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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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

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.

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).

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.

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.

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.

Multilayered thermal insulation formed of zirconia bonded layers of zirconia fibers and metal oxide fibers and method for making same

DOEpatents

Wrenn, Jr., George E.; Holcombe, Jr., Cressie E.

1988-01-01

A multilayered thermal insulating composite is formed of a first layer of zirconia-bonded zirconia fibers for utilization near the hot phase or surface of a furnace or the like. A second layer of zirconia-bonded metal oxide fibers is attached to the zirconia fiber layer by a transition layer formed of intermingled zirconia fibers and metal oxide fibers. The thermal insulation is fabricated by vacuum molding with the layers being sequentially applied from aqueous solutions containing the fibers to a configured mandrel. A portion of the solution containing the fibers forming the first layer is intermixed with the solution containing the fibers of the second layer for forming the layer of mixed fibers. The two layers of fibers joined together by the transition layer are saturated with a solution of zirconium oxynitrate which provides a zirconia matrix for the composite when the fibers are sintered together at their nexi.

Multilayered thermal insulation formed of zirconia bonded layers of zirconia fibers and metal oxide fibers and method for making same

DOEpatents

Wrenn, G.E. Jr.; Holcombe, C.E. Jr.

1988-09-13

A multilayered thermal insulating composite is formed of a first layer of zirconia-bonded zirconia fibers for utilization near the hot phase or surface of a furnace or the like. A second layer of zirconia-bonded metal oxide fibers is attached to the zirconia fiber layer by a transition layer formed of intermingled zirconia fibers and metal oxide fibers. The thermal insulation is fabricated by vacuum molding with the layers being sequentially applied from aqueous solutions containing the fibers to a configured mandrel. A portion of the solution containing the fibers forming the first layer is intermixed with the solution containing the fibers of the second layer for forming the layer of mixed fibers. The two layers of fibers joined together by the transition layer are saturated with a solution of zirconium oxynitrate which provides a zirconia matrix for the composite when the fibers are sintered together at their nexi.

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.

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.

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%.

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.

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.

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.

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.

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.

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.

Lift-off process for fine-patterned PZT film using metal oxide as a sacrificial layer

NASA Astrophysics Data System (ADS)

Trong Tue, Phan; Shimoda, Tatsuya; Takamura, Yuzuru

2017-01-01

Patterning of lead zirconium titanate (PZT) films is crucial for highly integrated piezoelectric/ferroelectric micro-devices. In this work, we report a novel lift-off method using solution-processed indium zinc oxide (IZO) thin film as a sacrificial layer for sub-5 µm fine-patterning PZT film. The processes include IZO layer deposition and patterning, PZT film preparation, and final lift-off. The results reveal that the lift-off PZT processes provide better structural and electrical properties than those formed by the conventional wet-etching method. The successful patterning by the lift-off was mainly due to the fact that the IZO sacrificial layer is easy to etch and has a high-temperature resistance. This finding shows great promise for highly integrated electronic devices.

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...

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...

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

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.

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.

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

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

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.

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

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...

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...

Characteristic of skin formation using zircon- and graphite-coated mold in thin wall ductile iron fabrication

NASA Astrophysics Data System (ADS)

Dhaneswara, Donanta; Suharno, Bambang; Nugroho, Janu Ageng; Ariobimo, Rianti Dewi S.; Sofyan, Nofrijon

2017-03-01

One of the problems in thin wall ductile iron (TWDI) fabrication is skin formation during the casting. The presence of this skin will decrease strength and strain of the TWDI. One of the ways to control this skin formation is to change the cooling rate during the process through a mold coating. In testing the effectiveness of skin prevention, the following variables were used for the mold coating i.e. (i) graphite: (ii) zirconium; and (iii) double layer of graphite-zirconium. After the process, the plates were characterized by non-etching, etching, tensile test, and SEM observation. The results showed that the average skin formation using graphite: 65 µm; zirconium: 13.04 µm; and double layer of graphite-zirconium: 33.25 µm. It seems that zirconium has the most effect on the skin prevention due to sulfur binding and magnesium locked, which then prevented rapid cooling resulting in less skin formation. The results also showed the number of nodules obtained in specimen with graphite: 703 nodules/mm2 with average diameter of 12.57 µm, zirconium: 798 nodules/mm2 with average diameter of 12.15 µm, and double layer of graphite-zirconium: 697 nodules/mm2 with average diameter of 11.9 µm and nodularity percentage of 82.58%, 84.53%, and 84.22%, respectively. Tensile test showed that the strength of the specimen with graphite is 301.1 MPa, with zirconium is 388.8 MPa, and with double layer of graphite-zirconium is 304 MPa. In overall, zirconium give the best performance on the skin formation prevention in TWDI fabrication.

Effects of compositional changes on the performance of a thermal barrier coating system. [yttria-stabilized zirconia coatings on gas turbine engine blades

NASA Technical Reports Server (NTRS)

Stecura, S.

1978-01-01

Currently proposed thermal barrier systems for aircraft gas turbine engines consist of NiCrAlY bond coating covered with an insulating oxide layer of yttria-stabilized zirconia. The effect of yttrium concentration (from 0.15 to 1.08 w/o) in the bond coating and the yttria concentration (4 to 24.4 w/o) in the oxide layer were evaluated. Furnace, natural gas-oxygen torch, and Mach 1.0 burner rig cyclic tests on solid specimens and air-cooled blades were used to identify trends in coating behavior. Results indicate that the combinations of yttrium levels between 0.15 - 0.35 w/o in the bond coating and the yttria concentration between 6 - 8 w/o in the zirconium oxide layer were the most adherent and resistant to high temperature cyclic exposure.

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.

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.

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.

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.

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.

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

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...

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

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.

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.

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.

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).

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.

Thermochemical Compatibility and Oxidation Resistance of Advanced LWR Fuel Cladding

DOE PAGES

Besmann, T. M.; Yamamoto, Y.; Unocic, K. A.

2016-06-21

We assessed the thermochemical compatibility of potential replacement cladding materials for zirconium alloys in light water reactors. Considered were FeCrAl steel (similar to Kanthal APMT), Nb-1%Zr (similar to PWC-11), and a hybrid SiC-composite with a metallic barrier layer. The niobium alloy was also seen as requiring an oxidation protective layer, and a diffusion silicide was investigated. Metallic barrier layers for the SiC-composite reviewed included a FeCrAl alloy, Nb-1%Zr, and chromium. Thermochemical calculations were performed to determine oxidation behavior of the materials in steam, and for hybrid SiC-composites possible interactions between the metallic layer and SiC. Additionally, experimental exposures of SiC-alloymore » reaction couples at 673K, 1073K, and 1273K for 168 h in an inert atmosphere were made and microanalysis performed. Whereas all materials were determined to oxidize under higher oxygen partial pressures in the steam environment, these varied by material with expected protective oxides forming. Finally, the computed and experimental results indicate the formation of liquid phase eutectic in the FeCrAl-SiC system at the higher temperatures.« less

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

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

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.

Perform Tests and Document Results and Analysis of Oxide Layer Effects and Comparisons

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

Collins, E. D.; DelCul, G. D.; Spencer, B. B.

2014-08-30

During the initial feasibility test using actual used nuclear fuel (UNF) cladding in FY 2012, an incubation period of 30–45 minutes was observed in the initial dry chlorination. The cladding hull used in the test had been previously oxidized in a dry air oxidation pretreatment prior to removal of the fuel. The cause of this incubation period was attributed to the resistance to chlorination of an oxide layer imparted by the dry oxidation pretreatment on the cladding. Subsequently in 2013, researchers at the Korea Atomic Energy Institute (KAERI) reported on their chlorination study [R1] on ~9-gram samples of unirradiated ZirloTMmore » cladding tubes that had been previously oxidized in air at 500oC for various time periods to impart oxide layers of varying thickness. In early 2014, discussions with Indefinite Delivery, Indefinite Quantity (IDIQ) contracted technical consultants from Westinghouse described their previous development (and patents) [R2] on methods of chemical washing to remove some or all of the hydrous oxide layer imparted on UNF cladding during irradiation in light water reactors (LWRs) . Thus, the Oak Ridge National Laboratory (ORNL) study, described herein, was planned to extend the KAERI study on the effects of anhydrous oxide layers, but on larger ~100-gram samples of unirradiated zirconium alloy cladding tubes, and to investigate the effects of various methods of chemical pretreatment prior to chlorination with 100% chlorine on the average reaction rates and Cl2 usage efficiencies.« less

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

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.

High-rate/high-temperature capability of a single-layer zicar-separator nickel-hydrogen cell

NASA Technical Reports Server (NTRS)

Wheeler, James R.

1995-01-01

A 50 Ampere-hour nickel-hydrogen cell with a single-layer Zircar separator stack design was fully charged and then discharged at a 2C current rate to an end voltage of 1 volt. This extreme test resulted in high temperatures which were recorded at three locations on the cell, i.e., the cell wall, the boss (barrel of the compression seal), and a terminal. The results provide new information about the high-temperature and high-discharge-rate capabilities of nickel-hydrogen cells. This information also adds to the growing data base for single-layer zirconium-oxide-cloth (Zircar) separator cell designs.

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.

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

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

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

Steering the Properties of MoOx Hole Transporting Layers in OPVs and OLEDs: Interface Morphology vs. Electronic Structure

PubMed Central

Marchal, Wouter; Verboven, Inge; Kesters, Jurgen; Moeremans, Boaz; De Dobbelaere, Christopher; Bonneux, Gilles; Elen, Ken; Conings, Bert; Maes, Wouter; Boyen, Hans Gerd; Deferme, Wim; Van Bael, Marlies; Hardy, An

2017-01-01

The identification, fine-tuning, and process optimization of appropriate hole transporting layers (HTLs) for organic solar cells is indispensable for the production of efficient and sustainable functional devices. In this study, the optimization of a solution-processed molybdenum oxide (MoOx) layer fabricated from a combustion precursor is carried out via the introduction of zirconium and tin additives. The evaluation of the output characteristics of both organic photovoltaic (OPV) and organic light emitting diode (OLED) devices demonstrates the beneficial influence upon the addition of the Zr and Sn ions compared to the generic MoOx precursor. A dopant effect in which the heteroatoms and the molybdenum oxide form a chemical identity with fundamentally different structural properties could not be observed, as the additives do not affect the molybdenum oxide composition or electronic band structure. An improved surface roughness due to a reduced crystallinity was found to be a key parameter leading to the superior performance of the devices employing modified HTLs. PMID:28772483

Steering the Properties of MoOx Hole Transporting Layers in OPVs and OLEDs: Interface Morphology vs. Electronic Structure.

PubMed

Marchal, Wouter; Verboven, Inge; Kesters, Jurgen; Moeremans, Boaz; De Dobbelaere, Christopher; Bonneux, Gilles; Elen, Ken; Conings, Bert; Maes, Wouter; Boyen, Hans Gerd; Deferme, Wim; Van Bael, Marlies; Hardy, An

2017-01-30

The identification, fine-tuning, and process optimization of appropriate hole transporting layers (HTLs) for organic solar cells is indispensable for the production of efficient and sustainable functional devices. In this study, the optimization of a solution-processed molybdenum oxide (MoOx) layer fabricated from a combustion precursor is carried out via the introduction of zirconium and tin additives. The evaluation of the output characteristics of both organic photovoltaic (OPV) and organic light emitting diode (OLED) devices demonstrates the beneficial influence upon the addition of the Zr and Sn ions compared to the generic MoOx precursor. A dopant effect in which the heteroatoms and the molybdenum oxide form a chemical identity with fundamentally different structural properties could not be observed, as the additives do not affect the molybdenum oxide composition or electronic band structure. An improved surface roughness due to a reduced crystallinity was found to be a key parameter leading to the superior performance of the devices employing modified HTLs.

