian; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

    2017-01-01

    Objectives: To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium–zirconium alloy dental implants. Methods: Zirconium, titanium and titanium–zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line–distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. Results: While titanium and titanium–zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium–zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium–zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium–zirconium alloy induced more severe artefacts than zirconium and titanium. Conclusions: MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium–zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting. PMID:27910719

  8. Artefacts in multimodal imaging of titanium, zirconium and binary titanium-zirconium alloy dental implants: an in vitro study.

    PubMed

    Smeets, Ralf; Schöllchen, Maximilian; Gauer, Tobias; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

    2017-02-01

    To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium-zirconium alloy dental implants. Zirconium, titanium and titanium-zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line-distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. While titanium and titanium-zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium-zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium-zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium-zirconium alloy induced more severe artefacts than zirconium and titanium. MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium-zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting.

  9. Crystal Orientation-Dependent Reactivity of Oxide Surfaces in Contact with Lithium Metal.

    PubMed

    Connell, Justin G; Zhu, Yisi; Zapol, Peter; Tepavcevic, Sanja; Sharafi, Asma; Sakamoto, Jeff; Curtiss, Larry A; Fong, Dillon D; Freeland, John W; Markovic, Nenad M

    2018-05-23

    Understanding ionic transport across interfaces between dissimilar materials and the intrinsic chemical stability of such interfaces is a fundamental challenge spanning many disciplines and is of particular importance for designing conductive and stable solid electrolytes for solid-state Li-ion batteries. In this work, we establish a surface science-based approach for assessing the intrinsic stability of oxide materials in contact with Li metal. Through a combination of experimental and computational insights, using Nb-doped SrTiO 3 (Nb/STO) single crystals as a model system, we were able to understand the impact of crystallographic orientation and surface morphology on the extent of the chemical reactions that take place between surface Nb, Ti, and Sr upon reaction with Li. By expanding our approach to investigate the intrinsic stability of the technologically relevant, polycrystalline Nb-doped lithium lanthanum zirconium oxide (Li 6.5 La 3 Zr 1.5 Nb 0.5 O 12 ) system, we found that this material reacts with Li metal through the reduction of Nb, similar to that observed for Nb/STO. These results clearly demonstrate the feasibility of our approach to assess the intrinsic (in)stability of oxide materials for solid-state batteries and point to new strategies for understanding the performance of such systems.

  10. Crystal Orientation-Dependent Reactivity of Oxide Surfaces in Contact with Lithium Metal.

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

    Connell, Justin G.; Zhu, Yisi; Zapol, Peter

    Understanding ionic transport across interfaces between dissimilar materials and the intrinsic chemical stability of such interfaces is a fundamental challenge spanning many disciplines and is of particular importance for designing conductive and stable solid electrolytes for solid-state Li-ion batteries. In this work, we establish a surface science-based approach for assessing the intrinsic stability of oxide materials in contact with Li metal. Through a combination of experimental and computational insights, using Nb-doped SrTiO3 (Nb/STO) single crystals as a model system, we were able to understand the impact of crystallographic orientation and surface morphology on the extent of the chemical reactions thatmore » take place between surface Nb, Ti, and Sr upon reaction with Li. By expanding our approach to investigate the intrinsic stability of the technologically relevant, polycrystalline Nb-doped lithium lanthanum zirconium oxide (Li6.5La3Zr1.5Nb0.5O12) system, we found that this material reacts with Li metal through the reduction of Nb, similar to that observed for Nb/STO. These results clearly demonstrate the feasibility of our approach to assess the intrinsic (in)stability of oxide materials for solid-state batteries and point to new strategies for understanding the performance of such systems.« less

  11. Internal stresses at the crystalline scale in textured ZrO2 films before lateral cracking

    NASA Astrophysics Data System (ADS)

    Berdin, Clotilde; Pascal, Serge; Tang, Yan

    2015-05-01

    Zirconium oxide layers are submitted to internal stresses that play a role in damage of the layer. Lateral cracking is often observed during Zr alloys oxidation. In this paper, we investigated the influence of the microstresses at the crystalline scale on the lateral cracking within a growing oxide on a plane substrate. A parametric study was carried out taking into account the crystallographic texture of the oxide and the presence of a tetragonal zirconia at the metal-oxide interface. Macroscopic computations and polycrystalline aggregate computations were performed. The result indicating the (1 0 6 bar) fiber texture as the most favorable was recovered. It was found that under macroscopic compressive stresses parallel to the plane metal-oxide interface, positive microstresses perpendicular to the interface develops. They can trigger the lateral cracking and the phenomenon is promoted by the presence of tetragonal zirconia at the metal-oxide interface.

  12. Formation of heterobimetallic zirconium/cobalt diimido complexes via a four-electron transformation.

    PubMed

    Wu, Bing; Hernández Sánchez, Raúl; Bezpalko, Mark W; Foxman, Bruce M; Thomas, Christine M

    2014-10-06

    The reactivity of the reduced heterobimetallic complex Zr((i)PrNP(i)Pr2)3CoN2 (1) toward aryl azides was examined, revealing a four-electron redox transformation to afford unusual heterobimetallic zirconium/cobalt diimido complexes. In the case of p-tolyl azide, the diamagnetic C3-symmetric bis(terminal imido) complex 3 is formed, but mesityl azide instead leads to asymmetric complex 4 featuring a bridging imido fragment.

  13. Distribution coefficients of rare earth ions in cubic zirconium dioxide

    NASA Astrophysics Data System (ADS)

    Romer, H.; Luther, K.-D.; Assmus, W.

    1994-08-01

    Cubic zirconium dioxide crystals are grown with the skull melting technique. The effective distribution coefficients for Nd(exp 3+), Sm(exp 3+) and Er(sup 3+) as dopants are determined experimentally as a function of the crystal growth velocity. With the Burton-Prim-Slichter theory, the equilibrium distribution coefficients can be calculated. The distribution coefficients of all other trivalent rare earth ions can be estimated by applying the correlation towards the ionic radii.

  14. 76 FR 17715 - Virginia Electric and Power Company North Anna Power Station, Units 1 and 2; Exemption

    Federal Register 2010, 2011, 2012, 2013, 2014

    2011-03-30

    ... oxidation from the metal/water reaction to be calculated using the Baker-Just equation (Baker, L., Just, L.C., ``Studies of Metal Water Reactions at High Temperatures, III. Experimental and Theoretical Studies of the Zirconium-Water Reaction,'' ANL-6548, page 7, May 1962). Both of the above requirements require the use of...

  15. Spectrophotometric determination of fluorine in silicate rocks

    USGS Publications Warehouse

    Peck, L.C.; Smith, V.C.

    1964-01-01

    The rock powder is sintered with a sodium carbonate flux containing zinc oxide and magnesium carbonate, the sinter-cake leached with water and the resulting solution filtered. Fluorine is separated from the acidified filtrate by steam distillation and determined spectrophotometrically by means of a zirconium-SPADNS reagent. If a multiple-unit distillation apparatus is used, 12 determinations can be completed per man-day. ?? 1964.

  16. Dynamic hyperfiltration membranes for high-temperature spacecraft wash water recycle

    NASA Technical Reports Server (NTRS)

    Gaddis, J. L.; Brandon, C. A.

    1978-01-01

    The effect of operating parameters on the performance of the hyperfiltration membrane when operating on washwater was examined. The parameters were pressure, temperature, velocity, and concentration. Data taken included rejections of organic materials, ammonia, urea, and an assortment of ions. The membrane used was a dual layer, polyacrylic acid over zirconium oxide, deposited in situ on a porcelain ceramic substrate.

  17. PRECIPITATION OF ZIRCONIUM, NIOBIUM, AND RUTHENIUM FROM AQUEOUS SOLUTIONS

    DOEpatents

    Wilson, A.S.

    1958-08-12

    An improvement on the"head end process" for decontaminating dissolver solutions of their Zr, Ni. and Ru values. The process consists in adding a water soluble symmetrical dialkyl ketone. e.g. acetone, before the formation of the manganese dioxide precipitate. The effect is that upon digestion, the ruthenium oxide does not volatilize, but is carried on the manganese dioxide precipitate.

  18. Resistive switching mechanism of Ag/ZrO2:Cu/Pt memory cell

    NASA Astrophysics Data System (ADS)

    Long, Shibing; Liu, Qi; Lv, Hangbing; Li, Yingtao; Wang, Yan; Zhang, Sen; Lian, Wentai; Zhang, Kangwei; Wang, Ming; Xie, Hongwei; Liu, Ming

    2011-03-01

    Resistive switching mechanism of zirconium oxide-based resistive random access memory (RRAM) devices composed of Cu-doped ZrO2 film sandwiched between an oxidizable electrode and an inert electrode was investigated. The Ag/ZrO2:Cu/Pt RRAM devices with crosspoint structure fabricated by e-beam evaporation and e-beam lithography show reproducible bipolar resistive switching. The linear I- V relationship of low resistance state (LRS) and the dependence of LRS resistance ( R ON) and reset current ( I reset) on the set current compliance ( I comp) indicate that the observed resistive switching characteristics of the Ag/ZrO2:Cu/Pt device should be ascribed to the formation and annihilation of localized conductive filaments (CFs). The physical origin of CF was further analyzed by transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS). CFs were directly observed by cross-sectional TEM. According to EDS and elemental mapping analysis, the main chemical composition of CF is determined by Ag atoms, coming from the Ag top electrode. On the basis of these experiments, we propose that the set and reset process of the device stem from the electrochemical reactions in the zirconium oxide under different external electrical stimuli.

  19. A comparative study of the mechanical behaviour of thermally oxidised commercially pure titanium and zirconium.

    PubMed

    Alansari, A; Sun, Y

    2017-10-01

    The objective of this study is to compare the mechanical behaviour of thermally oxidised commercially pure titanium (CP-Ti) and commercially pure zirconium (CP-Zr). For this purpose, these two bio-metals were thermally oxidised under the same condition (650°C for 6h) and the oxidised specimens were characterised using various analytical and experimental techniques, including oxygen uptake analysis, layer thickness and hardness measurements, scratch tests, dry sliding friction and wear tests and tribocorrosion tests in Ringer's solution. The results show that under the present thermal oxidation condition, 4 times more oxygen is introduced into CP-Zr than into CP-Ti and the oxide layer produced on CP-Zr is nearly 6 times thicker than that on CP-Ti. Thermally oxidised CP-Zr possesses a higher hardness, a deeper hardening depth and better scratch resistance than thermally oxidised CP-Ti. Under dry sliding and tribocorrosion conditions, thermally oxidised CP-Zr also possesses much better resistance to material removal and a higher load bearing capacity than thermally oxidised CP-Ti. Thus, thermally oxidised Zr possesses much better mechanical behaviour than thermally oxidised Ti. Copyright © 2017 Elsevier Ltd. All rights reserved.

  20. Alkali-resistant low-temperature atomic-layer-deposited oxides for optical fiber sensor overlays

    NASA Astrophysics Data System (ADS)

    Kosiel, K.; Dominik, M.; Ściślewska, I.; Kalisz, M.; Guziewicz, M.; Gołaszewska, K.; Niedziółka-Jonsson, J.; Bock, W. J.; Śmietana, M.