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.

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.

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.

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

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.).

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.

Influence of surface contamination on the wettability of heat transfer surfaces

DOE PAGES

Forrest, Eric Christopher; Schulze, Roland; Liu, Cheng; ...

2015-08-08

In this study, the wettability of heat transfer surfaces plays an important role in liquid–vapor phase change phenomena, including boiling incipience, the critical heat flux, the Leidenfrost transition, and condensation. The influence of adsorbed surface contamination at the nanoscale, though seldom considered, can have a profound impact on wetting behavior. This study quantitatively investigates the impact of contaminant layer thickness on wettability. Various cleaning treatments are explored on zirconium and 6061 aluminum to determine the effect on contaminant and oxide layer thickness. Angle-resolved X-ray photoelectron spectroscopy can be used to measure the thickness of oxide and contaminant layers, which ismore » then correlated to wettability by measuring the equilibrium contact angle. Results indicate that even after solvent cleaning, the contact angle of water on practical heat transfer surfaces is dominated by a hydrocarbon contaminant overlayer around five nanometers thick.« less

Influence of surface contamination on the wettability of heat transfer surfaces

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

Forrest, Eric Christopher; Schulze, Roland; Liu, Cheng

In this study, the wettability of heat transfer surfaces plays an important role in liquid–vapor phase change phenomena, including boiling incipience, the critical heat flux, the Leidenfrost transition, and condensation. The influence of adsorbed surface contamination at the nanoscale, though seldom considered, can have a profound impact on wetting behavior. This study quantitatively investigates the impact of contaminant layer thickness on wettability. Various cleaning treatments are explored on zirconium and 6061 aluminum to determine the effect on contaminant and oxide layer thickness. Angle-resolved X-ray photoelectron spectroscopy can be used to measure the thickness of oxide and contaminant layers, which ismore » then correlated to wettability by measuring the equilibrium contact angle. Results indicate that even after solvent cleaning, the contact angle of water on practical heat transfer surfaces is dominated by a hydrocarbon contaminant overlayer around five nanometers thick.« less

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.

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

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.

Direct nanopatterning of 100 nm metal oxide periodic structures by Deep-UV immersion lithography.

PubMed

Stehlin, Fabrice; Bourgin, Yannick; Spangenberg, Arnaud; Jourlin, Yves; Parriaux, Olivier; Reynaud, Stéphanie; Wieder, Fernand; Soppera, Olivier

2012-11-15

Deep-UV lithography using high-efficiency phase mask has been developed to print 100 nm period grating on sol-gel based thin layer. High efficiency phase mask has been designed to produce a high-contrast interferogram (periodic fringes) under water immersion conditions for 244 nm laser. The demonstration has been applied to a new developed immersion-compatible sol-gel layer. A sol-gel photoresist prepared from zirconium alkoxides caped with methacrylic acids was developed to achieve 50 nm resolution in a single step exposure. The nanostructures can be thermally annealed into ZrO(2). Such route considerably simplifies the process for elaborating nanopatterned surfaces of transition metal oxides, and opens new routes for integrating materials of interest for applications in the field of photocatalysis, photovoltaic, optics, photonics or microelectronics.

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

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

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.

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.

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.

Process for the deposition of high temperature stress and oxidation resistant coatings on silicon-based substrates

DOEpatents

Sarin, V.K.

1991-07-30

A process is disclosed for depositing a high temperature stress and oxidation resistant coating on a silicon nitride- or silicon carbide-based substrate body. A gas mixture is passed over the substrate at about 900--1500 C and about 1 torr to about ambient pressure. The gas mixture includes one or more halide vapors with other suitable reactant gases. The partial pressure ratios, flow rates, and process times are sufficient to deposit a continuous, fully dense, adherent coating. The halide and other reactant gases are gradually varied during deposition so that the coating is a graded coating of at least two layers. Each layer is a graded layer changing in composition from the material over which it is deposited to the material of the layer and further to the material, if any, deposited thereon, so that no clearly defined compositional interfaces exist. The gases and their partial pressures are varied according to a predetermined time schedule and the halide and other reactant gases are selected so that the layers include (a) an adherent, continuous intermediate layer about 0.5-20 microns thick of an aluminum nitride or an aluminum oxynitride material, over and chemically bonded to the substrate body, and (b) an adherent, continuous first outer layer about 0.5-900 microns thick including an oxide of aluminum or zirconium over and chemically bonded to the intermediate layer.

Process for the deposition of high temperature stress and oxidation resistant coatings on silicon-based substrates

DOEpatents

Sarin, Vinod K.

1991-01-01

A process for depositing a high temperature stress and oxidation resistant coating on a silicon nitride- or silicon carbide-based substrate body. A gas mixture is passed over the substrate at about 900.degree.-1500.degree. C. and about 1 torr to about ambient pressure. The gas mixture includes one or more halide vapors with other suitable reactant gases. The partial pressure ratios, flow rates, and process times are sufficient to deposit a continuous, fully dense, adherent coating. The halide and other reactant gases are gradually varied during deposition so that the coating is a graded coating of at least two layers. Each layer is a graded layer changing in composition from the material over which it is deposited to the material of the layer and further to the material, if any, deposited thereon, so that no clearly defined compositional interfaces exist. The gases and their partial pressures are varied according to a predetermined time schedule and the halide and other reactant gases are selected so that the layers include (a) an adherent, continuous intermediate layer about 0.5-20 microns thick of an aluminum nitride or an aluminum oxynitride material, over and chemically bonded to the substrate body, and (b) an adherent, continuous first outer layer about 0.5-900 microns thick including an oxide of aluminum or zirconium over and chemically bonded to the intermediate layer.

Some metal oxides and their applications for creation of Microsystems (MEMS) and Energy Harvesting Devices (EHD)

NASA Astrophysics Data System (ADS)

Denishev, K.

2016-10-01

This is a review of a part of the work of the Technological Design Group at Technical University of Sofia, Faculty of Electronic Engineering and Technologies, Department of Microelectronics. It is dealing with piezoelectric polymer materials and their application in different microsystems (MEMS) and Energy Harvesting Devices (EHD), some organic materials and their applications in organic (OLED) displays, some transparent conductive materials etc. The metal oxides Lead Zirconium Titanate (PZT) and Zinc Oxide (ZnO) are used as piezoelectric layers - driving part of different sensors, actuators and EHD. These materials are studied in term of their performance in dependence on the deposition conditions and parameters. They were deposited as thin films by using RF Sputtering System. As technological substrates, glass plates and Polyethylenetherephtalate (PET) foils were used. For characterization of the materials, a test structure, based on Surface Acoustic Waves (SAW), was designed and prepared. The layers were characterized by Fourier Transform Infrared spectroscopy (FTIR). The piezoelectric response was tested at variety of mechanical loads (tensile strain, stress) in static and dynamic (multiple bending) mode. The single-layered and double-layered structures were prepared for piezoelectric efficiency increase. A structure of piezoelectric energy transformer is proposed and investigated.

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.

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

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

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.

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.

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.

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.

In situ high temperature oxidation analysis of Zircaloy-4 using acoustic emission coupled with thermogravimetry

NASA Astrophysics Data System (ADS)

Omar, Al Haj; Véronique, Peres; Eric, Serris; François, Grosjean; Jean, Kittel; François, Ropital; Michel, Cournil

2015-06-01

Zircaloy-4 oxidation behavior at high temperature (900 °C), which can be reached in case of severe accidental situations in nuclear pressurised water reactor, was studied using acoustic emission analysis coupled with thermogravimetry. Two different atmospheres were used to study the oxidation of Zircaloy-4: (a) helium and pure oxygen, (b) helium and oxygen combined with slight addition of air. The experiments with 20% of oxygen confirm the dependence on oxygen anions diffusion in the oxide scale. Under a mixture of oxygen and air in helium, an acceleration of the corrosion was observed due to the detrimental effect of nitrogen. The kinetic rate increased significantly after a kinetic transition (breakaway). This acceleration was accompanied by an acoustic emission activity. Most of the acoustic emission bursts were recorded after the kinetic transition (post-transition) or during the cooling of the sample. The characteristic features of the acoustic emission signals appear to be correlated with the different populations of cracks and their occurrence in the ZrO2 layer or in the α-Zr(O) layer. Acoustic events were recorded during the isothermal dwell time at high temperature under air. They were associated with large cracks in the zirconia porous layer. Acoustic events were also recorded during cooling after oxidation tests both under air or oxygen. For the latter, cracks were observed in the oxygen enriched zirconium metal phase and not in the dense zirconia layer after 5 h of oxidation.

A high performance transparent resistive switching memory made from ZrO2/AlON bilayer structure

NASA Astrophysics Data System (ADS)

Tsai, Tsung-Ling; Chang, Hsiang-Yu; Lou, Jesse Jen-Chung; Tseng, Tseung-Yuen

2016-04-01

In this study, the switching properties of an indium tin oxide (ITO)/zirconium oxide (ZrO2)/ITO single layer device and those of a device with an aluminum oxynitride (AlON) layer were investigated. The devices with highly transparent characteristics were fabricated. Compared with the ITO/ZrO2/ITO single layer device, the ITO/ZrO2/AlON/ITO bilayer device exhibited a larger ON/OFF ratio, higher endurance performance, and superior retention properties by using a simple two-step forming process. These substantial improvements in the resistive switching properties were attributed to the minimized influence of oxygen migration through the ITO top electrode (TE), which can be realized by forming an asymmetrical conductive filament with the weakest part at the ZrO2/AlON interface. Therefore, in the ITO/ZrO2/AlON/ITO bilayer device, the regions where conductive filament formation and rupture occur can be effectively moved from the TE interface to the interior of the device.

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.

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.

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.

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

Corrosion Behavior of Zirconium Treated Mild Steel with and Without Organic Coating: a Comparative Study

NASA Astrophysics Data System (ADS)

Ghanbari, Alireza; Attar, Mohammadreza Mohammadzade

2014-10-01

In this study, the anti-corrosion performance of phosphated and zirconium treated mild steel (ZTMS) with and without organic coating was evaluated using AC and DC electrochemical techniques. The topography and morphology of the zirconium treated samples were studied using atomic force microscopy (AFM) and field emission scanning electron microscope (FE-SEM) respectively. The results revealed that the anti-corrosion performance of the phosphate layer was superior to the zirconium conversion layer without an organic coating due to very low thickness and porous nature of the ZTMS. Additionally, the corrosion behavior of the organic coated substrates was substantially different. It was found that the corrosion protection performance of the phosphate steel and ZTMS with an organic coating is in the same order.

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.

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.

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.

Bioactivity and cytocompatibility of zirconia (ZrO(2)) films fabricated by cathodic arc deposition.

PubMed

Liu, Xuanyong; Huang, Anping; Ding, Chuanxian; Chu, Paul K

2006-07-01

Zirconium oxide thin films were fabricated on silicon wafers using a filtered cathodic arc system in concert with oxygen plasma. The structure and phase composition of the zirconium oxide thin films were characterized by atomic force microscopy (AFM), X-ray diffraction (XRD), Rutherford backscattering spectrometry (RBS), and transmission electron microscopy (TEM). The bioactivity was assessed by investigating the formation of apatite on the film surface after soaking in simulated body fluids. Bone marrow mesenchymal stem cells (BMMSC) were used to further evaluate the cytocompatibility of the materials. The results indicate that the films are composed of stoichiometric ZrO(2) and the composition is quite uniform throughout the thickness. Bone-like apatite can be formed on the surface of the ZrO(2) thin film in our SBF immersion experiments, suggesting that the surface is bioactive. The outermost layer of the ZrO(2) thin film comprises nano-sized particles that can be identified by AFM images taken on the thin film surface and TEM micrographs obtained from the interface between the ZrO(2) thin film and apatite layer. The nanostructured surface is believed to be the key factor that apatite is induced to precipitate on the surface. Bone marrow mesenchymal stem cells are observed to grow and proliferate in good states on the film surface. Our results show that ZrO(2) thin films fabricated by cathodic arc deposition exhibit favorable bioactivity and cytocompatibility.