    2018-04-01

    This paper presents an investigation of properties of selected metallic oxides deposited at a low temperature (100 °C) by atomic layer deposition (ALD) technique, relating to their applicability as thin overlays for optical fiber sensors resistant in alkaline environments. Hafnium oxide (Hf x O y with y/x approx. 2.70), tantalum oxide (Ta x O y with y/x approx. 2.75) and zirconium oxide (Zr x O y with y/x approx. 2.07), which deposition was based, respectively, on tetrakis(ethylmethyl)hafnium, tantalum pentachloride and tetrakis(ethylmethyl)zirconium with deionized water, were tested as thin layers on planar Si (100) and glass substrates. Growth per cycle (GPC) in the ALD processes was 0.133-0.150 nm/cycle. Run-to-run GPC reproducibility of the ALD processes was best for Hf x O y (0.145 ± 0.001 nm/cycle) and the poorest for Ta x O y (0.133 ± 0.003 nm/cycle). Refractive indices n of the layers were 2.00-2.10 (at the wavelength λ = 632 nm), with negligible k value (at λ for 240-930 nm). The oxides examined by x-ray diffractometry proved to be amorphous, with only small addition of crystalline phases for the Zr x O y . The surfaces of the oxides had grainy but smooth topographies with root-mean square roughness ˜0.5 nm (at 10 × 10 μm2 area) according to atomic force microscopy. Ellipsometric measurements, by contrast, suggest rougher surfaces for the Zr x O y layers. The surfaces were also slightly rougher on the glass-based samples than on the Si-based ones. Nanohardness and Young modules were 4.90-8.64 GPa and 83.7-104.4 GPa, respectively. The tests of scratch resistance revealed better tribological properties for the Hf x O y and the Ta x O y than for the Zr x O y . The surfaces were hydrophilic, with wetting angles of 52.5°-62.9°. The planar oxides on Si, being resistive even to concentrated alkali (pH 14), proved to be significantly more alkali-resistive than Al2O3. The Ta x O y overlay was deposited on long-period grating sensor induced in optical fiber. Thanks to such an overlay the sensor proved to be long-lasting resistant when exposed to alkaline environment with a pH 9. Thereby, it also proved that it has a potential to be repeatedly reused as a regenerable optical fiber biosensor.

  1. Physicochemical and mechanical properties of zirconium oxide and niobium oxide modified Portland cement-based experimental endodontic sealers.

    PubMed

    Viapiana, R; Flumignan, D L; Guerreiro-Tanomaru, J M; Camilleri, J; Tanomaru-Filho, M

    2014-05-01

    To evaluate the physicochemical and mechanical properties of Portland cement-based experimental sealers (ES) with different radiopacifying agents (zirconium oxide and niobium oxide micro- and nanoparticles) in comparison with the following conventional sealers: AH Plus, MTA Fillapex and Sealapex. The materials were tested for setting time, compressive strength, flow, film thickness, radiopacity, solubility, dimensional stability and formaldehyde release. Data were subjected to anova and Tukey tests (P < 0.05). MTA Fillapex had the shortest setting time and lowest compressive strength values (P < 0.05) compared with the other materials. The ES had flow values similar to the conventional materials, but higher film thickness (P < 0.05) and lower radiopacity (P < 0.05). Similarly to AH Plus, the ES were associated with dimensional expansion (P > 0.05) and lower solubility when compared with MTA Fillapex and Sealapex (P < 0.05). None of the endodontic sealers evaluated released formaldehyde after mixing. With the exception of radiopacity, the Portland cement-based experimental endodontic sealers presented physicochemical properties according to the specifications no 57 ANSI/ADA (ADA Professional Product Review, 2008) and ISO 6876 (Dentistry - Root Canal Sealing Materials, 2012, British Standards Institution, London, UK). The sealers had setting times and flow ability that was adequate for clinical use, satisfactory compressive strength and low solubility. Additional studies should be carried out with the purpose of decreasing the film thickness and to determine the ideal ratio of radiopacifying agents in Portland cement-based root canal sealers. © 2013 International Endodontic Journal. Published by John Wiley & Sons Ltd.

  2. Articulation of Native Cartilage Against Different Femoral Component Materials. Oxidized Zirconium Damages Cartilage Less Than Cobalt-Chrome.

    PubMed

    Vanlommel, Jan; De Corte, Ronny; Luyckx, Jean Philippe; Anderson, Melissa; Labey, Luc; Bellemans, Johan

    2017-01-01

    Oxidized zirconium (OxZr) is produced by thermally driven oxidization creating an oxidized surface with the properties of a ceramic at the top of the Zr metal substrate. OxZr is much harder and has a lower coefficient of friction than cobalt-chrome (CoCr), both leading to better wear characteristics. We evaluated and compared damage to the cartilage of porcine patella plugs, articulating against OxZr vs CoCr. Our hypothesis was that, owing to its better wear properties, OxZr would damage cartilage less than CoCr. If this is true, OxZr might be a better material for the femoral component during total knee arthroplasty if the patella is not resurfaced. Twenty-one plugs from porcine patellae were prepared and tested in a reciprocating pin-on-disk machine while lubricated with bovine serum and under a constant load. Three different configurations were tested: cartilage-cartilage as the control group, cartilage-OxZr, and cartilage-CoCr. Macroscopic appearance, cartilage thickness, and the modified Mankin score were evaluated after 400,000 wear cycles. The control group showed statistically significant less damage than plugs articulating against both other materials. Cartilage plugs articulating against OxZr were statistically significantly less damaged than those articulating against CoCr. Although replacing cartilage by an implant always leads to deterioration of the cartilage counterface, OxZr results in less damage than CoCr. The use of OxZr might thus be preferable to CoCr in case of total knee arthroplasty without patella resurfacing. Copyright © 2016 Elsevier Inc. All rights reserved.

  3. Human biokinetic data and a new compartmental model of zirconium--a tracer study with enriched stable isotopes.

    PubMed

    Greiter, Matthias B; Giussani, Augusto; Höllriegl, Vera; Li, Wei Bo; Oeh, Uwe

    2011-09-01

    Biokinetic models describing the uptake, distribution and excretion of trace elements are an essential tool in nutrition, toxicology, or internal dosimetry of radionuclides. Zirconium, especially its radioisotope (95)Zr, is relevant to radiation protection due to its production in uranium fission and neutron activation of nuclear fuel cladding material. We present a comprehensive set of human data from a tracer study with stable isotopes of zirconium. The data are used to refine a biokinetic model of zirconium. Six female and seven male healthy adult volunteers participated in the study. It includes 16 complete double tracer investigations with oral ingestion and intravenous injection, and seven supplemental investigations. Tracer concentrations were measured in blood plasma and urine collected up to 100 d after tracer administration. The four data sets (two chemical tracer forms in plasma and urine) each encompass 105-240 measured concentration values above detection limits. Total fractional absorption of ingested zirconium was found to be 0.001 for zirconium in citrate-buffered drinking solution and 0.007 for zirconium oxalate solution. Biokinetic models were developed based on the linear first-order kinetic compartmental model approach used by the International Commission on Radiological Protection (ICRP). The main differences of the optimized systemic model of zirconium to the current ICRP model are (1) recycling into the transfer compartment made necessary by the observed tracer clearance from plasma, (2) different parameters related to fractional absorption for each form of the ingested tracer, and (3) a physiologically based excretion pathway to urine. The study considerably expands the knowledge on the biokinetics of zirconium, which was until now dominated by data from animal studies. The proposed systemic model improves the existing ICRP model, yet is based on the same principles and fits well into the ICRP radiation protection approach. Copyright © 2011 Elsevier B.V. All rights reserved.

  4. Piezoelectric and Electrostrictive Materials for Transducer Applications. Volume 3.

    DTIC Science & Technology

    1988-03-01

    the preparation and characterization of these required compositions. High-purity lead acetate, titanium isopropoxide , and zirconium n-propoxide were...method was similar to the procedure used in Reference 4 to prepare PbTiO 3. High-purity lead acetate [Pb(C2 H3 0 2 )2 -3H-2Oj, titanium isopropoxide [Ti(OC...dielectric constant as shown in Figure 14(A). P.𔃿 8 IV. CONCLUSION High-purity lead acetate, titanium isopropoxide and zirconium n-propoxide were used as

  5. ZIRCONIUM PHOSPHATE ADSORPTION METHOD

    DOEpatents

    Russell, E.R.; Adamson, A.S.; Schubert, J.; Boyd, G.E.

    1958-11-01

    A method is presented for separating plutonium values from fission product values in aqueous acidic solution. This is accomplished by flowing the solutlon containing such values through a bed of zirconium orthophosphate. Any fission products adsorbed can subsequently be eluted by washing the column with a solution of 2N HNO/sub 3/ and O.lN H/sub 3/PO/sub 4/. Plutonium values may subsequently be desorbed by contacting the column with a solution of 7N HNO/sub 3/ .

  6. High-temperature electrically conductive ceramic composite and method for making same

    DOEpatents

    Beck, David E.; Gooch, Jack G.; Holcombe, Jr., Cressie E.; Masters, David R.

    1983-01-01

    The present invention relates to a metal-oxide ceramic composition useful in induction heating applications for treating uranium and uranium alloys. The ceramic composition is electrically conductive at room temperature and is nonreactive with molten uranium. The composition is prepared from a particulate admixture of 20 to 50 vol. % niobium and zirconium oxide which may be stabilized with an addition of a further oxide such as magnesium oxide, calcium oxide, or yttria. The composition is prepared by blending the powders, pressing or casting the blend into the desired product configuration, and then sintering the casting or compact in an inert atmosphere. In the casting operation, calcium aluminate is preferably added to the admixture in place of a like quantity of zirconia for providing a cement to help maintain the integrity of the sintered product.

  7. Possible origin and roles of nano-porosity in ZrO2 scales for hydrogen pick-up in Zr alloys

    NASA Astrophysics Data System (ADS)

    Lindgren, Mikaela; Geers, Christine; Panas, Itai

    2017-08-01

    A mechanistic understanding of Wagnerian build-up and subsequent non-Wagnerian break-down of barrier oxide upon oxidation of zirconium alloys by water is reiterated. Hydrogen assisted build-up of nano-porosity is addressed. Growth of sub-nanometer wide stalactitic pores owing to increasing aggregation of neutral oxygen vacancies offering a means to permeate hydrogen into the alloy is explored by density functional theory. The Wagnerian channel utilizes charge separation allowing charged oxygen vacancies and electrons to move separately from nominal anode to nominal cathode. This process becomes increasingly controlled by the charging of the barrier oxide resulting in sub-parabolic rate law for oxide growth. The break-down of the barrier oxide is understood to be preceded by avalanching hydrogen pick-up in the alloy. Pore mediated diffusion allows water to effectively short circuit the barrier oxide.

  8. 40 CFR 421.333 - Effluent limitations guidelines representing the degree of effluent reduction attainable by the...

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 2.387 1.108 Nickel 4.688 3.154 Ammonia (as N) 1,136.000 499.500 (d) SiCl4 purification wet air....674 5.835 Ammonia (as N) 2,102.000 895.000 (q) Leaching rinse water from zirconium metal production... Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy production. BAT...

  9. 40 CFR 421.333 - Effluent limitations guidelines representing the degree of effluent reduction attainable by the...

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 2.387 1.108 Nickel 4.688 3.154 Ammonia (as N) 1,136.000 499.500 (d) SiCl4 purification wet air....674 5.835 Ammonia (as N) 2,102.000 895.000 (q) Leaching rinse water from zirconium metal production... Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy production. BAT...

  10. Divergent Pathways Involving 1,3-Dipolar Addition and N-N Bond Splitting of an Organic Azide across a Zirconium Methylidene.

    PubMed

    Kurogi, Takashi; Mane, Manoj V; Zheng, Shuai; Carroll, Patrick J; Baik, Mu-Hyun; Mindiola, Daniel J

    2018-02-12

    The zirconium methylidene (PNP)Zr=CH 2 (OAr) (1) reacts with N 3 Ad to give two products (PNP)Zr=NAd(OAr) (2) and (PNP)Zr(η 2 -N=NAd)(N=CH 2 )(OAr) (3), both resulting from a common cycloaddition intermediate (PNP)Zr(CH 2 N 3 Ad)(OAr) (A). Using a series of control experiments in combination with DFT calculations, it was found that 2 results from a nitrene by a carbene metathesis reaction in which N 2 acts as a delivery vehicle and forms N 2 CH 2 as a side product. In the case of 3, N-N bond splitting of the azide at the α-position allowed the isolation of a rare example of a parent ketimide complex of zirconium. Isotopic labeling studies and solid-state X-ray analysis are presented for 2 and 3, in addition to an independent synthesis for the former. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Combined Advanced Finishing and UV-Laser Conditioning for Producing UV-Damage-Resistant Fused Silica Optics

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

    Menapace, J A; Penetrante, B; Golini, D

    2001-11-01

    Laser induced damage initiation on fused silica optics can limit the lifetime of the components when used in high power UV laser environments. Foe example in inertial confinement fusion research applications, the optics can be exposed to temporal laser pulses of about 3-nsec with average fluences of 8 J/cm{sup 2} and peak fluences between 12 and 15 J/cm{sup 2}. During the past year, we have focused on optimizing the damage performance at a wavelength of 355-nm (3{omega}), 3-nsec pulse length, for optics in this category by examining a variety of finishing technologies with a challenge to improve the laser damagemore » initiation density by at least two orders of magnitude. In this paper, we describe recent advances in improving the 3{omega} damage initiation performance of laboratory-scale zirconium oxide and cerium oxide conventionally finished fused silica optics via application of processes incorporating magnetorheological finishing (MRF), wet chemical etching, and UV laser conditioning. Details of the advanced finishing procedures are described and comparisons are made between the procedures based upon large area 3{omega} damage performance, polishing layer contamination, and optical subsurface damage.« less

  12. Method of making crack-free zirconium hydride

    DOEpatents

    Sullivan, Richard W.