Parametric evaluation of a dual-layer dynamic hyperfiltration membrane for recovery of spacecraft wash water at elevated temperature

NASA Technical Reports Server (NTRS)

Brandon, C. A.; Gaddis, J. L.

1975-01-01

Performance data consisting of solute rejections and product flux have been measured, as dependent on the operational parameters. These parameters were pressure, 5,000,000 N/sq m (750 psia) to 7,000,000 N/sq m (1040 psia); temperature, 347 K (165 F) to 368 K (200 F); velocity, 1.6 m/s to 10 m/s; and concentration (up to 14x). Tests were carried out on analog wash water. Data taken include rejections of organic materials (TOC), 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.

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.

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.

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

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

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.

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.

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.

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.

Cathode for aluminum producing electrolytic cell

DOEpatents

Brown, Craig W.

2004-04-13

A method of producing aluminum in an electrolytic cell comprising the steps of providing an anode in a cell, preferably a non-reactive anode, and also providing a cathode in the cell, the cathode comprised of a base material having low electrical conductivity reactive with molten aluminum to provide a highly electrically conductive layer on the base material. Electric current is passed from the anode to the cathode and alumina is reduced and aluminum is deposited at the cathode. The cathode base material is selected from boron carbide, and zirconium oxide.

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.

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.

Surface and Interface Chemistry for Gate Stacks on Silicon

NASA Astrophysics Data System (ADS)

Frank, M. M.; Chabal, Y. J.

This chapter addresses the fundamental silicon surface science associated with the continued progress of nanoelectronics along the path prescribed by Moore's law. Focus is on hydrogen passivation layers and on ultrathin oxide films encountered during silicon cleaning and gate stack formation in the fabrication of metal-oxide-semiconductor field-effect transistors (MOSFETs). Three main topics are addressed. (i) First, the current practices and understanding of silicon cleaning in aqueous solutions are reviewed, including oxidizing chemistries and cleans leading to a hydrogen passivation layer. The dependence of the final surface termination and morphology/roughness on reactant choice and pH and the influence of impurities such as dissolved oxygen or metal ions are discussed. (ii) Next, the stability of hydrogen-terminated silicon in oxidizing liquid and gas phase environments is considered. In particular, the remarkable stability of hydrogen-terminated silicon surface in pure water vapor is discussed in the context of atomic layer deposition (ALD) of high-permittivity (high-k) gate dielectrics where water is often used as an oxygen precursor. Evidence is also provided for co-operative action between oxygen and water vapor that accelerates surface oxidation in humid air. (iii) Finally, the fabrication of hafnium-, zirconium- and aluminum-based high-k gate stacks is described, focusing on the continued importance of the silicon/silicon oxide interface. This includes a review of silicon surface preparation by wet or gas phase processing and its impact on high-k nucleation during ALD growth, and the consideration of gate stack capacitance and carrier mobility. In conclusion, two issues are highlighted: the impact of oxygen vacancies on the electrical characteristics of high-k MOS devices, and the way alloyed metal ions (such as Al in Hf-based gate stacks) in contact with the interfacial silicon oxide layer can be used to control flatband and threshold voltages.

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.

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

PLZT capacitor and method to increase the dielectric constant

DOEpatents

Taylor, Ralph S.; Fairchild, Manuel Ray; Balachjandran, Uthamalingam; Lee, Tae H.

2017-12-12

A ceramic-capacitor includes a first electrically-conductive-layer, a second electrically-conductive-layer arranged proximate to the first electrically-conductive-layer, and a dielectric-layer interposed between the first electrically-conductive-layer and the second electrically-conductive-layer. The dielectric-layer is formed of a lead-lanthanum-zirconium-titanate material (PLZT), wherein the PLZT is characterized by a dielectric-constant greater than 125, when measured at 25 degrees Celsius and zero Volts bias, and an excitation frequency of ten-thousand Hertz (10 kHz). A method for increasing a dielectric constant of the lead-lanthanum-zirconium-titanate material (PLZT) includes the steps of depositing PLZT to form a dielectric-layer of a ceramic-capacitor, and heating the ceramic-capacitor to a temperature not greater than 300.degree. C.

A high performance transparent resistive switching memory made from ZrO{sub 2}/AlON bilayer structure

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

Tsai, Tsung-Ling; Chang, Hsiang-Yu; Tseng, Tseung-Yuen, E-mail: tseng@cc.nctu.edu.tw

2016-04-11

In this study, the switching properties of an indium tin oxide (ITO)/zirconium oxide (ZrO{sub 2})/ITO single layer device and those of a device with an aluminum oxynitride (AlON) layer were investigated. The devices with highly transparent characteristics were fabricated. Compared with the ITO/ZrO{sub 2}/ITO single layer device, the ITO/ZrO{sub 2}/AlON/ITO bilayer device exhibited a larger ON/OFF ratio, higher endurance performance, and superior retention properties by using a simple two-step forming process. These substantial improvements in the resistive switching properties were attributed to the minimized influence of oxygen migration through the ITO top electrode (TE), which can be realized by formingmore » an asymmetrical conductive filament with the weakest part at the ZrO{sub 2}/AlON interface. Therefore, in the ITO/ZrO{sub 2}/AlON/ITO bilayer device, the regions where conductive filament formation and rupture occur can be effectively moved from the TE interface to the interior of the device.« less

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

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.

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

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.

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.

Effects of growth temperature on the properties of atomic layer deposition grown ZrO2 films

NASA Astrophysics Data System (ADS)

Scarel, G.; Ferrari, S.; Spiga, S.; Wiemer, C.; Tallarida, G.; Fanciulli, M.

2003-07-01

Zirconium dioxide films are grown in 200 atomic layer deposition cycles. Zirconium tetrachloride (ZrCl4) and water (H2O) are used as precursors. A relatively high dielectric constant (κ=22), wide band gap, and conduction band offset (5.8 and 1.4 eV, respectively) indicate that zirconium dioxide is a most promising substitute for silicon dioxide as a dielectric gate in complementary metal-oxide-semiconductor devices. However, crystallization and chlorine ions in the films might affect their electrical properties. These ions are produced during atomic layer deposition in which the ZrCl4 precursor reacts with the growth surface. It is desirable to tune the composition, morphology, and structural properties in order to improve their benefit on the electrical ones. To address this issue it is necessary to properly choose the growth parameters. This work focuses on the effects of the growth temperature Tg. ZrO2 films are grown at different substrate temperatures: 160, 200, 250, and 350 °C. Relevant modification of the film structure with a change in substrate temperature during growth is expected because the density of reactive sites [mainly Si+1-(OH)-1 bonds] decreases with an increase in temperature [Y. B. Kim et al., Electrochem. Solid-State Lett. 3, 346 (2000)]. The amorphous film component, for example, that develops at Si+1-(OH)-1 sites on the starting growth surface, is expected to decrease with an increase in growth temperature. The size and consequences of film property modifications with the growth temperature are investigated in this work using x-ray diffraction and reflectivity, and atomic force microscopy. Time of flight-secondary ion mass spectrometry is used to study contaminant species in the films. From capacitance-voltage (CV) and current-voltage (IV) measurements, respectively, the dielectric constant κZrO2 and the leakage current are studied as a function of the film growth temperature.

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.

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

Parametric test of a zirconium (4) oxide-polyacrylic acid dual layer hyperfiltration membrane with spacecraft washwater

NASA Technical Reports Server (NTRS)

Brandon, C. A.; Gaddis, J. L.; El-Nashar, A. M.

1975-01-01

Performance data consisting of solute rejections and product flux were measured, as dependent on the operation parameters. These parameters and ranges were pressure (500,000 n/m2 to 700,000 n/m2), temperature (74 C to 95 C), velocity (1.6 M/sec to 10 M/sec), and concentration (up to 14x). Tests were carried out on analog washwater. Data presented include rejections of organic materials, ammonia, urea, and an assortment of ions. The membrane used was deposited in situ on a porcelain ceramic substrate.

Combining monolithic zirconia crowns, digital impressioning, and regenerative cement for a predictable restorative alternative to PFM.

PubMed

Griffin, Jack D

2013-03-01

Advances in indirect esthetic materials in recent years have provided the dental profession higher levels of strength and esthetics than ever before with products like lithium disilicate and zirconium oxide. Providing excellent fit and versatile performance, and because there is no porcelain to delaminate, chip, or fracture, monolithic zirconia crowns have the potential to outperform other layered restorations such as porcelain-fused-to-metal (PFM). This review of monolithic zirconia highlights a clinical case in which all-zirconia restorations were combined with CAD/CAM technology for a successful esthetic restorative outcome.

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.

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.

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.

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

The effect of zirconium-based surface treatment on the cathodic disbonding resistance of epoxy coated mild steel

NASA Astrophysics Data System (ADS)

Ghanbari, A.; Attar, M. M.

2014-10-01

The effect of zirconium-based surface treatment on the cathodic disbonding resistance and adhesion performance of an epoxy coated mild steel substrate was investigated. The obtained data from pull-off, cathodic disbonding test and electrochemical impedance spectroscopy (EIS) indicated that the zirconium conversion layer significantly improved the adhesion strength and cathodic disbonding resistance of the epoxy coating. This may be attributed to formation of some polar zirconium compounds on the surface and increment of surface roughness, that were evident in the results of field emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM), respectively.

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

Modification and intercalation of layered zirconium phosphates: a solid-state NMR monitoring.