    1980-01-01

    Crack-free hydrides of zirconium and zirconium-uranium alloys are produced by alloying the zirconium or zirconium-uranium alloy with beryllium, or nickel, or beryllium and scandium, or nickel and scandium, or beryllium and nickel, or beryllium, nickel and scandium and thereafter hydriding.

  13. Superconducting composite with multilayer patterns and multiple buffer layers

    DOEpatents

    Wu, Xin D.; Muenchausen, Ross E.

    1993-01-01

    An article of manufacture including a substrate, a patterned interlayer of a material selected from the group consisting of magnesium oxide, barium-titanium oxide or barium-zirconium oxide, the patterned interlayer material overcoated with a secondary interlayer material of yttria-stabilized zirconia or magnesium-aluminum oxide, upon the surface of the substrate whereby an intermediate article with an exposed surface of both the overcoated patterned interlayer and the substrate is formed, a coating of a buffer layer selected from the group consisting of cerium oxide, yttrium oxide, curium oxide, dysprosium oxide, erbium oxide, europium oxide, iron oxide, gadolinium oxide, holmium oxide, indium oxide, lanthanum oxide, manganese oxide, lutetium oxide, neodymium oxide, praseodymium oxide, plutonium oxide, samarium oxide, terbium oxide, thallium oxide, thulium oxide, yttrium oxide and ytterbium oxide over the entire exposed surface of the intermediate article, and, a ceramic superco n FIELD OF THE INVENTION The present invention relates to the field of superconducting articles having two distinct regions of superconductive material with differing in-plane orientations whereby the conductivity across the boundary between the two regions can be tailored. This invention is the result of a contract with the Department of Energy (Contract No. W-7405-ENG-36).

  14. Manufacturing process to reduce large grain growth in zirconium alloys

    DOEpatents

    Rosecrans, Peter M.

    1987-01-01

    A method of treating cold-worked zirconium alloys to reduce large grain gth during thermal treatment at temperatures above the recrystallization temperature of the alloy comprising heating the cold-worked alloy between about 1300.degree.-1350.degree. F. for 1 to 3 hours prior to treatment above its recrystallization temperature.

  15. Investigation of phase transition properties of ZrO2 thin films

    NASA Astrophysics Data System (ADS)

    Kumar, Davinder; Singh, Avtar; Kaur, Manpreet; Rana, Vikrant Singh; Kaur, Raminder

    2018-05-01

    This paper presents the synthesis of transparent thin films of zirconium oxide (ZrO2) deposited on glass substrates by sol-gel dip coating technique. Synthesized films were characterized for different annealing time and withdrawal speed. Change in crystallographic properties of thin films was investigated by using X-ray diffraction. Surface morphology of transparent thin films was estimated by using scanning electron microscope.

  16. Castable hot corrosion resistant alloy

    NASA Technical Reports Server (NTRS)

    Barrett, Charles A. (Inventor); Holt, William H. (Inventor)

    1988-01-01

    Some 10 wt percent nickel is added to an Fe-base alloy which has a ferrite microstructure to improve the high temperature castability and crack resistance while about 0.2 wt percent zirconium is added for improved high temperatur cyclic oxidation and corrosion resistance. The basic material is a high temperature FeCrAl heater alloy, and the addition provides a material suitable for burner rig nozzles.

  17. Investigation of hydrogen interaction with defects in zirconia

    NASA Astrophysics Data System (ADS)

    Melikhova, O.; Kuriplach, J.; Čížek, J.; Procházka, I.; Brauer, G.; Anwand, W.

    2010-04-01

    Defect studies of a ZrO2 + 9 mol. % Y2O3 single crystal were performed in this work using a high resolution positron lifetime spectroscopy combined with slow positron implantation spectroscopy. In order to elucidate the nature of positron trapping sites observed experimentally, the structural relaxations of several types of vacancy-like defects in zirconia were performed and positron characteristics for them were calculated. Relaxed atomic configurations of studied defects were obtained by means of ab initio pseudopotential method within the supercell approach. Theoretical calculations indicated that neither oxygen vacancies nor their neutral complexes with substitute yttrium atoms are capable of positron trapping. On the other hand, zirconium vacancies are deep positron traps and are most probably responsible for the saturated positron trapping observed in yttria stabilized zirconia single crystals. However, the calculated positron lifetime for zirconium vacancy is apparently longer than the experimental value corresponding to a single-component spectrum measured for the cubic ZrO2 + 9 mol. % Y2O3 single crystal. It was demonstrated that this effect can be explained by hydrogen trapped in zirconium vacancies. On the basis of structure relaxations, we found that zirconium vacancy - hydrogen complexes represent deep positron traps with the calculated lifetime close to the experimental one. In zirconium vacancy - hydrogen complexes the hydrogen atom forms an O-H bond with one of the nearest neighbour oxygen atoms. The calculated bond length is close to 1 Å.

  18. Plasma electrolytic oxidation treatment mode influence on corrosion properties of coatings obtained on Zr-1Nb alloy in silicate-phosphate electrolyte

    NASA Astrophysics Data System (ADS)

    Farrakhov, R. G.; Mukaeva, V. R.; Fatkullin, A. R.; Gorbatkov, M. V.; Tarasov, P. V.; Lazarev, D. M.; Babu, N. Ramesh; Parfenov, E. V.

    2018-01-01

    This research is aimed at improvement of corrosion properties for Zr-1Nb alloy via plasma electrolytic oxidation (PEO). The coatings obtained in DC, pulsed unipolar and pulsed bipolar modes were assessed using SEM, XRD, PDP and EIS techniques. It was shown that pulsed unipolar mode provides the PEO coatings having promising combination of the coating thickness, surface roughness, porosity, corrosion potential and current density, and charge transfer resistance, all contributing to corrosion protection of the zirconium alloy for advanced fuel cladding applications.

  19. Phase Equilibria Diagrams Database

    National Institute of Standards and Technology Data Gateway

    SRD 31 NIST/ACerS Phase Equilibria Diagrams Database (PC database for purchase)   The Phase Equilibria Diagrams Database contains commentaries and more than 21,000 diagrams for non-organic systems, including those published in all 21 hard-copy volumes produced as part of the ACerS-NIST Phase Equilibria Diagrams Program (formerly titled Phase Diagrams for Ceramists): Volumes I through XIV (blue books); Annuals 91, 92, 93; High Tc Superconductors I & II; Zirconium & Zirconia Systems; and Electronic Ceramics I. Materials covered include oxides as well as non-oxide systems such as chalcogenides and pnictides, phosphates, salt systems, and mixed systems of these classes.

  20. Processing and Properties Of Refractory Zirconium Diboride Composites For Use In High Temperature Applications

    NASA Technical Reports Server (NTRS)

    Stackpoole, Margaret; Gusman, M.; Ellerby, D.; Johnson, S. M.; Arnold, Jim (Technical Monitor)

    2001-01-01

    The Thermal Protection Materials and Systems Branch at NASA Ames Research Center is involved in the development of a class of refractory oxidation-resistant diboride composites termed Ultra High Temperature Ceramics or UHTCs. These composites have good high temperature properties making them candidate materials for thermal protection system (TPS) applications. The current research focuses on improving processing methods to develop more reliable composites with enhanced thermal and mechanical properties. This presentation will concentrate on the processing of ZrB2/SiC composites. Some preliminary mechanical properties and oxidation data will also be presented.

  1. Magnesium-Aluminum-Zirconium Oxide Amorphous Ternary Composite: A Dense and Stable Optical Coating

    NASA Technical Reports Server (NTRS)

    Sahoo, N. K.; Shapiro, A. P.

    1998-01-01

    In the present work, the process parameter dependent optical and structural properties of MgO-Al(2)O(3)-ZrO(2) ternary mixed-composite material have been investigated. Optical properties were derived from spectrophotometric measurements. The surface morphology, grain size distributions, crystallographic phases and process dependent material composition of films have been investigated through the use of Atomic Force Microscopy (AFM), X-ray diffraction analysis and Energy Dispersive X- ray (EDX) analysis. EDX analysis made evident the correlation between the optical constants and the process dependent compositions in the films. It is possible to achieve environmentally stable amorphous films with high packing density under certain optimized process conditions.

  2. Iron-chrome-aluminum alloy cladding for increasing safety in nuclear power plants

    NASA Astrophysics Data System (ADS)

    Rebak, Raul B.

    2017-12-01

    After a tsunami caused plant black out at Fukushima, followed by hydrogen explosions, the US Department of Energy partnered with fuel vendors to study safer alternatives to the current UO2-zirconium alloy system. This accident tolerant fuel alternative should better tolerate loss of cooling in the core for a considerably longer time while maintaining or improving the fuel performance during normal operation conditions. General electric, Oak ridge national laboratory, and their partners are proposing to replace zirconium alloy cladding in current commercial light water power reactors with an iron-chromium-aluminum (FeCrAl) cladding such as APMT or C26M. Extensive testing and evaluation is being conducted to determine the suitability of FeCrAl under normal operation conditions and under severe accident conditions. Results show that FeCrAl has excellent corrosion resistance under normal operation conditions and FeCrAl is several orders of magnitude more resistant than zirconium alloys to degradation by superheated steam under accident conditions, generating less heat of oxidation and lower amount of combustible hydrogen gas. Higher neutron absorption and tritium release effects can be minimized by design changes. The implementation of FeCrAl cladding is a near term solution to enhance the safety of the current fleet of commercial light water power reactors.

  3. INERT GAS SHIELD FOR WELDING

    DOEpatents

    Jones, S.O.; Daly, F.V.

    1958-10-14

    S>An inert gas shield is presented for arc-welding materials such as zirconium that tend to oxidize rapidly in air. The device comprises a rectangular metal box into which the welding electrode is introduced through a rubber diaphragm to provide flexibility. The front of the box is provided with a wlndow having a small hole through which flller metal is introduced. The box is supplied with an inert gas to exclude the atmosphere, and with cooling water to promote the solidification of the weld while in tbe inert atmosphere. A separate water-cooled copper backing bar is provided underneath the joint to be welded to contain the melt-through at the root of the joint, shielding the root of the joint with its own supply of inert gas and cooling the deposited weld metal. This device facilitates the welding of large workpieces of zirconium frequently encountered in reactor construction.

  4. Comparison of abundances of chemical elements in mineralized and unmineralized sandstone of the Brushy Basin Member of the Morrison Formation, Smith Lake District, Grants uranium region, New Mexico

    USGS Publications Warehouse

    Pierson, C.T.; Spirakis, C.S.; Robertson, J.F.

    1983-01-01

    Statistical treatment of analytical data from the Mariano Lake and Ruby uranium deposits in the Smith Lake district, New Mexico, indicates that organic carbon, arsenic, barium, calcium, cobalt, copper, gallium, iron, lead, manganese, molybdenum, nickel, selenium, strontium, sulfur, vanadium, yttrium, and zirconium are concentrated along with uranium in primary ore. Comparison of the Smith Lake data with information from other primary deposits in the Grants uranium region and elsewhere in the Morrison Formation of the Colorado Plateau suggests that these elements, with the possible exceptions of zirconium and gallium and with the probable addition of aluminum and magnesium, are typically associated with primary, tabular uranium deposits. Chemical differences between the Ruby and Mariano Lake deposits are consistent with the interpretation that the Ruby deposit has been more affected by post-mineralization oxidizing solutions than has the Mariano Lake deposit.

  5. Remanufacture of Zirconium-Based Conversion Coatings on the Surface of Magnesium Alloy

    NASA Astrophysics Data System (ADS)

    Liu, Zhe; Jin, Guo; Song, Jiahui; Cui, Xiufang; Cai, Zhaobing

    2017-04-01

    Brush plating provides an effective method for creating a coating on substrates of various shapes. A corroded zirconium-based conversion coating was removed from the surface of a magnesium alloy and then replaced with new coatings prepared via brush plating. The structure and composition of the remanufactured coating were determined via x-ray photoelectron spectroscopy, x-ray diffraction, and Fourier transform infrared spectroscopy. The results revealed that the coatings consist of oxide, fluoride, and tannin-related organics. The composition of the coatings varied with the voltage. Furthermore, as revealed via potentiodynamic polarization spectroscopy, these coatings yielded a significant increase in the corrosion resistance of the magnesium alloy. The friction coefficient remained constant for almost 300s during wear resistance measurements performed under a 1-N load and dry sliding conditions, indicating that the remanufactured coatings provide effective inhibition to corrosion.

  6. Lightweight, Ultra-High-Temperature, CMC-Lined Carbon/Carbon Structures

    NASA Technical Reports Server (NTRS)

    Wright, Matthew J.; Ramachandran, Gautham; Williams, Brian E.

    2011-01-01

    Carbon/carbon (C/C) is an established engineering material used extensively in aerospace. The beneficial properties of C/C include high strength, low density, and toughness. Its shortcoming is its limited usability at temperatures higher than the oxidation temperature of carbon . approximately 400 C. Ceramic matrix composites (CMCs) are used instead, but carry a weight penalty. Combining a thin laminate of CMC to a bulk structure of C/C retains all of the benefits of C/C with the high temperature oxidizing environment usability of CMCs. Ultramet demonstrated the feasibility of combining the light weight of C/C composites with the oxidation resistance of zirconium carbide (ZrC) and zirconium- silicon carbide (Zr-Si-C) CMCs in a unique system composed of a C/C primary structure with an integral CMC liner with temperature capability up to 4,200 F (.2,315 C). The system effectively bridged the gap in weight and performance between coated C/C and bulk CMCs. Fabrication was demonstrated through an innovative variant of Ultramet fs rapid, pressureless melt infiltration processing technology. The fully developed material system has strength that is comparable with that of C/C, lower density than Cf/SiC, and ultra-high-temperature oxidation stability. Application of the reinforced ceramic casing to a predominantly C/C structure creates a highly innovative material with the potential to achieve the long-sought goal of long-term, cyclic high-temperature use of C/C in an oxidizing environment. The C/C substructure provided most of the mechanical integrity, and the CMC strengths achieved appeared to be sufficient to allow the CMC to perform its primary function of protecting the C/C. Nozzle extension components were fabricated and successfully hot-fire tested. Test results showed good thermochemical and thermomechanical stability of the CMC, as well as excellent interfacial bonding between the CMC liner and the underlying C/C structure. In particular, hafnium-containing CMCs on C/C were shown to perform well at temperatures exceeding 3,500 F (.1,925 C). The melt-infiltrated CMC-lined C/C composites offered a lower density than Cf/SiC. The melt-infiltrated composites offer greater use temperature than Cf/SiC because of the more refractory ceramic matrices and the C/C substructure provides greater high-temperature strength. The progress made in this work will allow multiple high-temperature components used in oxidizing environments to take advantage of the low density and high strength of C/C combined with the high-temperature oxidation resistance of melt-infiltrated CMCs.

  7. Modification in band gap of zirconium complexes

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

    Sharma, Mayank, E-mail: mayank30134@gmail.com; Singh, J.; Chouhan, S.

    2016-05-06

    The optical properties of zirconium complexes with amino acid based Schiff bases are reported here. The zirconium complexes show interesting stereo chemical features, which are applicable in organometallic and organic synthesis as well as in catalysis. The band gaps of both Schiff bases and zirconium complexes were obtained by UV-Visible spectroscopy. It was found that the band gap of zirconium complexes has been modified after adding zirconium compound to the Schiff bases.

  8. METHOD OF FABRICATING A URANIUM-ZIRCONIUM HYDRIDE REACTOR CORE

    DOEpatents

    Weeks, I.F.; Goeddel, W.V.

    1960-03-22

    A method is described of evenly dispersing uranlum metal in a zirconium hydride moderator to produce a fuel element for nuclear reactors. According to the invention enriched uranium hydride and zirconium hydride powders of 200 mesh particle size are thoroughly admixed to form a mixture containing 0.1 to 3% by weight of U/sup 235/ hydride. The mixed powders are placed in a die and pressed at 100 tons per square inch at room temperature. The resultant compacts are heated in a vacuum to 300 deg C, whereby the uranium hydride deoomposes into uranium metal and hydrogen gas. The escaping hydrogen gas forms a porous matrix of zirconium hydride, with uramum metal evenly dispersed therethrough. The advantage of the invention is that the porosity and uranium distribution of the final fuel element can be more closely determined and controlled than was possible using prior methods of producing such fuel ele- ments.

  9. Hot Corrosion Behavior of Bare, Cr3C2-(NiCr) and Cr3C2-(NiCr) + 0.2wt.%Zr Coated SuperNi 718 at 900 °C

    NASA Astrophysics Data System (ADS)

    Mudgal, Deepa; Singh, Surendra; Prakash, Satya

    2015-01-01

    Corrosion in incinerators, power plants, and chemical industries are frequently encountered due to the presence of salts containing sodium, sulphur, and chlorine. To obviate this problem, bare and coated alloys were tested under environments simulating the conditions present inside incinerators and power plants. 0.2 wt.% zirconium powder was incorporated in the Cr3C2-(NiCr) coating powder. The original powder and Zr containing powder was sprayed on Superni 718 alloy by D-gun technique. The bare and coated alloys were tested under Na2SO4 + K2SO4 + NaCl + KCl and Na2SO4 + NaCl environment. The corrosion rate of specimens was monitored using weight change measurements. Characterization of the corrosion products has been done using FE-SEM/EDS and XRD techniques. Bare and coated alloys showed very good corrosion resistance under given molten salt environments. Addition of 0.2wt.%Zr in Cr3C2-25%(NiCr) coating further greatly reduced the oxidation rate as well as improved the adherence of oxide scale to the coating surface during the time of corrosion.

  10. Soft-Templating Synthesis of Mesoporous Silica-Based Materials for Environmental Applications

    NASA Astrophysics Data System (ADS)

    Gunathilake, Chamila Asanka

    Dissertation research is mainly focus on: 1) the development of mesoporous silica materials with organic pendant and bridging groups (isocyanurate, amidoxime, benzene) and incorporated metal (aluminum, zirconium, calcium, and magnesium) species for high temperature carbon dioxide (CO2) sorption, 2) phosphorous-hydroxy functionalized mesoporous silica materials for water treatment, and 3) amidoxime-modified ordered mesoporous silica materials for uranium sorption under seawater conditions. The goal is to design composite materials for environmental applications with desired porosity, surface area, and functionality by selecting proper metal oxide precursors, organosilanes, tetraethylorthosilicate, (TEOS), and block copolymer templates and by adjusting synthesis conditions. The first part of dissertation presents experimental studies on the merge of aluminum, zirconium, calcium, and magnesium oxides with mesoporous silica materials containing organic pendant (amidoxime) and bridging groups (isocyanurate, benzene) to obtain composite sorbents for CO2 sorption at ambient (0-25 °C) and elevated (60-120 °C) temperatures. These studies indicate that the aforementioned composite sorbents are fairly good for CO2 capture at 25 °C via physisorption mechanism and show a remarkably high affinity toward CO2 chemisorption at 60-120 °C. The second part of dissertation is devoted to silica-based materials with organic functionalities for removal of heavy metal ions such as lead from contaminated water and for recovery of metal ions such as uranium from seawater. First, ordered mesoporous organosilica (OMO) materials with diethylphosphatoethyl and hydroxyphosphatoethyl surface groups were examined for Pb2+ adsorption and showed unprecedented adsorption capacities up to 272 mg/g and 202 mg/g, respectively However, the amidoxime-modified OMO materials were explored for uranium extraction under seawater conditions and showed remarkable capacities reaching 57 mg of uranium per gram of adsorbent.

  11. Zirconium diselenite microstructures, formation and mechanism

    NASA Astrophysics Data System (ADS)

    Naik, Chandan C.; Salker, A. V.

    2018-04-01

    In this work, a series of microstructures of zirconium diselenite (Zr(SeO3)2) has been prepared via a simple precipitation method at room temperature without adding any organic surfactants. Phase purity of the sample has been checked by X-ray Diffraction. From the SEM, FESEM, and TEM images spheroid nanoparticles to the starfish-like structure of zirconium diselenite are detected. The morphological evolution processes were investigated carefully following time-dependent experiments and a growth mechanism has been proposed. Two different crystal growth processes, the oriented attachment process accompanying the Ostwald ripening process were held responsible for the formation of a structure resembling starfish having four arms.

  12. Application of diffusion barriers to the refractory fibers of tungsten, columbium, carbon and aluminum oxide

    NASA Technical Reports Server (NTRS)

    Douglas, F. C.; Paradis, E. L.; Veltri, R. D.

    1973-01-01

    A radio frequency powered ion-plating system was used to plate protective layers of refractory oxides and carbide onto high strength fiber substrates. Subsequent overplating of these combinations with nickel and titanium was made to determine the effectiveness of such barrier layers in preventing diffusion of the overcoat metal into the fibers with consequent loss of fiber strength. Four substrates, five coatings, and two metal matrix materials were employed for a total of forty material combinations. The substrates were tungsten, niobium, NASA-Hough carbon, and Tyco sapphire. The diffusion-barrier coatings were aluminum oxide, yttrium oxide, titanium carbide, tungsten carbide with 14% cobalt addition, and zirconium carbide. The metal matrix materials were IN 600 nickel and Ti 6/4 titanium. Adhesion of the coatings to all substrates was good except for the NASA-Hough carbon, where flaking off of the oxide coatings in particular was observed.

  13. Hot corrosion of the B2 nickel aluminides

    NASA Technical Reports Server (NTRS)

    Ellis, David L.

    1993-01-01

    The hot corrosion behavior of the B2 nickel aluminides was studied to determine the inherent hot corrosion resistance of the beta nickel aluminides and to develop a mechanism for the hot corrosion of the beta nickel aluminides. The effects of the prior processing of the material, small additions of zirconium, stoichiometry of the materials, and preoxidation of the samples were also examined. Additions of 2, 5, and 15 w/o chromium were used to determine the effect of chromium on the hot corrosion of the beta nickel aluminides and the minimum amount of chromium necessary for good hot corrosion resistance. The results indicate that the beta nickel aluminides have inferior inherent hot corrosion resistance despite their excellent oxidation resistance. Prior processing and zirconium additions had no discernible effect on the hot corrosion resistance of the alloys. Preoxidation extended the incubation period of the alloys only a few hours and was not considered to be an effective means of stopping hot corrosion. Stoichiometry was a major factor in determining the hot corrosion resistance of the alloys with the higher aluminum alloys having a definitely superior hot corrosion resistance. The addition of chromium to the alloys stopped the hot corrosion attack in the alloys tested. From a variety of experimental results, a complex hot corrosion mechanism was proposed. During the early stages of the hot corrosion of these alloys the corrosion is dominated by a local sulphidation/oxidation form of attack. During the intermediate stages of the hot corrosion, the aluminum depletion at the surface leads to a change in the oxidation mechanism from a protective external alumina layer to a mixed nickel-aluminum spinel and nickel oxide that can occur both externally and internally. The material undergoes extensive cracking during the later portions of the hot corrosion.

  14. Enhanced Antimicrobial Activity Of Antibiotics Mixed With Metal Nanoparticles

    NASA Astrophysics Data System (ADS)

    Kumar, Sandeep; Kumar, Neeraj; Bhanjana, Gaurav; Thakur, Rajesh; Dilbaghi, Neeraj

    2011-12-01

    Current producers of antimicrobial technology have a long lasting, environmentally safe, non-leaching, water soluble solution that will eventually replace all poisons and heavy metals. The transition metal ions inevitably exist as metal complexes in biological systems by interaction with the numerous molecules possessing groupings capable of complexation or chelation. Nanoparticles of metal oxides offer a wide variety of potential applications in medicine due to the unprecedented advances in nanobiotechnology research. the bacterial action of antibiotics like penicillin, erythryomycin, ampicillin, streptomycin, kanamycin etc. and that of a mixture of antibiotics and metal and metal oxide nanoparticles like zinc oxide, zirconium, silver and gold on microbes was examined by the agar-well-diffusion method, enumeration of colony-forming units (CFU) and turbidimetry.