PubMed

Bakhmutov, Vladimir I; Kan, Yuwei; Sheikh, Javeed Ahmad; González-Villegas, Julissa; Colón, Jorge L; Clearfield, Abraham

2017-07-01

Several layered zirconium phosphates treated with Zr(IV) ions, modified by monomethoxy-polyethyleneglycol-monophosphate and intercalated with doxorubicin hydrochloride have been studied by solid-state MAS NMR techniques. The organic components of the phosphates have been characterized by the 13 C{ 1 H} CP MAS NMR spectra compared with those of initial compounds. The multinuclear NMR monitoring has provided to establish structure and covalent attachment of organic/inorganic moieties to the surface and interlayer spaces of the phosphates. The MAS NMR experiments including kinetics of proton-phosphorus cross polarization have resulted in an unusual structure of zirconium phosphate 6 combining decoration of the phosphate surface by polymer units and their partial intercalation into the interlayer space. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Atomic Layer Deposited Thin Films for Dielectrics, Semiconductor Passivation, and Solid Oxide Fuel Cells

NASA Astrophysics Data System (ADS)

Xu, Runshen

Atomic layer deposition (ALD) utilizes sequential precursor gas pulses to deposit one monolayer or sub-monolayer of material per cycle based on its self-limiting surface reaction, which offers advantages, such as precise thickness control, thickness uniformity, and conformality. ALD is a powerful means of fabricating nanoscale features in future nanoelectronics, such as contemporary sub-45 nm metal-oxide-semiconductor field effect transistors, photovoltaic cells, near- and far-infrared detectors, and intermediate temperature solid oxide fuel cells. High dielectric constant, kappa, materials have been recognized to be promising candidates to replace traditional SiO2 and SiON, because they enable good scalability of sub-45 nm MOSFET (metal-oxide-semiconductor field-effect transistor) without inducing additional power consumption and heat dissipation. In addition to high dielectric constant, high-kappa materials must meet a number of other requirements, such as low leakage current, high mobility, good thermal and structure stability with Si to withstand high-temperature source-drain activation annealing. In this thesis, atomic layer deposited Er2O3 doped TiO2 is studied and proposed as a thermally stable amorphous high-kappa dielectric on Si substrate. The stabilization of TiO2 in its amorphous state is found to achieve a high permittivity of 36, a hysteresis voltage of less than 10 mV, and a low leakage current density of 10-8 A/cm-2 at -1 MV/cm. In III-V semiconductors, issues including unsatisfied dangling bonds and native oxides often result in inferior surface quality that yields non-negligible leakage currents and degrades the long-term performance of devices. The traditional means for passivating the surface of III-V semiconductors are based on the use of sulfide solutions; however, that only offers good protection against oxidation for a short-term (i.e., one day). In this work, in order to improve the chemical passivation efficacy of III-V semiconductors, ultra-thin layer of encapsulating ZnS is coated on the surface of GaSb and GaSb/InAs substrates. The 2 nm-thick ZnS film is found to provide a long-term protection against reoxidation for one order and a half longer times than prior reported passivation likely due to its amorphous structure without pinholes. Finally, a combination of binary ALD processes is developed and demonstrated for the growth of yttria-stabilized zirconia films using alkylamido-cyclopentadiengyls zirconium and tris(isopropyl-cyclopentadienyl)yttrium, as zirconium and yttrium precursors, respectively, with ozone being the oxidant. The desired cubic structure of YSZ films is apparently achieved after post-deposition annealing. Further, platinum is atomic layer deposited as electrode on YSZ (8 mol% of Yttria) within the same system. In order to control the morphology of as-deposited Pt thin structure, the nucleation behavior of Pt on amorphous and cubic YSZ is investigated. Three different morphologies of Pt are observed, including nanoparticle, porous and dense films, which are found to depend on the ALD cycle number and the structure and morphology of they underlying ALD YSZ films.

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.

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.

In situ ceramic layer growth on coated fuel particles dispersed in a zirconium metal matrix

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

Terrani, Kurt A; Silva, G W Chinthaka M; Kiggans, Jim

2013-01-01

The extent and nature of the chemical interaction between the outermost coating layer of coated fuel particles embedded in zirconium metal during fabrication of metal matrix microencapsulated fuels was examined. Various particles with outermost coating layers of pyrocarbon, SiC, and ZrC have been investigated in this study. ZrC-Zr interaction was least substantial while PyC-Zr reaction can be exploited to produce a ZrC layer at the interface in an in situ manner. The thickness of the ZrC layer in the latter case can be controlled by adjusting the time and temperature during processing. The kinetics of ZrC layer growth is significantlymore » faster from what is predicted using literature carbon diffusivity data in ZrC. SiC-Zr interaction is more complex and results in formation of various chemical phases in a layered aggregate morphology at the interface.« less

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

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.

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.

Process for electroless deposition of metals on zirconium materials

DOEpatents

Donaghy, Robert E.

1978-01-01

A process for the electroless deposition of a metal layer on an article comprised of zirconium or a zirconium alloy is disclosed. The article is activated in an aged aqueous solution comprising from about 10 to about 20 grams per liter ammonium bifluoride and from about 0.75 to about 2 grams per liter of sulfuric acid. The solution is aged by immersion of pickled zirconium in the solution for at least about 10 minutes. The loosely adhering film formed on the article in the activating step is removed and the article is contacted with an electroless plating solution containing the metal to be deposited on the article upon sufficient contact with the article.

Process for electrolytic deposition of metals on zirconium materials

DOEpatents

Donaghy, Robert E.

1979-01-30

A process for the electrolytic deposition of a metal layer on an article comprised of zirconium or a zirconium alloy is disclosed. The article is activated in an aged aqueous solution comprising from about 10 to about 20 grams per liter ammonium bifluoride and from about 0.75 to about 2 grams per liter of sulfuric acid. The solution is aged by immersion of pickled zirconium in the solution for at least about 10 minutes. The loosely adhering film formed on the article in the activating step is removed and the article is contacted with an electrolytic plating solution containing the metal to be deposited on the article in the presence of an electrode receiving current.

Sol-gel-derived double-layered nanocrystal memory

NASA Astrophysics Data System (ADS)

Ko, Fu-Hsiang; You, Hsin-Chiang; Lei, Tan-Fu

2006-12-01

The authors have used the sol-gel spin-coating method to fabricate a coexisting hafnium silicate and zirconium silicate double-layered nanocrystal (NC) memories. From transmission electron microscopic and x-ray photoelectron spectroscopic analyses, the authors determined that the hafnium silicate and zirconium silicate NCs formed after annealing at 900°C for 1min. When using channel hot electron injection for charging and band-to-band tunneling-induced hot hole injection for discharging, the NC memories exhibited superior Vth shifting because of the higher probability for trapping the charge carrier.

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.

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.

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

The synthesis and application of fine particles for coatings and composites

NASA Astrophysics Data System (ADS)

Stephenson, Richard Charles

A variety of coating methods are presented for producing titanium and zirconium oxide coatings on spherical alpha-alumina substrates. Some methods did not completely coat the alumina substrate leaving surface areas exposed. Techniques such as surface modifications with PDVB and 4-VP did produce coatings of metal oxides of very high quality. The best metal oxide coatings are produced from pre-treatment of the alumina microspheres followed by the acid catalyzed hydrolysis of the metal tetra-alkoxides. Methods to investigate converting titanium oxide and zirconium oxide coated alumina microspheres to the corresponding metal carbide coated alumina microspheres have been done. The methods involving direct reduction of the metal oxides by methane and methane-hydrogen gas proved inefficient in producing high quality metal carbide coatings. It is evident higher processing temperatures are required to achieve good metal carbide yield by these methods. Metal oxide coated products carbided by ART (Buffalo, NY) proved the carbiding can be accomplished at higher temperatures and with a different carburizing gas. In addition to the ART carbiding method, the magnesium thermite reaction is a promising method in converting metal oxides to metal carbides at much lower temperatures and shorter processing times. The electrophoretic deposition of Bi2Sr2CaCu 2O8 powder was in ethanol. Of critical consequence were the design of the cathode geometry and the arrangement of the electrodes so that all faces and edges of the silver anode were coated simultaneously. This was achieved by shaping the platinum cathode into a configuration that allowed the silver tape to be completely surrounded by the platinum. The electrophoretic cell was set up to keep the electrodes stationary thereby maintaining a constant distance from the cathode and anode (3 mm). The relationship between deposition time and coating thickness was determined for various powder loadings for a given electric field strength (62 V). For low powder loadings (10 and 20 g/L), the thickness of the coating increases with increasing deposition time (6, 12, and 24 hours). At a powder loading of 30 g/L, the thickness of the BSCCO layer decreases from a deposition time of 6 to 12 hours. At 24 hours, the layer thickness increases. Very high powder loadings (40 g/L) showed a linear decrease in the BSCCO layer thickness with increasing deposition time. Analysis by XRD showed the EPD superconductor exhibited preferential orientation on the silver tape. The degree of orientation was related to the layer thickness and hence the deposition times. Thermal treatment at 800°C in 90% Ar-10% O2 improved the orientation effects. A marked improvement in the surface texture was also observed by SEM. Carbon nanotubes were synthesized via Fe catalysis in an aerosol column in the presence of Ar, CO, and H2 gas. Fe particles were generated by the thermal decarbonylation of Fe(CO)5. Multiwalled and single-walled carbon nanotubes were grown from the decomposition of CO gas on the forming Fe particles. Optimal conditions were determined for producing high yields of single-walled nanotubes. A growth theory is proposed based on the results. (Abstract shortened by UMI.)

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.

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.

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.

Material distribution in light water reactor-type bundles tested under severe accident conditions

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

Noack, V.; Hagen, S.J.L.; Hofmann, P.

1997-02-01

Severe fuel damage experiments simulating small-break loss-of-coolant accidents have been carried out in the CORA out-of-pile test facility at Forschungszentrum Karlsruhe. Rod bundles with electrically heated fuel rod simulators containing annular UO{sub 2} pellets, UO{sub 2} full pellet rods, and absorber rods of two kinds (Ag/In/Cd to represent pressurized water reactor conditions and B{sub 4}C to represent boiling water reactor and VVER-1000 fuel elements) were subjected to temperature transients up to 2,300 K. A special method was applied to determine the axial mass distribution of bundle materials. The low-temperature melt formation by various interactions between zirconium and components of absorbermore » and spacer grids strongly influences the bundle degradation and material relocation. Absorber materials can separate from the fuel by a noncoherent relocation of the materials at different temperatures. The distributions of solidified materials in the different test bundles show a clear dependence on the axial temperature profile. Coolant channel blockages are observed mainly at the lower end of the bundle, i.e., near the lowest elevation at which an oxidation excursion resulting from the highly exothermic zirconium-steam reaction had been experienced. This elevation corresponds with a steep axial temperature gradient in the maximum temperature attained. Oxide layers on Zircaloy result in reduced melt formation.« less

Effects of alpha-zirconium phosphate on thermal degradation and flame retardancy of transparent intumescent fire protective coating

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

Xing, Weiyi; Zhang, Ping; Song, Lei

2014-01-01

Graphical abstract: - Highlights: • A transparent intumescent fire protective coating was obtained by UV-cured technology. • OZrP could enhance the thermal stability and anti-oxidation of the coating. • OZrP could reduce the combustion properties of the coatings. - Abstract: Organophilic alpha-zirconium phosphate (OZrP) was used to improve the thermal and fire retardant behaviors of the phenyl di(acryloyloxyethyl)phosphate (PDHA)-triglycidyl isocyanurate acrylate (TGICA)-2-phenoxyethyl acrylate (PHEA) (PDHA-TGICA-PHEA) coating. The morphology of nanocomposite coating was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The effect of OZrP on the flame retardancy, thermal stability, fireproofing time and char formation of the coatingsmore » was investigated by microscale combustion calorimeter (MCC), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), laser Raman spectroscopy (LRS) and scanning electric microscope (SEM). The results showed that by adding OZrP, the peak heat release rate and total heat of combustion were significantly reduced. The highest improvement was achieved with 0.5 wt% OZrP. XPS analysis indicated that the performance of anti-oxidation of the coating was improved with the addition of OZrP, and SEM images showed that a good synergistic effect was obtained through a ceramic-like layer produced by OZrP covered on the surface of char.« less

Rare earth zirconium oxide buffer layers on metal substrates

DOEpatents

Williams, Robert K.; Paranthaman, Mariappan; Chirayil, Thomas G.; Lee, Dominic F.; Goyal, Amit; Feenstra, Roeland

2001-01-01

A laminate article comprises a substrate and a biaxially textured (RE.sub.x A.sub.(1-x)).sub.2 O.sub.2-(x/2) buffer layer over the substrate, wherein 0

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.

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.

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

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

The Influence of the In-Situ Clad Staining on the Corrosion of Zircaloy in PWR Water Environment

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

Kammenzind, B.F., Eklund, K.L. and Bajaj, R.