  15. Aerosol chemical vapor deposition of metal oxide films

    DOEpatents

    Ott, K.C.; Kodas, T.T.

    1994-01-11

    A process of preparing a film of a multicomponent metal oxide including: forming an aerosol from a solution comprised of a suitable solvent and at least two precursor compounds capable of volatilizing at temperatures lower than the decomposition temperature of said precursor compounds; passing said aerosol in combination with a suitable oxygen-containing carrier gas into a heated zone, said heated zone having a temperature sufficient to evaporate the solvent and volatilize said precursor compounds; and passing said volatilized precursor compounds against the surface of a substrate, said substrate having a sufficient temperature to decompose said volatilized precursor compounds whereby metal atoms contained within said volatilized precursor compounds are deposited as a metal oxide film upon the substrate is disclosed. In addition, a coated article comprising a multicomponent metal oxide film conforming to the surface of a substrate selected from the group consisting of silicon, magnesium oxide, yttrium-stabilized zirconium oxide, sapphire, or lanthanum gallate, said multicomponent metal oxide film characterized as having a substantially uniform thickness upon said substrate.

  16. Electrical and dielectric properties of ZnO and CeO{sub 2} doped ZrTi{sub 2}O{sub 6} ceramic

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

    George, Aneesh; Thomas, Jijimon K.; John, Annamma

    2014-01-28

    Zirconium oxide (ZrO{sub 2}) and titanium dioxide (TiO{sub 2}) are the important catalyst supports, since it has acidic and basic properties. The intermediate phase zirconium titanate ZrTi{sub 2}O{sub 6}, which is a solid solution with Zr:Ti ratio 1:2 has outstanding dielectric properties. The effects of doping of ZnO and CeO{sub 2} on the dielectric and electrical properties of ZrTi{sub 2}O{sub 6} ceramic are investigated. On adding 0.5 wt% ZnO, the dielectric constant is increased but, on adding CeO{sub 2}, the dielectric constant is decreased. The bulk density of pure sample sintered at 1530 °C is 91% of theoretical density whilemore » that of the doped samples sintered at 1450 °C is more than 94% of theoretical density. Scanning electron micrographs reveal that the samples are well sintered with minimum porosity. The semicircle behavior in the Cole-Cole plots at room temperature reveals that the samples are good ionic conductor. The induced impedance is reduced for doped samples and this can be used as a material for electrolyte in Solid Oxide Fuel Cell.« less

  17. Cationic polyelectrolyte induced separation of some inorganic contaminants and their mixture (zirconium silicate, kaolin, K-feldspar, zinc oxide) as well as of the paraffin oil from water.

    PubMed

    Ghimici, Luminita

    2016-03-15

    The flocculation efficiency of a cationic polyelectrolyte with quaternary ammonium salt groups in the backbone, namely PCA5 was evaluated on zirconium silicate (kreutzonit), kaolin, K- feldspar and zinc oxide (ZnO) suspensions prepared either with each pollutant or with their mixture. The effect of several parameters such as settling time, polymer dose and the pollutant type on the separation efficacy was evaluated and followed by optical density and zeta potential measurements. Except for ZnO, the interactions between PCA5 and suspended particles led to low residual turbidity values (around 4% for kreutzonit, 5% for kaolin and 8% for K-feldspar) as well as to the reduction of flocs settling time (from 1200 min to 30 min and 120 min in case of kaolinit and K-feldspar, respectively), that meant a high efficiency in their separation. The negative value of the zeta potential and flocs size measurements, at the optimum polymer dose, point to contribution from charge patch mechanism for the particles flocculation. A good efficiency of PCA5 in separation of paraffin oil (a minimum residual turbidity of 9.8%) has been also found. Copyright © 2015 Elsevier Ltd. All rights reserved.

  18. Fabrication of a Biomass-Based Hydrous Zirconium Oxide Nanocomposite for Preferable Phosphate Removal and Recovery.

    PubMed

    Qiu, Hui; Liang, Chen; Zhang, Xiaolin; Chen, Mindong; Zhao, Yunxia; Tao, Tao; Xu, Zhengwen; Liu, Gang

    2015-09-23

    Advanced removal of phosphate by low-cost adsorbents from municipal wastewater or industrial effluents is an effective and economic way to prevent the occurrence of eutrophication. Here, we proposed a novel method to immobilize hydrous zirconium oxide nanoparticle within quaternary-aminated wheat straw, and obtained an inexpensive, eco-friendly nanocomposite Ws-N-Zr. The biomass-based Ws-N-Zr exhibited higher preference toward phosphate than commercial anion exchanger IRA-900 when competing sulfate ions coexisted at relatively high levels. Such excellent performance of Ws-N-Zr resulted from its specific hybrid structure, the quaternary ammonium groups bonded on the host favor the preconcentration of phosphate ions inside the wheat straw based on Donnan effect, and the encapsulated HZO nanoparticle exhibits preferable sequestration of phosphate ions through specific interaction, as further demonstrated by FTIR and X-ray photoelectron spectroscopy. Cycle adsorption and regeneration experiments demonstrated that Ws-N-Zr could be employed for repeated use without significant capacity loss, when the binary NaOH-NaCl solution was employed as the regenerant. The influence of solution pH and contact time was also examined. The results suggested that Ws-N-Zr has a great potential in efficient removal of phosphate in contaminated waters.

  19. Examination of Calcium Silicate Cements with Low-Viscosity Methyl Cellulose or Hydroxypropyl Cellulose Additive.

    PubMed

    Baba, Toshiaki; Tsujimoto, Yasuhisa

    2016-01-01

    The purpose of this study was to improve the operability of calcium silicate cements (CSCs) such as mineral trioxide aggregate (MTA) cement. The flow, working time, and setting time of CSCs with different compositions containing low-viscosity methyl cellulose (MC) or hydroxypropyl cellulose (HPC) additive were examined according to ISO 6876-2012; calcium ion release analysis was also conducted. MTA and low-heat Portland cement (LPC) including 20% fine particle zirconium oxide (ZO group), LPC including zirconium oxide and 2 wt% low-viscosity MC (MC group), and HPC (HPC group) were tested. MC and HPC groups exhibited significantly higher flow values and setting times than other groups ( p < 0.05). Additionally, flow values of these groups were higher than the ISO 6876-2012 reference values; furthermore, working times were over 10 min. Calcium ion release was retarded with ZO, MC, and HPC groups compared with MTA. The concentration of calcium ions was decreased by the addition of the MC or HPC group compared with the ZO group. When low-viscosity MC or HPC was added, the composition of CSCs changed, thus fulfilling the requirements for use as root canal sealer. Calcium ion release by CSCs was affected by changing the CSC composition via the addition of MC or HPC.

  20. Examination of Calcium Silicate Cements with Low-Viscosity Methyl Cellulose or Hydroxypropyl Cellulose Additive

    PubMed Central

    Tsujimoto, Yasuhisa

    2016-01-01

    The purpose of this study was to improve the operability of calcium silicate cements (CSCs) such as mineral trioxide aggregate (MTA) cement. The flow, working time, and setting time of CSCs with different compositions containing low-viscosity methyl cellulose (MC) or hydroxypropyl cellulose (HPC) additive were examined according to ISO 6876-2012; calcium ion release analysis was also conducted. MTA and low-heat Portland cement (LPC) including 20% fine particle zirconium oxide (ZO group), LPC including zirconium oxide and 2 wt% low-viscosity MC (MC group), and HPC (HPC group) were tested. MC and HPC groups exhibited significantly higher flow values and setting times than other groups (p < 0.05). Additionally, flow values of these groups were higher than the ISO 6876-2012 reference values; furthermore, working times were over 10 min. Calcium ion release was retarded with ZO, MC, and HPC groups compared with MTA. The concentration of calcium ions was decreased by the addition of the MC or HPC group compared with the ZO group. When low-viscosity MC or HPC was added, the composition of CSCs changed, thus fulfilling the requirements for use as root canal sealer. Calcium ion release by CSCs was affected by changing the CSC composition via the addition of MC or HPC. PMID:27981048

  1. Five year survival analysis of an oxidised zirconium total knee arthroplasty.

    PubMed

    Holland, Philip; Santini, Alasdair J A; Davidson, John S; Pope, Jill A

    2013-12-01

    Zirconium total knee arthroplasties theoretically have a low incidence of failure as they are low friction, hard wearing and hypoallergenic. We report the five year survival of 213 Profix zirconium total knee arthroplasties with a conforming all polyethylene tibial component. Data was collected prospectively and multiple strict end points were used. SF12 and WOMAC scores were recorded pre-operatively, at three months, at twelve months, at 3 years and at 5 years. Eight patients died and six were "lost to follow-up". The remaining 199 knees were followed up for five years. The mean WOMAC score improved from 56 to 35 and the mean SF12 physical component score improved from 28 to 34. The five year survival for failure due to implant related reasons was 99.5% (95% CI 97.4-100). This was due to one tibial component becoming loose aseptically in year zero. Our results demonstrate that the Profix zirconium total knee arthroplasty has a low medium term failure rate comparable to the best implants. Further research is needed to establish if the beneficial properties of zirconium improve long term implant survival. Copyright © 2012 Elsevier B.V. All rights reserved.

  2. Electron-hole pairs generated in ZrO2 nanoparticle resist upon exposure to extreme ultraviolet radiation

    NASA Astrophysics Data System (ADS)

    Kozawa, Takahiro; Santillan, Julius Joseph; Itani, Toshiro

    2018-02-01

    Metal oxide nanoparticle resists have attracted much attention as the next-generation resist used for the high-volume production of semiconductor devices. However, the sensitization mechanism of the metal oxide nanoparticle resists is unknown. Understanding the sensitization mechanism is important for the efficient development of resist materials. In this study, the energy deposition in a zirconium oxide (ZrO2) nanoparticle resist was investigated. The numbers of electron-hole pairs generated in a ZrO2 core and an methacrylic acid (MAA) ligand shell upon exposure to 1 mJ cm-2 (exposure dose) extreme ultraviolet (EUV) radiations were theoretically estimated to be 0.16 at most and 0.04-0.17 cm2 mJ-1, respectively. By comparing the calculated distribution of electron-hole pairs with the line-and-space patterns of the ZrO2 nanoparticle resist fabricated by an EUV exposure tool, the number of electron-hole pairs required for the solubility change of the resist films was estimated to be 1.3-2.2 per NP. NP denotes a nanoparticle consisting of a metal oxide core with a ligand shell. In the material design of metal oxide nanoparticle resists, it is important to efficiently use the electron-hole pairs generated in the metal oxide core for the chemical change of ligand molecules.

  3. Effects of the Fabrication Process and Thermal Cycling on the Oxidation of Zirconium-Niobium Pressure Tubes

    NASA Astrophysics Data System (ADS)

    Nam, Cheol

    2009-12-01

    Pressure tubes made of Zr-2.5%Nb alloy are used to contain fuels and coolant in CANDU nuclear power reactors The pressure tube oxidizes during reactor operation and hydrogen ingress through the oxide grown on the tube limits its lifetime. Little attention was paid to the intermediate tube manufacturing processes in enhancing the oxidation resistance. In addition, the oxide grown on the tube experiences various thermal cycles depending on the reactor shutdown and startup cycles. To address these two aspects and to better understand the oxidation process of the Zr-2.5Nb tube, research was conducted in two parts: (i) effects of tube fabrication on oxidation behavior, and (ii) thermal cycling behaviors of oxides grown on a pressure tube. In the first part, the optimum manufacturing process was pursued to improve the corrosion resistance of Zr-2.5Nb tubes. Experimental micro-tubes were fabricated with various manufacturing routes in the stages of billet preparation, hot extrusion and cold drawing. These were oxidized in air at 400°C and 500°C, and in an autoclave at 360°C lithiated water. Microstructure and texture of the tubes and oxides were characterized with X-ray diffraction, scanning electron microscope and optical microscope. Special emphasis was given to examinations of the metal/oxide interface structures. A correlation between the manufacturing process and oxidation resistance was investigated in terms of tube microstructure and the metal/oxide interface structure. As a result, it was consistently observed that uniform interface structures were formed on the tubes which had a fine distribution of secondary phases. These microstructures were found to be beneficial in enhancing the oxidation resistance as opposed to the tubes that had coarse and continuous beta-Zr phases. Based on these observations, a schematic model of the oxidation process was proposed with respect to the oxidation resistance under oxidizing temperatures of 360°C, 400°C and 500°C. In the second part, the oxides grown on a standard Zr-2.5Nb pressure tube were analyzed by X-ray diffraction peak broadening and line shift. Crystallite size, t-ZrO2 fraction and residual stress of the zirconium oxides were investigated upon several thermal cycles at DeltaT range of 500°C--750°C. The oxide residual stresses measured by the sin2psi method were always compressive around 2 GPa. Different stress-states were noticed with the oxides grown on different sections of pressure tube. The compressive stress was released when the oxide was thermally cycled at the highest DeltaT of 750°C. Discussion was given to the effects of anisotropic nature of thermal expansion coefficients and crystallographic texture on the stress-state of Zr oxides.

  4. Y3Fe5O12/Na,Bi,Sr-doped PZT particulate magnetoelectric composites

    NASA Astrophysics Data System (ADS)

    Lisnevskaya, I. V.; Bobrova, I. A.; Lupeiko, T. G.; Agamirzoeva, M. R.; Myagkaya, K. V.

    2016-05-01

    Magnetoelectric (ME) composites of Na, Bi, Sr substituted lead zirconate titanate (PZT) and yttrium iron garnet having representative formula (100-x) wt% Na,Bi,Sr-doped PZT (PZTNB-1)+x wt% Y3Fe5O12 (YIG) with x=10-90 were manufactured using powdered components obtained through sol-gel processes. It is shown that the decrease in sintering temperature provided by the use of finely dispersed PZTNB-1 and YIG powders allows to significantly reduce content of fluorite-like foreign phase based on zirconium oxide, which forms due to the interfacial interaction during heat treatment and becomes stabilized by yttrium oxide. Connectivity has considerable effect on the value of ME coefficient of composite ceramics. With the same x value, ΔE/ΔH characteristic decreases when changing from 0-3-type structured composites (PZT grains embedded in ferrite matrix) to 3-3-(interpenetrating network of two phases) and especially 3-0-type samples (YIG grains embedded in PZT matrix); in the last case this can be attributed to the substrate clamping effect when ferrite grains are clamped with piezoelectric matrix. ΔE/ΔH value of 0-3 composites with x=40-60 wt% was found to be ∼1.6 mV/(cm Oe).

  5. SEPARATION PROCESS FOR ZIRCONIUM AND COMPOUNDS THEREOF

    DOEpatents

    Crandall, H.W.; Thomas, J.R.

    1959-06-30

    The separation of zirconium from columbium, rare earths, yttrium and the alkaline earth metals, such mixtures of elements occurring in zirconium ores or neutron irradiated uranium is described. According to the invention a suitable separation of zirconium from a one normal acidic aqueous solution containing salts, nitrates for example, of tetravalent zirconium, pentavalent columbium, yttrium, rare earths in the trivalent state and alkaline earths can be obtained by contacting the aqueous solution with a fluorinated beta diketonc alone or in an organic solvent solution, such as benzene, to form a zirconium chelate compound. When the organic solvent is present the zirconium chelate compound is directly extracted; otherwise it is separated by filtration. The zirconium may be recovered from contacting the organic solvent solution containing the chelated compound by back extraction with either an aqueous hydrofluoric acid or an oxalic acid solution.

  6. Evaluation of cutting efficiency of ultrasonic tips used in orthograde endodontic treatment.

    PubMed

    Lin, Yu-Heng; Mickel, André K; Jones, Jefferson J; Montagnese, Thomas A; González, Alvaro F

    2006-04-01

    The purpose of the present study was to evaluate the cutting efficiency of the three different ultrasonic tips for orthograde endodontic treatment: stainless steel, zirconium nitride-coated, and diamond-coated tips. An ultrasonic handpiece was mounted on a custom-made automated balance, and each tip repeatedly penetrated dental stone blocks to a depth of 3 mm for 10 times. The amount of time taken to penetrate 3 mm of stone was measured. The diamond-coated tips showed significantly greater cutting efficiency than either stainless steel tips or zirconium-nitride coated tips. The stainless steel tips showed initial better cutting efficiency, but over time , there is no significant difference between the cutting efficiency of the stainless steel tips and the zirconium nitride coated tips. The diamond coated tips were the only group that showed breakage in this study.

  7. Solid oxide fuel cell having a glass composite seal

    DOEpatents

    De Rose, Anthony J.; Mukerjee, Subhasish; Haltiner, Jr., Karl Jacob

    2013-04-16

    A solid oxide fuel cell stack having a plurality of cassettes and a glass composite seal disposed between the sealing surfaces of adjacent cassettes, thereby joining the cassettes and providing a hermetic seal therebetween. The glass composite seal includes an alkaline earth aluminosilicate (AEAS) glass disposed about a viscous glass such that the AEAS glass retains the viscous glass in a predetermined position between the first and second sealing surfaces. The AEAS glass provides geometric stability to the glass composite seal to maintain the proper distance between the adjacent cassettes while the viscous glass provides for a compliant and self-healing seal. The glass composite seal may include fibers, powders, and/or beads of zirconium oxide, aluminum oxide, yttria-stabilized zirconia (YSZ), or mixtures thereof, to enhance the desirable properties of the glass composite seal.

  8. Zirconium determination by cooling curve analysis during the pyroprocessing of used nuclear fuel

    NASA Astrophysics Data System (ADS)

    Westphal, B. R.; Price, J. C.; Bateman, K. J.; Marsden, K. C.

    2015-02-01

    An alternative method to sampling and chemical analyses has been developed to monitor the concentration of zirconium in real-time during the casting of uranium products from the pyroprocessing of used nuclear fuel. The method utilizes the solidification characteristics of the uranium products to determine zirconium levels based on standard cooling curve analyses and established binary phase diagram data. Numerous uranium products have been analyzed for their zirconium content and compared against measured zirconium data. From this data, the following equation was derived for the zirconium content of uranium products:

  9. Properties of zirconium silicate and zirconium-silicon oxynitride high-k dielectric alloys for advanced microelectronic applications: Chemical and electrical characterizations

    NASA Astrophysics Data System (ADS)

    Ju, Byongsun

    2005-11-01

    As the microelectronic devices are aggressively scaled down to the 1999 International Technology Roadmap, the advanced complementary metal oxide semiconductor (CMOS) is required to increase packing density of ultra-large scale integrated circuits (ULSI). High-k alternative dielectrics can provide the required levels of EOT for device scaling at larger physical thickness, thereby providing a materials pathway for reducing the tunneling current. Zr silicates and its end members (SiO2 and ZrO2) and Zr-Si oxynitride films, (ZrO2)x(Si3N 4)y(SiO2)z, have been deposited using a remote plasma-enhanced chemical vapor deposition (RPECVD) system. After deposition of Zr silicate, the films were exposed to He/N2 plasma to incorporate nitrogen atoms into the surface of films. The amount of incorporated nitrogen atoms was measured by on-line Auger electron spectrometry (AES) as a function of silicate composition and showed its local minimum around the 30% silicate. The effect of nitrogen atoms on capacitance-voltage (C-V) and leakage-voltage (J-V) were also investigated by fabricating metal-oxide-semiconductor (MOS) capacitors. Results suggested that incorporating nitrogen into silicate decreased the leakage current in SiO2-rich silicate, whereas the leakage increased in the middle range of silicate. Zr-Si oxynitride was a pseudo-ternary alloy and no phase separation was detected by x-ray photoelectron spectroscopy (XPS) analysis up to 1100°C annealing. The leakage current of Zr-Si oxynitride films showed two different temperature dependent activation energies, 0.02 eV for low temperature and 0.3 eV for high temperature. Poole-Frenkel emission was the dominant leakage mechanism. Zr silicate alloys with no Si3N4 phase were chemically separated into the SiO2 and ZrO2 phase as annealed above 900°C. While chemical phase separation in Zr silicate films with Si 3N4 phase (Zr-Si oxynitride) were suppressed as increasing the amount of Si3N4 phase due to the narrow bonding network m Si3N4 phase. (3.4 bonds/atom for Si3 N4 network, 2.67 bonds/atom for SiO2 network).

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

    Wood, Elizabeth Sooby; Parker, Stephen Scott; Nelson, Andrew Thomas

    The Fuel Cycle Research and Development program’s Advanced Fuels Campaign is currently supporting a range of experimental efforts aimed at the development and qualification of ‘accident tolerant’ nuclear fuel forms. One route to enhance the accident tolerance of nuclear fuel is to replace the zirconium alloy cladding, which is prone to rapid oxidation in steam at elevated temperatures, with a more oxidation-resistant cladding. Several cladding replacement solutions have been envisaged. The cladding can be completely replaced with a more oxidation resistant alloy, a layered approach can be used to optimize the strength, creep resistance, and oxidation tolerance of various materials,more » or the existing zirconium alloy cladding can be coated with a more oxidation-resistant material. Molybdenum is one candidate cladding material favored due to its high temperature creep resistance. However, it performs poorly under autoclave testing and suffers degradation under high temperature steam oxidation exposure. Development of composite cladding architectures consisting of a molybdenum core shielded by a molybdenum disilicide (MoSi 2) coating is hypothesized to improve the performance of a Mo-based cladding system. MoSi 2 was identified based on its high temperature oxidation resistance in O 2 atmospheres (e.g. air and “wet air”). However, its behavior in H 2O is less known. This report presents thermogravimetric analysis (TGA), scanning electron microscopy (SEM), and x-ray diffraction (XRD) results for MoSi 2 exposed to 670-1498 K water vapor. Synthetic air (80-20%, Ar-O 2) exposures were also performed, and those results are presented here for a comparative analysis. It was determined that MoSi 2 displays drastically different oxidation behavior in water vapor than in dry air. In the 670-1498 K temperature range, four distinct behaviors are observed. Parabolic oxidation is exhibited in only 670-773 K water vapor, a temperature range in which the material pests in dry O 2 environments. From 877-1084 K in water vapor, MoSi 2 undergoes rapid mass gain resulting in oxidation throughout the bulk of the sample at 980 K and 1084 K. The resulting material displays swelling and warping after the 980-1084 K exposures. A pre-passivation heat treatment performed at 1395 K was found capable of producing a coarse SiO 2 layer that limited pesting at lower temperatures in water vapor over the time periods investigated.« less

  11. ZIRCONIUM-CLADDING OF THORIUM

    DOEpatents

    Beaver, R.J.

    1961-11-21

    A method of cladding thorium with zirconium is described. The quality of the bond achieved between thorium and zirconium by hot-rolling is improved by inserting and melting a thorium-zirconium alloy foil between the two materials prior to rolling. (AEC)

  12. Using Yttra-Stabilized Zirconium Oxide Ceramics to Sense pH and Oxygen in Hydrothermal and Geothermal Applications

    NASA Astrophysics Data System (ADS)

    Manna, M. F.; Grandstaff, D. E.; Ulmer, G. C.