Zircaloy cladding tubes strain in-situ during service life in the corrosive environment of a Pressurized Water Reactor for a variety of reasons. First, the tube undergoes stress free growth due to the preferential alignment of irradiation induced vacancy loops on basal planes. Positive strains develop in the textured tubes along prism orientations while negative strains develop along basal orientations (Reference (a)). Second, early in life, free standing tubes will often shrink by creep in the diametrical direction under the external pressure of the water environment, but potentially grow later in life in the diametrical direction once the expanding fuel pelletmore » contacts the cladding inner wall (Reference (b)). Finally, the Zircaloy cladding absorbs hydrogen as a by product of the corrosion reaction (Reference (c)). Once above the solubility limit in Zircaloy, the hydride precipitates as zirconium hydride (References (c) through (j)). Both hydrogen in solid solution and precipitated as Zirconium hydride cause a volume expansion of the Zircaloy metal (Reference (k)). Few studies are reported on that have investigated the influence that in-situ clad straining has on corrosion of Zircaloy. If Zircaloy corrosion rates are governed by diffusion of anions through a thin passivating boundary layer at the oxide-to-metal interface (References (l) through (n)), in-situ straining of the cladding could accelerate the corrosion process by prematurely breaking that passivating oxide boundary layer. References (o) through (q) investigated the influence that an applied tensile stress has on the corrosion resistance of Zircaloy. Knights and Perkins, Reference (o), reported that the applied tensile stress increased corrosion rates above a critical stress level in 400 C and 475 C steam, but not at lower temperatures nor in dry oxygen environments. This latter observation suggested that hydrogen either in the oxide or at the oxide-to-metal interface is involved in the observed stress effect. Kim et al. (Reference (p)) and Kim and Kim (Reference (q)) more recently investigated the influence that an applied hoop stress has on the corrosion resistance of Zircaloy tubes in a 400 C steam and in a 350 C concentrated lithia water environment. Both of these studies found the applied tensile hoop stress to have no effect on cladding corrosion rates in the 400 C steam environment but to have accelerated corrosion in the lithiated water environment. In both cases, the corrosion acceleration in the lithiated water environment was attributed to the accumulation of the increased hydrogen picked up in the lithiated environment into the tensile regions of the test specimen. Dense hydride rims have been shown, independent of clad strain, to accelerate the corrosion of Zirconium alloys (References (r) and (s)), suggesting that the primary effect of applied stresses on the corrosion of Zircaloy in the above studies is through the accumulation of hydrogen at the oxide-to-metal interface and not through a direct mechanical breakdown of the passivating boundary layer. To further investigate the potential role of in-situ clad straining (or stress) on Zircaloy corrosion rates, two experimental studies were performed. First, several samples that were irradiated with and without an applied stress were destructively examined for the extent of corrosion occurring in strained and nonstrained regions of the test samples. The extent of corrosion was determined, posttest, by metallographic examination. Second, the corrosion process was monitored in-situ using electrochemical impedance spectroscopy on samples exposed out-of-reactor with and without an applied stress. Post test, these autoclave samples were also metallographically examined.« less

Evolution of zirconyl-stearate Langmuir monolayers and the synthesized ZrO2 thin films with pH

NASA Astrophysics Data System (ADS)

Choudhary, Raveena; Sharma, Rajni; Brar, Loveleen K.

2018-04-01

ZrO2 thin films have a wide range of applications ranging from photonics, antireflection coatings, and resistive oxygen gas sensors, as a gate dielectric and in high temperature fuel cells. We have used the deposition of zirconyl stearate monolayers followed by their oxidation as a method for the synthesis of zirconium oxide thin films. The zirconyl stearate films have been studied and deposited for first time to the best of our knowledge. The Langmuir monolayers are studied using pressure-Area (π-A) isotherms and oscillatory barrier method. The morphology of the films for limited number of layers was studied with FE-SEM to determine the effect of pH on the final ZrO2 film. The 200 layer deposition films show pure monoclinic phase. The films have a band gap ˜6.0eV with a strong PL emission peak is at 490 nm and a weak peak is at 423 nm. So the films formed by this deposition method are suitable for luminescent applications

Influence of Ar-ion implantation on the structural and mechanical properties of zirconia as studied by Raman spectroscopy and nanoindentation techniques

NASA Astrophysics Data System (ADS)

Kurpaska, L.; Jasinski, J.; Wyszkowska, E.; Nowakowska-Langier, K.; Sitarz, M.

2018-04-01

In this study, structural and nanomechanical properties of zirconia polymorphs induced by ion irradiation were investigated by means of Raman spectroscopy and nanoindentation techniques. The zirconia layer have been produced by high temperature oxidation of pure zirconium at 600 °C for 5 h at normal atmospheric pressure. In order to distinguish between the internal and external parts of zirconia, the spherical metallographic sections have been prepared. The samples were irradiated at room temperature with 150 keV Ar+ ions at fluences ranging from 1 × 1015 to 1 × 1017 ions/cm2. The main objective of this study was to distinguish and confirm different structural and mechanical properties between the interface layer and fully developed scale in the internal/external part of the oxide. Conducted studies suggest that increasing ion fluence impacts Raman bands positions (especially characteristic for tetragonal phase) and increases the nanohardness and Young's modulus of individual phases. This phenomenon has been examined from the point of view of stress-induced hardening effect and classical monoclinic → tetragonal (m → t) martensitic phase transformation.

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.

Oxidation resistance, thermal conductivity, and spectral emittance of fully dense zirconium diboride with silicon carbide and tantalum diboride additives

NASA Astrophysics Data System (ADS)

Van Laningham, Gregg Thomas

Zirconium diboride (ZrB2) is a ceramic material possessing ultra-high melting temperatures. As such, this compound could be useful in the construction of thermal protection systems for aerospace applications. This work addresses a primary shortcoming of this material, namely its propensity to destructively oxidize at high temperatures, as well as secondary issues concerning its heat transport properties. To characterize and improve oxidation properties, thermogravimetric studies were performed using a specially constructed experimental setup. ZrB 2-SiC two-phase ceramic composites were isothermally oxidized for ~90 min in flowing air in the range 1500-1900°C. Specimens with 30 mol% SiC formed distinctive reaction product layers which were highly protective; 28 mol% SiC - 6 mol% TaB2 performed similarly. At higher temperatures, specimens containing lower amounts of SiC were shown to be non-protective, whereas specimens containing greater amounts of SiC produced unstable oxide layers due to gas evolution. Oxide coating thicknesses calculated from weight loss data were consistent with those measured from SEM micrographs. In order to characterize one aspect of the materials' heat transport properties, the thermal diffusivities of ZrB2-SiC composites were measured using the laser flash technique. These were converted to thermal conductivities using temperature dependent specific heat and density data; thermal conductivity decreased with increasing temperature over the range 25-2000°C. The composition with the highest SiC content showed the highest thermal conductivity at room temperature, but the lowest at temperatures in excess of ~400°C, because of the greater temperature sensitivity of the thermal conductivity of the SiC phase, as compared to more electrically-conductive ZrB2. Subsequent finite difference calculations were good predictors of multi-phase thermal conductvities for the compositions examined. The thermal conductivities of pure ZrB2 as a function of temperature were back-calculated from the experimental results for the multi-phase materials, and literature thermal conductivities of the other two phases. This established a relatively constant thermal conductivity of 88-104 W·K over the evaluated temperature range. Further heat transport characterization was performed using pre-oxidized, directly resistively heated ZrB2-30 mol% SiC ribbon specimens under the observation of a spectral radiometer. The ribbons were heated and held at specific temperatures over the range 1100-1330°C in flowing Ar, and normal spectral emittance values were recorded over the 1-6 μm range with a resolution of 10 nm. The normal spectral emittance was shown to decrease with loss of the borosilicate layer over the course of the data collection time periods. This change was measured and compensated for to produce traces showing the emittance of the oxidized composition rising from ~0.7 to ~0.9 over the range of wavelengths measured (1-6 μm).

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.

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

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.

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.

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.

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

Synthesis and Characterization of Polydiacetylene Films and Nanotubes

PubMed Central

Gatebe, Erastus; Herron, Hayley; Zakeri, Rashid; Rajasekaran, Pradeep Ramiah; Aouadi, Samir; Kohli, Punit

2009-01-01

We report here the synthesis and characterization of polydiacetylene (PDA) films and nanotubes using layer-by-layer (LBL) chemistry. 10,12-Docosadiyndioic acid (DCDA) monomer was self-assembled on flat surfaces and inside of nanoporous alumina templates. UV irradiation of DCDA provided polymerized-DCDA (PDCDA) films and nanotubes. We have used zirconium-carboxylate interlayer chemistry to synthesize PDCDA multilayers on flat surfaces and in nanoporous template. PDCDA multilayers were characterized using optical (UV–vis, fluorescence, ellipsometry, FTIR) spectroscopies, ionic current–voltage (I–V) analysis, and scanning electron microscopy. Ellipsometry, FTIR, electronic absorption and emission spectroscopies showed a uniform DCDA deposition at each deposition cycle. Our optical spectroscopic analysis indicates that carboxylate-zirconium interlinking chemistry is robust. To explain the disorganization in the alkyl portion of PDCDA multilayer films, we propose carboxylate-zirconium interlinkages act as “locks” in between PDCDA layers which restrict the movement of alkyl portion in the films. Because of this locking, the induced-stresses in the polymer chains can not be efficiently relieved. Our ionic resistance data from I–V analysis correlate well with calculated resistance at smaller number of PDCDA layers but significantly deviated for thicker PDCDA nanotubes. These differences were attributed to ion-blocking because some of the PDCDA nanotubes were totally closed and the nonohmic and permselective ionic behaviors when the diameter of the pores approaches the double-layer thickness of the solution inside of the nanotubes. PMID:18823090

Atomic layer deposition of zirconium silicate films using zirconium tetrachloride and tetra-n-butyl orthosilicate

NASA Astrophysics Data System (ADS)

Kim, Won-Kyu; Kang, Sang-Woo; Rhee, Shi-Woo; Lee, Nae-In; Lee, Jong-Ho; Kang, Ho-Kyu

2002-11-01

Atomic layer chemical vapor deposition of zirconium silicate films with a precursor combination of ZrCl4 and tetra-n-butyl orthosilicate (TBOS) was studied for high dielectric gate insulators. The effect of deposition conditions, such as deposition temperature, pulse time for purge and precursor injection on the deposition rate per cycle, and composition of the film were studied. At 400 °C, the growth rate saturated to 1.35 Å/cycle above 500 sccm of the argon purge flow rate. The growth rate, composition ratio ((Zr/Zr+Si)), and impurity contents (carbon and chlorine) saturated with the increase of the injection time of ZrCl4 and TBOS and decreased with the increased deposition temperature from 300 to 500 °C. The growth rate, composition ratio, carbon, and chlorine contents of the Zr silicate thin films deposited at 500 °C were 1.05 Å/cycle, 0.23, 1.1 at. %, and 2.1 at. %, respectively. It appeared that by using only zirconium chloride and silicon alkoxide sources, the content of carbon and chlorine impurities could not be lowered below 1%. It was also found that the incorporation rate of metal from halide source was lower than alkoxide source.

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.

Surface engineering of zirconium particles by molecular layer deposition: Significantly enhanced electrostatic safety at minimum loss of the energy density

NASA Astrophysics Data System (ADS)

Qin, Lijun; Yan, Ning; Hao, Haixia; An, Ting; Zhao, Fengqi; Feng, Hao

2018-04-01

Because of its high volumetric heat of oxidation, Zr powder is a promising high energy fuel/additive for rocket propellants. However, the application of Zr powder is restricted by its ultra-high electrostatic discharge sensitivity, which poses great hazards for handling, transportation and utilization of this material. By performing molecular layer deposition of polyimide using 1,2,4,5-benzenetetracarboxylic anhydride and ethylenediamine as the precursors, Zr particles can be uniformly encapsulated by thin layers of the polymer. The thicknesses of the encapsulation layers can be precisely controlled by adjusting the number of deposition cycle. High temperature annealing converts the polymer layer into a carbon coating. Results of thermal analyses reveal that the polymer or carbon coatings have little negative effect on the energy release process of the Zr powder. By varying the thickness of the polyimide or carbon coating, electrostatic discharge sensitivity of the Zr powder can be tuned in a wide range and its uncontrolled ignition hazard can be virtually eliminated. This research demonstrates the great potential of molecular layer deposition in effectively modifying the surface properties of highly reactive metal based energetic materials with minimum sacrifices of their energy densities.

Microstructural and mechanical properties of Al2O3/ZrO2 nanomultilayer thin films prepared by pulsed laser deposition

NASA Astrophysics Data System (ADS)

Balakrishnan, G.; Sastikumar, D.; Kuppusami, P.; Babu, R. Venkatesh; Song, Jung Il

2018-02-01

Single layer aluminium oxide (Al2O3), zirconium oxide (ZrO2) and Al2O3/ZrO2 nano multilayer films were deposited on Si (100) substrates at room temperature by pulsed laser deposition. The development of Al2O3/ZrO2 nanolayered structure is an important method used to stabilize the high temperature phase (tetragonal and cubic) of ZrO2 at room temperature. In the Al2O3/ZrO2 multilayer structure, the Al2O3 layer was kept constant at 5 nm, while the ZrO2 layer thickness varied from 5 to 20 nm (5/5, 5/10, 5/15 and 5/20 nm) with a total of 40 bilayers. The X-ray diffraction studies of single layer Al2O3 indicated the γ-Al2O3 of cubic structure, while the single layer ZrO2 indicated both monoclinic and tetragonal phases. The 5/5 and 5/10 nm multilayer films showed the nanocrystalline nature of ZrO2 with tetragonal phase. The high resolution transmission electron microscopy studies indicated the formation of well-defined Al2O3 and ZrO2 layers and that they are of uniform thickness. The atomic force microscopy studies revealed the uniform and dense distribution of nanocrystallites. The nanoindentation studies indicated the hardness of 20.8 ± 1.10 and 10 ± 0.60 GPa, for single layer Al2O3 and ZrO2, respectively, and the hardness of multilayer films varied with bilayer thickness.

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

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).

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.

Effect of hydrogenation conditions on the microstructure and mechanical properties of zirconium hydride

NASA Astrophysics Data System (ADS)

Muta, Hiroaki; Nishikane, Ryoji; Ando, Yusuke; Matsunaga, Junji; Sakamoto, Kan; Harjo, Stefanus; Kawasaki, Takuro; Ohishi, Yuji; Kurosaki, Ken; Yamanaka, Shinsuke

2018-03-01

Precipitation of brittle zirconium hydrides deteriorate the fracture toughness of the fuel cladding tubes of light water reactor. Although the hydride embrittlement has been studied extensively, little is known about physical properties of the hydride due to the experimental difficulties. In the present study, to elucidate relationship between mechanical properties and microstructure, two δ-phase zirconium hydrides and one ε-phase zirconium hydride were carefully fabricated considering volume changes at the metal-to-hydride transformation. The δ-hydride that was fabricated from α-zirconium exhibits numerous inner cracks due to the large volume change. Analyses of the neutron diffraction pattern and electron backscatter diffraction (EBSD) data show that the sample displays significant stacking faults in the {111} plane and in the pseudo-layered microstructure. On the other hand, the δ-hydride sample fabricated from β-zirconium at a higher temperature displays equiaxed grains and no cracks. The strong crystal orientation dependence of mechanical properties were confirmed by indentation test and EBSD observation. The δ-hydride hydrogenated from α-zirconium displays a lower Young's modulus than that prepared from β-zirconium. The difference is attributed to stacking faults within the {111} plane, for which the Young's modulus exhibits the highest value in the perpendicular direction. The strong influence of the crystal orientation and dislocation density on the mechanical properties should be considered when evaluating hydride precipitates in nuclear fuel cladding.

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.

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.

Study on the hydrogenation of Zircaloy-4

NASA Astrophysics Data System (ADS)

da Silva Dupim, Ivaldete; Moreira, João M. L.; Silva, Selma Luiza; Silva, Cecilia Chaves Guedes e.; Nunes, Oswaldo; Gomide, Ricardo Gonçalves

2012-08-01

In this article we investigate producing Zirconium powder from discarded Zircaloy-4 material through the hydride-dehydride method. We restrict our study to the first part of the method, namely the hydrogenation process. Differential thermal analyses of the hydrogenation process of the Zircaloy-4 show that no hydrogen absorption occurs at temperatures below 573 K and hydrogen gas pressure of 25 kPa. When the system temperature is raised to around 770 K, with the same gas pressure, the protecting oxide layer of the specimens can be overcome and they are quickly hydrogenated. The bulk of the reaction occurs in about 5 min with the precipitation of Zirconium hydrides in the Zr-δ and Zr-ɛ phases. Once the temperature passes 573 K, the incubation time to initiate the reaction is short (about 5 min). Tests in a tube furnace system with larger samples, hydrogen pressure varying from 30 to 180 kPa, and temperature from 700 to 833.15 K, show that the specimens are fully hydrogenated and can be easily pulverized. The results indicate that the hydrogenation of the Zircaloy-4 chips can be successfully undertaken at temperatures around 770 K and hydrogen gas pressure as low as 30 kPa.

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.

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.

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.

[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.

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.

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.

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.

pH-responsive drug delivery system based on AIE luminogen functionalized layered zirconium phosphate nano-platelets

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

Li, Dongdong, E-mail: lidongdong@jlu.edu.cn; Zhang, Yuping; Zhou, Bingbing

2015-05-15

Aggregation-induced emission (AIE) luminogen, quaternary tetraphenylethene cation (TPEN), was successfully incorporated into layered α-zirconium phosphate (α-ZrP) by using co-precipitation method to form inorganic–organic hybrid materials. The obtained materials show the characteristic hexagonal platelet shape with the interlayer distance did not reveal significant difference compared with pure α-ZrP. In addition, the obtained hybrid materials emit strong blue emission centered at 476 nm in aqueous media due to the electrostatic interactions of TPEN with the anionic framework of α-ZrP, which largely restrict their intramolecular rotation. More importantly, the materials provide a pH dependent release of doxorubicin (DOX), suggesting that AIE luminogen functionalizedmore » α-ZrP may be used as an imaging guided and pH-responsive delivery system for targeting therapy. - Graphical abstract: AIE luminogen was successfully incorporated into layered α-zirconium phosphate by a co-precipitation method to form inorganic–organic hybrid materials, showing a pH dependent release of DOX. - Highlights: • AIE luminogen cation was incorporated into layered α-ZrP by co-precipitation method. • The obtained material emits strong blue emission upon UV irradiation. • The material exhibits pH dependent release of DOX. • The AIE functionalized α-ZrP has potential applications in imaging guided therapy.« less

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.

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)

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

ELECTROLYTIC CLADDING OF ZIRCONIUM ON URANIUM

DOEpatents

Wick, J.J.

1959-09-22

A method is presented for coating uranium with zircoalum by rendering the uranium surface smooth and oxidefree, immersing it in a molten electrolytic bath in NaCI, K/sub 2/ZrF/sub 6/, KF, and ZrO/sub 2/, and before the article reaches temperature equilibrium with the bath, applying an electrolyzing current of 60 amperes per square dectmeter at approximately 3 volts to form a layer of zirconium metal on the uranium.

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.

Structural and dielectric properties of thin ZrO2 films on silicon grown by atomic layer deposition from cyclopentadienyl precursor

NASA Astrophysics Data System (ADS)

Niinistö, J.; Putkonen, M.; Niinistö, L.; Kukli, K.; Ritala, M.; Leskelä, M.

2004-01-01

ZrO2 thin films with thicknesses below 20 nm were deposited by the atomic layer deposition process on Si(100) substrates at 350 °C. An organometallic precursor, Cp2Zr(CH3)2 (Cp=cyclopentadienyl, C5H5) was used as the zirconium source and water or ozone as oxygen source. The influence of oxygen source and substrate pretreatment on the dielectric properties of ZrO2 films was investigated. Structural characterization with high-resolution transmission electron microscopy was performed to films grown onto HF-etched or native oxide covered silicon. Strong inhibition of ZrO2 film growth was observed with the water process on HF-etched Si. Ozone process on HF-etched Si resulted in interfacial SiO2 formation between the dense and uniform film and the substrate while water process produced interfacial layer with intermixing of SiO2 and ZrO2. The effective permittivity of ZrO2 in Al/ZrO2/Si/Al capacitor structures was dependent on the ZrO2 layer thickness and oxygen source used. The interfacial layer formation increased the capacitance equivalent oxide thickness (CET). CET of 2.0 nm was achieved with 5.9 nm ZrO2 film deposited with the H2O process on HF-stripped Si. The ozone-processed films showed good dielectric properties such as low hysteresis and nearly ideal flatband voltage. The leakage current density was lower and breakdown field higher for the ozone-processed ZrO2 films.

Tailoring properties of lossy-mode resonance optical fiber sensors with atomic layer deposition technique

NASA Astrophysics Data System (ADS)

Kosiel, Kamil; Koba, Marcin; Masiewicz, Marcin; Śmietana, Mateusz

2018-06-01

The paper shows application of atomic layer deposition (ALD) technique as a tool for tailoring sensorial properties of lossy-mode-resonance (LMR)-based optical fiber sensors. Hafnium dioxide (HfO2), zirconium dioxide (ZrO2), and tantalum oxide (TaxOy), as high-refractive-index dielectrics that are particularly convenient for LMR-sensor fabrication, were deposited by low-temperature (100 °C) ALD ensuring safe conditions for thermally vulnerable fibers. Applicability of HfO2 and ZrO2 overlays, deposited with ALD-related atomic level thickness accuracy for fabrication of LMR-sensors with controlled sensorial properties was presented. Additionally, for the first time according to our best knowledge, the double-layer overlay composed of two different materials - silicon nitride (SixNy) and TaxOy - is presented for the LMR fiber sensors. The thin films of such overlay were deposited by two different techniques - PECVD (the SixNy) and ALD (the TaxOy). Such approach ensures fast overlay fabrication and at the same time facility for resonant wavelength tuning, yielding devices with satisfactory sensorial properties.

Nanocrystalline diamond protects Zr cladding surface against oxygen and hydrogen uptake: Nuclear fuel durability enhancement.

PubMed

Škarohlíd, Jan; Ashcheulov, Petr; Škoda, Radek; Taylor, Andrew; Čtvrtlík, Radim; Tomáštík, Jan; Fendrych, František; Kopeček, Jaromír; Cháb, Vladimír; Cichoň, Stanislav; Sajdl, Petr; Macák, Jan; Xu, Peng; Partezana, Jonna M; Lorinčík, Jan; Prehradná, Jana; Steinbrück, Martin; Kratochvílová, Irena

2017-07-25

In this work, we demonstrate and describe an effective method of protecting zirconium fuel cladding against oxygen and hydrogen uptake at both accident and working temperatures in water-cooled nuclear reactor environments. Zr alloy samples were coated with nanocrystalline diamond (NCD) layers of different thicknesses, grown in a microwave plasma chemical vapor deposition apparatus. In addition to showing that such an NCD layer prevents the Zr alloy from directly interacting with water, we show that carbon released from the NCD film enters the underlying Zr material and changes its properties, such that uptake of oxygen and hydrogen is significantly decreased. After 100-170 days of exposure to hot water at 360 °C, the oxidation of the NCD-coated Zr plates was typically decreased by 40%. Protective NCD layers may prolong the lifetime of nuclear cladding and consequently enhance nuclear fuel burnup. NCD may also serve as a passive element for nuclear safety. NCD-coated ZIRLO claddings have been selected as a candidate for Accident Tolerant Fuel in commercially operated reactors in 2020.