    2002-05-01

    Zirconium-Oxide ceramics stabilized with ~8-wt% Yttrium-Oxide can be employed to sense pH in high temperature (>90oC) aqueous environments with an accuracy of 0.05 pH log units (Lvov et al., in press), and to sense the fugacity of oxygen (fO2) in low temperature (>230oC) gaseous environments with an accuracy of 0.2 (fO2) log units. The major components, in two commercially available yttria-stabilized ceramics are yttria ( ~8-wt%) and zirconia ( ~91-wt%) with minor amounts of Ti, Fe and U. The textural differences in the two ceramics produces significantly different emf vs. 10,000/T responses. Response error can be introduced by: the ionic contribution of the softening glass, the catalytic action of the Pt sensor components, and the presence of Ti and Fe in the ceramic, which has been shown to alter the oxygen diffusivity of the ceramic. (Merino et al., 1996) The first type of ceramic contains a 3-dimensionally-continuous Ca-Al-Si feldspathic glass that acts as a sintering aid during manufacturing. The glass, which has a higher ionic conductivity than the zirconia ceramic, reduces the bulk resistivity and induces an error over the temperature ranges representing the softening point of the glass. The glass also reduces durability of the ceramic. When the glass hydrates it produces zeolites, which grow primarily in the triple-grain-junctions of the ceramic. Thus mechanically weakening the ceramic generating electronic, ionic and mechanical stability problems. The second type of ceramic contains no grain boundary glass, but does contain discrete silicate phases (such as diopside, wollastonite, periclase, silica, etc.) in the triple-grain-junctions. Because there is no inter-granular glass, the type two ceramic does have a greater bulk resistivity compared with the type one ceramic. In a gas-sensing configuration, resistivity has been shown to affect the minimum temperature of sensor operation. A sensor with a higher bulk resistivity must reach a higher minimum temperature before the sensor will sense oxygen. Literature suggests that the same is true for the sensor in its aqueous pH configuration. In addition to the mechanical degradation, there are also chemical leaching issues with both ceramics. While zirconium is relatively unleachable in its pure form, the addition of yttria, while creating the necessary lattice defects, increases the vulnerability of the solid solution grains to acidic solutions. This, creates ceramic durability problems during long-term down-hole operation. The ceramics do function well as a sensor and can produce highly accurate results (with calibration) and if the durability issues are taken into account, the ceramic sensor could be a highly desirable for many high temperature geologic and industrial applications.

  13. Solid oxide electrochemical cell fabrication process

    DOEpatents

    Dollard, Walter J.; Folser, George R.; Pal, Uday B.; Singhal, Subhash C.

    1992-01-01

    A method to form an electrochemical cell (12) is characterized by the steps of thermal spraying stabilized zirconia over a doped lanthanum manganite air electrode tube (14) to provide an electrolyte layer (15), coating conductive particles over the electrolyte, pressurizing the outside of the electrolyte layer, feeding halide vapors of yttrium and zirconium to the outside of the electrolyte layer and feeding a source of oxygen to the inside of the electrolyte layer, heating to cause oxygen reaction with the halide vapors to close electrolyte pores if there are any and to form a metal oxide coating on and between the particles and provide a fuel electrode (16).

  14. Phase stability of zirconium oxide films during focused ion beam milling

    NASA Astrophysics Data System (ADS)

    Baxter, Felicity; Garner, Alistair; Topping, Matthew; Hulme, Helen; Preuss, Michael; Frankel, Philipp

    2018-06-01

    Focused ion beam (FIB) is a widely used technique for preparation of electron transparent samples and so it is vital to understand the potential for introduction of FIB-induced microstructural artefacts. The bombardment of both Xe+ and Ga+ ions is observed to cause extensive monoclinic to tetragonal phase transformation in ZrO2 corrosion films, however, this effect is diminished with reduced energy and is not observed below 5 KeV. This study emphasises the importance of careful FIB sample preparation with a low energy cleaning step, and also gives insight into the stabilisation mechanism of the tetragonal phase during oxidation.

  15. Phase formation during the carbothermic reduction of eudialyte concentrate

    NASA Astrophysics Data System (ADS)

    Krasikov, S. A.; Upolovnikova, A. G.; Sitnikova, O. A.; Ponomarenko, A. A.; Agafonov, S. N.; Zhidovinova, S. V.; Maiorov, D. V.

    2013-07-01

    The phase transformations of eudialyte concentrate during the carbothermic reduction in the temperature range 25-2000°C are studied by thermodynamic simulation, differential thermal analysis, and X-ray diffraction. As the temperature increases to 1500°C, the following phases are found to form sequentially: iron and manganese carbides, free iron, niobium carbide, iron silicides, silicon and titanium carbides, and free silicon. Strontium, yttrium, and uranium in the temperature range under study are not reduced and are retained in an oxide form, and insignificant reduction of zirconium oxides with the formation of carbide ZrC is possible only at temperatures above 1500°C.

  16. Scaling behavior of fully spin-coated TFT

    NASA Astrophysics Data System (ADS)

    Mondal, Sandip; Kumar, Arvind; Rao, K. S. R. Koteswara; Venkataraman, V.

    2017-05-01

    We studied channel scaling behavior of fully spin coated, low temperature solution processed thin film transistor (TFT) fabricated on p++ - Si (˜1021 cm-3) as bottom gate. The solution processed, spin coated 40 nm thick amorphous Indium Gallium Zinc Oxide (a-IGZO) and 50 nm thick amorphous zirconium di-oxide (a-ZrO2) has been used as channel and low leakage dielectric at 350°C respectively. The channel scaling effect of the TFT with different width/length ratio (W/L= 2.5, 5 and 15) for same channel length (L = 10 μm) has been demonstrated. The lowest threshold voltage (Vth) is 6.25 V for the W/L=50/10. The maximum field effect mobility (μFE) has been found to be 0.123 cm2/Vs from W/L of 50/10 with the drain to source voltage (VD) of 10V and 20V gate to source voltage (VG). We also demonstrated that there is no contact resistance effect on the mobility of the fully sol-gel spin coated TFT.

  17. Decay properties and reaction dynamics of zirconium isotopes in the relativistic mean-field model

    NASA Astrophysics Data System (ADS)

    Panigrahi, M.; Panda, R. N.; Kumar, Bharat; Patra, S. K.

    In the framework of relativistic mean-field theory, the ground state properties like binding energy, charge radius and quadrupole deformation parameter for various isotopes of zirconium from the valley of stability to drip-line region have been studied. The results are compared with the experimental data and we found reasonable agreement. The calculations are carried out for β-decay energy and β-decay half-life up to the drip-line. Total reaction and elastic differential cross-sections are also studied for few zirconium isotopes as projectiles with 12C as target, using different parameter sets namely NL3*, DD-ME2 and DD-PC1 in conjunction with Glauber model.

  18. Luminescent properties of ZrO2:Tb nanoparticles for applications in neuroscience

    NASA Astrophysics Data System (ADS)

    Słońska, A.; Kaszewski, J.; Wolska-Kornio, E.; Witkowski, B.; Wachnicki, Ł.; Mijowska, E.; Karakitsou, V.; Gajewski, Z.; Godlewski, M.; Godlewski, M. M.

    2016-09-01

    In this paper a new generation of non-toxic nanoparticles based on the zirconium oxide doped with 0.5%Tb and co-doped by the range of 0-70% with Y was evaluated for the use as a fluorescent biomarker of neuronal trafficking. The ZrO2:Tb nanoparticles were created by microwave driven hydrothermal method. Influence of the yttrium content and thermal processing on the Tb3+ related luminescence emission was discussed. The higher intensities were achieved, when host was cubic and for the nanoparticles with 33 nm. Presence of yttrium was associated with the energy coupling of the host and dopant, wide excitation band is present at 309 and 322 nm before and after calcination respectively.

  19. Parametric and experimentally informed BWR Severe Accident Analysis Utilizing FeCrAl - M3FT-17OR020205041

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

    Ott, Larry J.; Howell, Michael; Robb, Kevin R.

    Iron-chromium-aluminum (FeCrAl) alloys are being considered as advanced fuel cladding concepts with enhanced accident tolerance. At high temperatures, FeCrAl alloys have slower oxidation kinetics and higher strength compared with zirconium-based alloys. FeCrAl could be used for fuel cladding and spacer or mixing vane grids in light water reactors and/or as channel box material in boiling water reactors (BWRs). There is a need to assess the potential gains afforded by the FeCrAl accident-tolerant-fuel (ATF) concept over the existing zirconium-based materials employed today. To accurately assess the response of FeCrAl alloys under severe accident conditions, a number of FeCrAl properties and characteristicsmore » are required. These include thermophysical properties as well as burst characteristics, oxidation kinetics, possible eutectic interactions, and failure temperatures. These properties can vary among different FeCrAl alloys. Oak Ridge National Laboratory has pursued refined values for the oxidation kinetics of the B136Y FeCrAl alloy (Fe-13Cr-6Al wt %). This investigation included oxidation tests with varying heating rates and end-point temperatures in a steam environment. The rate constant for the low-temperature oxidation kinetics was found to be higher than that for the commercial APMT FeCrAl alloy (Fe-21Cr-5Al-3Mo wt %). Compared with APMT, a 5 times higher rate constant best predicted the entire dataset (root mean square deviation). Based on tests following heating rates comparable with those the cladding would experience during a station blackout, the transition to higher oxidation kinetics occurs at approximately 1,500°C. A parametric study varying the low-temperature FeCrAl oxidation kinetics was conducted for a BWR plant using FeCrAl fuel cladding and channel boxes using the MELCOR code. A range of station blackout severe accident scenarios were simulated for a BWR/4 reactor with Mark I containment. Increasing the FeCrAl low-temperature oxidation rate constant (3 times and 10 times that of the rate constant for APMT) had a negligible impact on the early stages of the accident and minor impacts on the accident progression after the first relocation of the fuel. At temperatures below 1,500°C, increasing the rate constant for APMT by a factor of 10 still resulted in only minor FeCrAl oxidation. In general, the gains afforded by the FeCrAl enhanced ATF concept with respect to accident sequence timing and combustible gas generation are consistent with previous efforts. Compared with the traditional Zircaloy-based cladding and channel box system, the FeCrAl concept could provide a few extra hours of time for operators to take mitigating actions and/or for evacuations to take place. A coolable core geometry is retained longer, enhancing the ability to stabilize an accident. For example, a station blackout was simulated in which cooling water injection was lost 36 hours after shutdown. The timing to first fuel relocation was delayed by approximately 5 h for the FeCrAl ATF concept compared with that of the traditional Zircaloy-based cladding and channel box system.« less

  20. Results of NDE Technique Evaluation of Clad Hydrides

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

    Kunerth, Dennis C.

    2014-09-01

    This report fulfills the M4 milestone, M4FT-14IN0805023, Results of NDE Technique Evaluation of Clad Hydrides, under Work Package Number FT-14IN080502. During service, zirconium alloy fuel cladding will degrade via corrosion/oxidation. Hydrogen, a byproduct of the oxidation process, will be absorbed into the cladding and eventually form hydrides due to low hydrogen solubility limits. The hydride phase is detrimental to the mechanical properties of the cladding and therefore it is important to be able to detect and characterize the presence of this constituent within the cladding. Presently, hydrides are evaluated using destructive examination. If nondestructive evaluation techniques can be used tomore » detect and characterize the hydrides, the potential exists to significantly increase test sample coverage while reducing evaluation time and cost. To demonstrate the viability this approach, an initial evaluation of eddy current and ultrasonic techniques were performed to demonstrate the basic ability to these techniques to detect hydrides or their effects on the microstructure. Conventional continuous wave eddy current techniques were applied to zirconium based cladding test samples thermally processed with hydrogen gas to promote the absorption of hydrogen and subsequent formation of hydrides. The results of the evaluation demonstrate that eddy current inspection approaches have the potential to detect both the physical damage induced by hydrides, e.g. blisters and cracking, as well as the combined effects of absorbed hydrogen and hydride precipitates on the electrical properties of the zirconium alloy. Similarly, measurements of ultrasonic wave velocities indicate changes in the elastic properties resulting from the combined effects of absorbed hydrogen and hydride precipitates as well as changes in geometry in regions of severe degradation. However, for both approaches, the signal responses intended to make the desired measurement incorporate a number of contributing parameters. These contributing factors need to be recognized and a means to control them or separate their contributions will be required to obtain the desired information.« less

  1. 6-Peroxo-6-zirconium crown and its hafnium analogue embedded in a triangular polyanion: [M6(O2)6(OH)6(gamma-SiW10O36)3]18- (M = Zr, Hf).

    PubMed

    Bassil, Bassem S; Mal, Sib Sankar; Dickman, Michael H; Kortz, Ulrich; Oelrich, Holger; Walder, Lorenz

    2008-05-28

    We have synthesized and structurally characterized the unprecedented peroxo-zirconium(IV) containing [Zr6(O2)6(OH)6(gamma-SiW10O36)3]18- (1). Polyanion 1 comprises a cyclic 6-peroxo-6-zirconium core stabilized by three decatungstosilicate units. We have also prepared the isostructural hafnium(IV) analogue [Hf6(O2)6(OH)6(gamma-SiW10O36)3]18- (2). We investigated the acid/base and redox properties of 1 by UV-vis spectroscopy and electrochemistry studies. Polyanion 1 represents the first structurally characterized Zr-peroxo POM with side-on, bridging peroxo units. The simple, one-pot synthesis of 1 and 2 involving dropwise addition of aqueous hydrogen peroxide could represent a general procedure for incorporating peroxo groups into a large variety of transition metal and lanthanide containing POMs.