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.

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

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.

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.

Application of encapsulated superabsorbent polymers in cementitious materials for stimulated autogenous healing

NASA Astrophysics Data System (ADS)

Pelto, Jani; Leivo, Markku; Gruyaert, Elke; Debbaut, Brenda; Snoeck, Didier; De Belie, Nele

2017-10-01

Superabsorbent polymers have shown potential for use in mortar and concrete as self-healing agents. The main drawback is, however, that these superabsorbent polymers also absorb mixing water during the preparation and casting of mortar or concrete, leading to a loss in workability. To avoid the absorption of mixing water, superabsorbent polymers were coated using a fluid bed spraying process. The barrier coating consisted of three successive coating layers: polyvinylbutyral as primer/wetting layer, cyclo-olefin copolymer as a barrier layer and a sol-gel derived zirconium-silicon oxide as an adhesion-promoting topcoat layer. The coated SAPs were characterized, and their swelling determined to quantify the delay in uptake of water and Ca(OH)2 solution. The last was considered as the most important, as the SAPs will finally be applied in mortar or concrete having a pore solution with high pH. The results showed that swelling could be delayed to a large extent, but for a short time. Results showed that the self-sealing efficiency of mortars was not affected by coating the SAPs. Moreover, due to the reduced uptake of mixing water, the strength reduction, noticed when uncoated SAPs were added to the mortar, could partly be compensated.

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.

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.

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

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.

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.

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.

PLZT capacitor on glass substrate

DOEpatents

Fairchild, Manuel Ray; Taylor, Ralph S.; Berlin, Carl W.; Wong, Celine Wk; Ma, Beihai; Balachandran, Uthamalingam

2016-03-29

A lead-lanthanum-zirconium-titanate (PLZT) capacitor on a substrate formed of glass. The first metallization layer is deposited on a top side of the substrate to form a first electrode. The dielectric layer of PLZT is deposited over the first metallization layer. The second metallization layer deposited over the dielectric layer to form a second electrode. The glass substrate is advantageous as glass is compatible with an annealing process used to form the capacitor.

PLZT capacitor on glass substrate

DOEpatents

Fairchild, M. Ray; Taylor, Ralph S.; Berlin, Carl W.; Wong, Celine W. K.; Ma, Beihai; Balachandran, Uthamalingam

2016-01-05

A lead-lanthanum-zirconium-titanate (PLZT) capacitor on a substrate formed of glass. The first metallization layer is deposited on a top side of the substrate to form a first electrode. The dielectric layer of PLZT is deposited over the first metallization layer. The second metallization layer deposited over the dielectric layer to form a second electrode. The glass substrate is advantageous as glass is compatible with an annealing process used to form the capacitor.

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

Intercalation chemistry of zirconium 4-sulfophenylphosphonate

NASA Astrophysics Data System (ADS)

Svoboda, Jan; Zima, Vítězslav; Melánová, Klára; Beneš, Ludvík; Trchová, Miroslava

2013-12-01

Zirconium 4-sulfophenylphosphonate is a layered material which can be employed as a host for the intercalation reactions with basic molecules. A wide range of organic compounds were chosen to represent intercalation ability of zirconium 4-sulfophenylphosphonate. These were a series of alkylamines from methylamine to dodecylamine, 1,4-phenylenediamine, p-toluidine, 1,8-diaminonaphthalene, 1-aminopyrene, imidazole, pyridine, 4,4‧-bipyridine, poly(ethylene imine), and a series of amino acids from glycine to 6-aminocaproic acid. The prepared compounds were characterized by powder X-ray diffraction, thermogravimetry analysis and IR spectroscopy and probable arrangement of the guest molecules in the interlayer space of the host is proposed based on the interlayer distance of the prepared intercalates and amount of the intercalated guest molecules.

Compatibility of buffered uranium carbides with tungsten.

NASA Technical Reports Server (NTRS)

Phillips, W. M.

1971-01-01

Results of compatibility tests between tungsten and hyperstoichiometric uranium carbide alloys run at 1800 C for 1000 and 2500 hours. These tests compared tungsten-buffered uranium carbide with tungsten-buffered uranium-zirconium carbide. The zirconium carbide addition appeared to widen the homogeneity range of the uranium carbide, making additional carbon available for reaction. Reaction layers could be formed by either of two diffusion paths, one producing UWC2, while the second resulted in the formation of W2C. UWC2 acts as a diffusion barrier for carbon and slows the growth of the reaction layer with time, while carbon diffusion is relatively rapid in W2C, allowing equilibrium to be reached in less than 2500 hours at a temperature of 1800 C.

Study of corrosion-related defects of zirconium alloys with slow positron beam

NASA Astrophysics Data System (ADS)

Zhu, Zhejie; Yao, Meiyi; Shi, Jianjian; Yao, Chunlong; Lu, Eryang; Cao, Xingzhong; Wang, Baoyi; Wu, Yichu

2018-09-01

The corrosion behavior of Zr-4 and N5 alloy specimens corroded in 0.01 mol/L LiOH aqueous solution at 360 °C/18.6 MPa and in super heated steam at 400 °C/10.3 MPa for 1, 3 and 14 days were investigated by slow positron beam based Doppler broadening spectroscopy. Results showed that there was an evident interfacial layer with pre-existed vacancies and voids in uncorroded Zr-4 specimens, while in uncorroded N5 specimen, the interfacial defect layer can not be identified or a thin interfacial layer was only contained. When the specimens were corroded in super heated steam at 400 °C/10.3 MPa for a few days, the existence of the interface layer in the Zr-4 specimen would delay the diffusion rate of the oxygen atoms and decelerated the oxidation rate of the corrosion process. However, at very early stage of the corrosion, as Zr-4 and N5 specimens were corrded in 0.01 mol/L LiOH aqueous solution at 360 °C/18.6 MPa, the effect of Li+ accelerated the diffusion rate of the oxygen atoms, while the effect of the interface defect layer became a minor effect.

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.

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.

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

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.

Atomic layer deposition in a metal–organic framework: Synthesis, characterization, and performance of a solid acid

DOE PAGES

Rimoldi, Martino; Bernales, Varinia; Borycz, Joshua; ...

2017-01-05

NU-1000, a zirconium-based metal-organic framework featuring mesoporous channels, has been post-synthetically metalated via atomic layer deposition in MOF (AIM) employing dimethylaluminum iso-propoxide ([AlMe 2 iOPr] 2 – DMAI), a milder precursor than widely used trimethylaluminum (AlMe 3 - TMA). The aluminum-modified NU-1000 (Al-NU-1000) has been characterized with a comprehensive suite of techniques that points to the formation of aluminum oxide clusters well dispersed through the framework and stabilized by confinement within small pores intrinsic to the NU-1000 structure. Experimental evidence allows for identification of spectroscopic similarities between Al-NU-1000 and γ-Al 2O 3. Density functional theory modeling provides structures and simulatedmore » spectra the relevance of which can be assessed via comparison to experimental IR and EXAFS data. As a result, the catalytic performance of Al-NU-1000 has been benchmarked against γ-Al 2O 3, with promising results in terms of selectivity.« less

METHOD OF FORMING A PROTECTIVE COATING ON FERROUS METAL SURFACES

DOEpatents

Schweitzer, D.G.; Weeks, J.R.; Kammerer, O.F.; Gurinsky, D.H.

1960-02-23

A method is described of protecting ferrous metal surfaces from corrosive attack by liquid metals, such as liquid bismuth or lead-bismuth alloys. The nitrogen content of the ferrous metal surface is first reduced by reacting the metal surface with a metal which forms a stable nitride. Thereafter, the surface is contacted with liquid metal containing at least 2 ppm zirconium at a temperature in the range of 550 to 1100 deg C to form an adherent zirconium carbide layer on the ferrous surface.

Improved fill factor in inverted planar perovskite solar cells with zirconium acetate as the hole-and-ion-blocking layer.

PubMed

Zhang, Xuewen; Liang, Chunjun; Sun, Mengjie; Zhang, Huimin; Ji, Chao; Guo, Zebang; Xu, Yajun; Sun, Fulin; Song, Qi; He, Zhiqun

2018-03-14

Planar perovskite solar cells (PSCs) have gained great interest due to their low-temperature solution preparation and simple process. In inverted planar PSCs, an additional buffer layer is usually needed on the top of the PCBM electron-transport layer (ETL) to enhance the device performance. In this work, we used a new buffer layer, zirconium acetate (Zr(Ac) 4 ). The inclusion of the Zr(Ac) 4 buffer layer leads to the increase of FF from ∼68% to ∼79% and PCE from ∼14% to ∼17% in the planar PSCs. The UPS measurement indicates that the Zr(Ac) 4 layer has a low HOMO level of -8.2 eV, indicating that the buffer layer can act as a hole-blocking layer. Surface morphology and surface chemistry investigations reveal that the elements I, MA and Pb can diffuse across the PCBM ETL, damaging the device performance. The covering Zr(Ac) 4 molecules fill in the pinholes of the PCBM layer and effectively block the ions/molecules of the perovskite from diffusion across the ETL. The resulting more robust PCBM/Zr(Ac) 4 ETL leads to weaker ionic charge accumulation and lower diode leakage current. The double role of hole-and-ion blocking of the Zr(Ac) 4 layer explains the improved FF and PCE in the PSCs.

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).

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.

Electrochemical study of pre- and post-transition corrosion of Zr alloys in PWR coolant

NASA Astrophysics Data System (ADS)

Macák, Jan; Novotný, Radek; Sajdl, Petr; Renčiuková, Veronika; Vrtílková, Věra

Corrosion properties of Zr-Sn and Zr-Nb zirconium alloys were studied under simulated PWR conditions (or, more exactly, VVER conditions — boric acid, potassium hydroxide, lithium hydroxide) at temperatures up to 340°C and 15MPa using in-situ electrochemical impedance spectroscopy (EIS) and polarization measurements. EIS spectra were obtained in a wide range of frequencies (typically 100kHz — 100μHz). It enabled to gain information of both dielectric properties of oxide layers developing on the Zr-alloys surface and of the kinetics of the corrosion process and the associated charge and mass transfer phenomena. Experiments were run for more than 380 days; thus, the study of all the corrosion stages (pre-transition, transition, post-transition) was possible.

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.

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

High performance polymer solar cells with as-prepared zirconium acetylacetonate film as cathode buffer layer

PubMed Central

Tan, Zhan'ao; Li, Shusheng; Wang, Fuzhi; Qian, Deping; Lin, Jun; Hou, Jianhui; Li, Yongfang

2014-01-01

Low-work-function active metals are commonly used as cathode in polymer solar cells (PSCs), but sensitivity of the active metals towards moisture and oxygen results in poor stability of the devices. Therefore, solution-proceessable and stable cathode buffer layer is of great importance for the application of PSCs. Here we demonstrate high performance PSCs by employing as-prepared zirconium acetylacetonate (a-ZrAcac) film spin-cast from its ethanol solution as cathode buffer layer. The PSCs based on a low bandgap polymer PBDTBDD as donor and PC60BM as acceptor with a-ZrAcac/Al cathode demonstrated an average power conversion efficiency (PCE) of 8.75% which is significantly improved than that of the devices with traditional Ca/Al cathode. The improved photovoltaic performance is benefitted from the decreased series resistance and enhanced light harvest of the PSCs with the a-ZrAcac/Al cathode. The results indicate that a-ZrAcac is a promising high performance cathode buffer layer for fabricating large area flexible PSCs. PMID:24732976

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.