  2. Isolating Gas Sensor From Pressure And Temperature Effects

    NASA Technical Reports Server (NTRS)

    Sprinkle, Danny R.; Chen, Tony T. D.; Chaturvedi, Sushi K.

    1994-01-01

    Two-stage flow system enables oxygen sensor in system to measure oxygen content of low-pressure, possibly-high-temperature atmosphere in test environment while protecting sensor against possibly high temperature and fluctuations in pressure of atmosphere. Sensor for which flow system designed is zirconium oxide oxygen sensor sampling atmospheres in high-temperature wind tunnels. Also adapted to other gas-analysis instruments that must be isolated from pressure and temperature effects of test environments.

  3. A mild and efficient flow procedure for the transfer hydrogenation of ketones and aldehydes using hydrous zirconia.

    PubMed

    Battilocchio, Claudio; Hawkins, Joel M; Ley, Steven V

    2013-05-03

    A flow chemistry Meerwein-Ponndorf-Verley (MPV) reduction procedure using partially hydrated zirconium oxide via a machine-assisted approach is reported. The heterogeneous reductive system could be applied to a wide range of functionalized substrates, allowing clean and fast delivery of the alcohol products within a few minutes (6-75 min). In three examples the system was scaled to deliver 50 mmol of product.

  4. 40 CFR 721.9973 - Zirconium dichlorides (generic).

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Zirconium dichlorides (generic). 721... Substances § 721.9973 Zirconium dichlorides (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as zirconium dichlorides (PMNs P...

  5. 40 CFR 471.93 - New source performance standards (NSPS).

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... monthly average mg/off-kg (pounds per million off-pounds) of zirconium-hafnium extruded Chromium 0.104 0... monthly average mg/off-kg (pounds per million off-pounds) of zirconium-hafnium heat treated Chromium 0.015... Chromium 0.150 0.061 Cyanide 0.099 0.041 Nickel 0.653 0.432 Ammonia 45.3 20.0 Fluoride 20.0 8.98 Oil and...

  6. 40 CFR 471.93 - New source performance standards (NSPS).

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... monthly average mg/off-kg (pounds per million off-pounds) of zirconium-hafnium extruded Chromium 0.104 0... monthly average mg/off-kg (pounds per million off-pounds) of zirconium-hafnium heat treated Chromium 0.015... Chromium 0.150 0.061 Cyanide 0.099 0.041 Nickel 0.653 0.432 Ammonia 45.3 20.0 Fluoride 20.0 8.98 Oil and...

  7. 40 CFR 421.336 - Pretreatment standards for new sources.

    Code of Federal Regulations, 2013 CFR

    2013-07-01

    ....000 499.500 (d) SiCl4 purification wet air pollution control. PSNS for the Primary Zirconium and....262 Lead 4.416 2.050 Nickel 8.674 5.835 Ammonia (as N) 2,102.000 895.800 (q) Leaching rinse water from... Nickel 32.410 21.810 Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy...

  8. 40 CFR 421.336 - Pretreatment standards for new sources.

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ....000 499.500 (d) SiCl4 purification wet air pollution control. PSNS for the Primary Zirconium and....262 Lead 4.416 2.050 Nickel 8.674 5.835 Ammonia (as N) 2,102.000 895.800 (q) Leaching rinse water from... Nickel 32.410 21.810 Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy...

  9. 40 CFR 421.336 - Pretreatment standards for new sources.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ....000 499.500 (d) SiCl4 purification wet air pollution control. PSNS for the Primary Zirconium and....262 Lead 4.416 2.050 Nickel 8.674 5.835 Ammonia (as N) 2,102.000 895.800 (q) Leaching rinse water from... Nickel 32.410 21.810 Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy...

  10. 40 CFR 421.336 - Pretreatment standards for new sources.

    Code of Federal Regulations, 2014 CFR

    2014-07-01

    ....000 499.500 (d) SiCl4 purification wet air pollution control. PSNS for the Primary Zirconium and....262 Lead 4.416 2.050 Nickel 8.674 5.835 Ammonia (as N) 2,102.000 895.800 (q) Leaching rinse water from... Nickel 32.410 21.810 Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy...

  11. 40 CFR 421.336 - Pretreatment standards for new sources.

    Code of Federal Regulations, 2012 CFR

    2012-07-01

    ....000 499.500 (d) SiCl4 purification wet air pollution control. PSNS for the Primary Zirconium and....262 Lead 4.416 2.050 Nickel 8.674 5.835 Ammonia (as N) 2,102.000 895.800 (q) Leaching rinse water from... Nickel 32.410 21.810 Ammonia (as N) 7,856.000 3,453.000 (r) Leaching rinse water from zirconium alloy...

  12. Nuclear-grade zirconium prepared by combining combustion synthesis with molten-salt electrorefining technique

    NASA Astrophysics Data System (ADS)

    Li, Hui; Nersisyan, Hayk H.; Park, Kyung-Tae; Park, Sung-Bin; Kim, Jeong-Guk; Lee, Jeong-Min; Lee, Jong-Hyeon

    2011-06-01

    Zirconium has a low absorption cross-section for neutrons, which makes it an ideal material for use in nuclear reactor applications. However, hafnium typically contained in zirconium causes it to be far less useful for nuclear reactor materials because of its high neutron-absorbing properties. In the present study, a novel effective method has been developed for the production of hafnium-free zirconium. The process includes two main stages: magnesio-thermic reduction of ZrSiO 4 under a combustion mode, to produce zirconium silicide (ZrSi), and recovery of hafnium-free zirconium by molten-salt electrorefining. It was found that, depending on the electrorefining procedure, it is possible to produce zirconium powder with a low hafnium content: 70 ppm, determined by ICP-AES analysis.

  13. Properties of Tricalcium Silicate Sealers.

    PubMed

    Khalil, Issam; Naaman, Alfred; Camilleri, Josette

    2016-10-01

    Sealers based on tricalcium silicate cement aim at an interaction of the sealer with the root canal wall, alkalinity with potential antimicrobial activity, and the ability to set in a wet field. The aim of this study was to characterize and investigate the properties of a new tricalcium silicate-based sealer and verify its compliance to ISO 6876 (2012). A new tricalcium silicate-based sealer (Bio MM; St Joseph University, Beirut, Lebanon), BioRoot RCS (Septodont, St Maure de Fosses, France), and AH Plus (Dentsply, DeTrey, Konstanz, Germany) were investigated. Characterization using scanning electron microscopy, energy-dispersive spectroscopy, and X-ray diffraction analysis was performed. Furthermore, sealer setting time, flow, film thickness, and radiopacity were performed following ISO specifications. pH and ion leaching in solution were assessed by pH analysis and inductively coupled plasma. Bio MM and BioRoot RCS were both composed of tricalcium silicate and tantalum oxide in Bio MM and zirconium oxide in BioRoot RCS. In addition, the Bio MM contained calcium carbonate and a phosphate phase. The inorganic components of AH Plus were calcium tungstate and zirconium oxide. AH Plus complied with the ISO norms for both flow and film thickness. BioRoot RCS and Bio MM exhibited a lower flow and a higher film thickness than that specified for sealer cements in ISO 6876. All test sealers exhibited adequate radiopacity. Bio MM interacted with physiologic solution, thus showing potential for bioactivity. Sealer properties were acceptable and comparable with other sealers available clinically. Copyright © 2016 American Association of Endodontists. Published by Elsevier Inc. All rights reserved.

  14. 40 CFR 471.90 - Applicability; description of the zirconium-hafnium forming subcategory.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... zirconium-hafnium forming subcategory. 471.90 Section 471.90 Protection of Environment ENVIRONMENTAL... POINT SOURCE CATEGORY Zirconium-Hafnium Forming Subcategory § 471.90 Applicability; description of the zirconium-hafnium forming subcategory. This subpart applies to discharges of pollutants to waters of the...

  15. 40 CFR 421.330 - Applicability: Description of the primary zirconium and hafnium subcategory.

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... primary zirconium and hafnium subcategory. 421.330 Section 421.330 Protection of Environment ENVIRONMENTAL... CATEGORY Primary Zirconium and Hafnium Subcategory § 421.330 Applicability: Description of the primary zirconium and hafnium subcategory. The provisions of this subpart are applicable to discharges resulting...

  16. Ablation Resistant Zirconium and Hafnium Ceramics

    NASA Technical Reports Server (NTRS)

    Bull, Jeffrey (Inventor); White, Michael J. (Inventor); Kaufman, Larry (Inventor)

    1998-01-01

    High temperature ablation resistant ceramic composites have been made. These ceramics are composites of zirconium diboride and zirconium carbide with silicon carbide, hafnium diboride and hafnium carbide with silicon carbide and ceramic composites which contain mixed diborides and/or carbides of zirconium and hafnium. along with silicon carbide.

  17. 40 CFR 721.10089 - Modified salicylic acid, zirconium complex (generic).

    Code of Federal Regulations, 2011 CFR

    2011-07-01

    ... 40 Protection of Environment 31 2011-07-01 2011-07-01 false Modified salicylic acid, zirconium... Specific Chemical Substances § 721.10089 Modified salicylic acid, zirconium complex (generic). (a) Chemical... as modified salicylic acid, zirconium complex (PMN P-00-552) is subject to reporting under this...

  18. 40 CFR 721.10089 - Modified salicylic acid, zirconium complex (generic).

    Code of Federal Regulations, 2010 CFR

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Modified salicylic acid, zirconium... Specific Chemical Substances § 721.10089 Modified salicylic acid, zirconium complex (generic). (a) Chemical... as modified salicylic acid, zirconium complex (PMN P-00-552) is subject to reporting under this...

  19. CONTINUOUS CHELATION-EXTRACTION PROCESS FOR THE SEPARATION AND PURIFICATION OF METALS

    DOEpatents

    Thomas, J.R.; Hicks, T.E.; Rubin, B.; Crandall, H.W.

    1959-12-01

    A continuous process is presented for separating metal values and groups of metal values from each other. A complex mixture. e.g., neutron-irradiated uranium, can be resolved into component parts. In the present process the values are dissolved in an acidic solution and adjusted to the proper oxidation state. Thenceforth the solution is contacted with an extractant phase comprising a fluorinated beta -diketone in an organic solvent under centain pH conditions whereupon plutonium and zirconium are extracted. Plutonium is extracted from the foregoing extract with reducing aqueous solutions or under specified acidic conditions and can be recovered from the aqueous solution. Zirconium is then removed with an oxalic acid aqueous phase. The uranium is recovered from the residual original solution using hexone and hexone-diketone extractants leaving residual fission products in the original solution. The uranium is extracted from the hexone solution with dilute nitric acid. Improved separations and purifications are achieved using recycled scrub solutions and the "self-salting" effect of uranyl ions.

  20. Refractory metal joining for first wall applications

    NASA Astrophysics Data System (ADS)

    Cadden, C. H.; Odegard, B. C.

    2000-12-01

    The potential use of high temperature coolant (e.g. 900°C He) in first wall structures would preclude the applicability of copper alloy heat sink materials and refractory metals would be potential replacements. Brazing trials were conducted in order to examine techniques to join tungsten armor to high tungsten (90-95 wt%) or molybdenum TZM heat sink materials. Palladium-, nickel- and zirconium-based filler metals were investigated using brazing temperatures ranging from 1000°C to 1275°C. Palladium-nickel and palladium-cobalt braze alloys were successful in producing generally sound metallurgical joints in tungsten alloy/tungsten couples, although there was an observed tendency for the pure tungsten armor material to exhibit grain boundary cracking after bonding. The zirconium- and nickel-based filler metals produced defect-containing joints, specifically cracking and porosity, respectively. The palladium-nickel braze alloy produced sound joints in the Mo TZM/tungsten couple. Substitution of a lanthanum oxide-containing, fine-grained tungsten material (for the pure tungsten) eliminated the observed tungsten grain boundary cracking.

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