Evaluation of dip and spray coating techniques in corrosion inhibition of AA2024 alloy using a silicon/zirconium sol-gel film as coating

NASA Astrophysics Data System (ADS)

Garcia, R. B. R.; Silva, F. S.; Kawachi, E. Y.

2017-02-01

For corrosion protection of aluminum alloy AA2024 -T3 a silicon/zirconium films were obtained via sol-gel process, prepared from tetraethoxysilane and zirconium acetate, in acid medium with a 5 wt% of nonionic surfactant in order to replace the pre-treatment based on chromium conversion coatings. A homogeneous film was obtained and deposited, at low viscosity condition of the sol (˜10cP), by dip and spray coating techniques. The films morphology was evaluated by Scanning Electron Microscopy (SEM), and to know more about the used deposition methodology, the deposited mass and the film thickness were measured. The corrosion protection efficiency of deposited films was evaluated by potentiodynamic polarization. The film deposition by both dip and spray coatings were effective for the deposition of a homogeneous film layer, and the results showed the thickness is directly related with the deposited mass, and the film deposited by spray technique presented the lower value. Potentiodynamic polarization indicated that the film deposited by spray coating apparently has a better inert ceramic film due the polarization resistance increased around 57% against 27 and 14% of dip coating samples (4 and 1 layer, respectively).

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

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

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.

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.

Eudialyte-group minerals in rocks of Lovozero layered complex at Mt. Karnasurt and Mt. Kedykvyrpakhk

NASA Astrophysics Data System (ADS)

Ivanyuk, G. Yu.; Pakhomovsky, Ya. A.; Yakovenchuk, V. N.

2015-12-01

Eudialyte-bearing interbeds within layers I-4 (Mt. Karnasurt) and II-4 (Mt. Kedykvyrpakhk) in the layered complex of the Lovozero Pluton are localized symmetrically relative to the loparite-bearing ijolite-malignite layer; the content of eudialyte decreases from underlying nepheline syenite to overlying foidolite. Eudialyte-group minerals fill the interstices between nepheline, sodalite, and microcline-perthite crystals in all rock types and are partially replaced with georgechaoite and minerals of the lovozerite group as a result of hydrothermal alteration. Variations in the chemical composition of the eudialyte-group minerals are mainly controlled by block substitution NaFeZrCl ↔ LnMn(Nb,Ti)S producing eudialyte proper, manganoeudialyte (sharply predominant), kentbrooksite, alluaivite, and a phase intermediate between manganoeudialyte and alluaivite. As the total Ln2O3 content increases, the relative amounts of Ce and La oxides increases linearly in the proportion Ce2O3: La2O3 = 2.5: 1. In the phases containing lower than 3 wt % La2O3, Nd becomes the next REE after Ce. It is very likely that (mangano)eudialyte was mostly formed after parakeldyshite and other anhydrous zirconium-silicate under effect of residual fluids enriched in Ca and Mn, which took part in fenitization of basalt, tuff, and tuffite of the Lovozero Formation.

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

Effects of Plasma ZrN Metallurgy and Shot Peening Duplex Treatment on Fretting Wear and Fretting Fatigue Behavior of Ti6Al4V Alloy.

PubMed

Tang, Jingang; Liu, Daoxin; Zhang, Xiaohua; Du, Dongxing; Yu, Shouming

2016-03-23

A metallurgical zirconium nitride (ZrN) layer was fabricated using glow metallurgy using nitriding with zirconiuming prior treatment of the Ti6Al4V alloy. The microstructure, composition and microhardness of the corresponding layer were studied. The influence of this treatment on fretting wear (FW) and fretting fatigue (FF) behavior of the Ti6Al4V alloy was studied. The composite layer consisted of an 8-μm-thick ZrN compound layer and a 50-μm-thick nitrogen-rich Zr-Ti solid solution layer. The surface microhardness of the composite layer is 1775 HK 0.1 . A gradient in cross-sectional microhardness distribution exists in the layer. The plasma ZrN metallurgical layer improves the FW resistance of the Ti6Al4V alloy, but reduces the base FF resistance. This occurs because the improvement in surface hardness results in lowering of the toughness and increasing in the notch sensitivity. Compared with shot peening treatment, plasma ZrN metallurgy and shot peening composite treatment improves the FW resistance and enhances the FF resistance of the Ti6Al4V alloy. This is attributed to the introduction of a compressive stress field. The combination of toughness, strength, FW resistance and fatigue resistance enhance the FF resistance for titanium alloy.

Effects of Plasma ZrN Metallurgy and Shot Peening Duplex Treatment on Fretting Wear and Fretting Fatigue Behavior of Ti6Al4V Alloy

PubMed Central

Tang, Jingang; Liu, Daoxin; Zhang, Xiaohua; Du, Dongxing; Yu, Shouming

2016-01-01

A metallurgical zirconium nitride (ZrN) layer was fabricated using glow metallurgy using nitriding with zirconiuming prior treatment of the Ti6Al4V alloy. The microstructure, composition and microhardness of the corresponding layer were studied. The influence of this treatment on fretting wear (FW) and fretting fatigue (FF) behavior of the Ti6Al4V alloy was studied. The composite layer consisted of an 8-μm-thick ZrN compound layer and a 50-μm-thick nitrogen-rich Zr–Ti solid solution layer. The surface microhardness of the composite layer is 1775 HK0.1. A gradient in cross-sectional microhardness distribution exists in the layer. The plasma ZrN metallurgical layer improves the FW resistance of the Ti6Al4V alloy, but reduces the base FF resistance. This occurs because the improvement in surface hardness results in lowering of the toughness and increasing in the notch sensitivity. Compared with shot peening treatment, plasma ZrN metallurgy and shot peening composite treatment improves the FW resistance and enhances the FF resistance of the Ti6Al4V alloy. This is attributed to the introduction of a compressive stress field. The combination of toughness, strength, FW resistance and fatigue resistance enhance the FF resistance for titanium alloy. PMID:28773345

Properties of calcium silicate-monobasic calcium phosphate materials for endodontics containing tantalum pentoxide and zirconium oxide.

PubMed

Zamparini, Fausto; Siboni, Francesco; Prati, Carlo; Taddei, Paola; Gandolfi, Maria Giovanna

2018-05-08

The aim of the study was to evaluate chemical-physical properties and apatite-forming ability of three premixed calcium silicate materials containing monobasic calcium phosphate (CaH 4 P 2 O 8 ) bioceramic, tantalum pentoxide and zirconium oxide, recently marketed for endodontics (TotalFill BC-Sealer, BC-RRM-Paste, BC-RRM-Putty). Microchemical and micromorphological analyses, radiopacity, initial and final setting times, calcium release and alkalising activity were tested. The nucleation of calcium phosphates (CaPs) and/or apatite after 28 days ageing was evaluated by ESEM-EDX and micro-Raman spectroscopy. BC-Sealer and BC-RRM-Paste showed similar initial (23 h), prolonged final (52 h) setting times and good radiopacity (> 7 mm Al); BC-RRM-Putty showed fast initial (2 h) and final setting times (27 h) and excellent radiopacity (> 9 mm Al). All materials induced a marked alkalisation (pH 11-12) up to 28 days and showed the release of calcium ions throughout the entire test period (cumulative calcium release 641-806 ppm). After 28 days ageing, a well-distributed mineral layer was present on all samples surface; EDX demonstrated relevant calcium and phosphorous peaks. B-type carbonated apatite and calcite deposits were identified by micro-Raman spectroscopy on all the 28-day-aged samples; the deposit thickness was higher on BC-RRM-Paste and BC-RRM-Putty, in agreement with calcium release data. These materials met the required chemical and physical standards and released biologically relevant ions. The CaSi-CaH 4 P 2 O 8 system present in the materials provided Ca and OH ions release with marked abilities to nucleate a layer of B-type carbonated apatite favoured/accelerated by the bioceramic presence. The ability to nucleate apatite may lead many clinical advantages: In orthograde endodontics, it may improve the sealing ability by the deposition of CaPs at the material-root dentine interface, and in endodontic surgery, it could promote bone and periodontal tissue regeneration. As premixed materials, their application in endodontics may result easier in several complex endodontic situations (apicoectomy, root perforation, presence of wide/wet apices).

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.

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...

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...

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.

Atomic layer deposition of zirconium silicate films using zirconium tetra-tert-butoxide and silicon tetrachloride

NASA Astrophysics Data System (ADS)

Kim, Won-Kyu; Kang, Sang-Woo; Rhee, Shi-Woo

2003-09-01

A new precursor combination (SiCl4 and Zr(OtC4H9)4) was used to deposit Zr silicate with Zr(OtC4H9)4 as a zirconium source and oxygen source at the same time. SiCl4 and Zr(OtC4H9)4 have higher vapor pressures than their counterpart, ZrCl4 and tetra-n-butyl orthosilicate (TBOS), and it was expected that the cycle time would be shorter. The deposition temperature of the new combination was about 150 °C lower than that of ZrCl4 and TBOS. The film was zirconium rich while it was silicon rich with ZrCl4 and TBOS. Growth rate (nm/cycle), composition ratio [Zr/(Zr+Si)], and chlorine impurity were decreased with increasing deposition temperature from 125 to 225 °C. The composition ratio of the film deposited at 225 °C was 0.53 and the chlorine content was about 0.4 at. %. No carbon was detected by x-ray photoelectron spectroscopy.

Influence of Ar-irradiation on structural and nanomechanical properties of pure zirconium measured by means of GIXRD and nanoindentation techniques

NASA Astrophysics Data System (ADS)

Kurpaska, L.; Gapinska, M.; Jasinski, J.; Lesniak, M.; Sitarz, M.; Nowakowska-Langier, K.; Jagielski, J.; Wozniak, K.

2016-12-01

An effect of Ar-irradiation on structural and nanomechanical properties of pure zirconium at room temperature was investigated. In order to simulate the radiation damage, the argon ions were implanted into the pure zirconium coupons with fluences ranging from 1 × 1015 to 1 × 1017 cm-2. Prior to irradiation, zirconium samples were chemically polished with a solution of HF/HNO3/H2O. Structural properties of the implanted layer were studied using Grazing Incidence X-Ray Diffraction (GIXRD) technique. The nanomechanical properties of the material were measured by means of nanoindentation technique. The obtained results revealed correlation between Ar-implantation fluence, hardness and structural properties (as confirmed by the modification of the diffraction peaks). Material hardening and peak shift & broadening in GIXD spectra were associated with the local increase of micro-strains, which is related to the increased density of type - dislocation loops. Presented study confirms that the structural changes induced by ion irradiation are directly linked to the mechanical response of the sample.

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

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.

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.

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.

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

High Temperature Materials for Chemical Propulsion Applications

NASA Technical Reports Server (NTRS)

Elam, Sandra; Hickman, Robert; O'Dell, Scott

2007-01-01

Radiation or passively cooled thrust chambers are used for a variety of chemical propulsion functions including apogee insertion, reaction control for launch vehicles, and primary propulsion for planetary spacecraft. The performance of these thrust chambers is limited by the operating temperature of available materials. Improved oxidation resistance and increased operating temperatures can be achieved with the use of thermal barrier coatings such as zirconium oxide (ZrO2) and hafnium oxide (HfO2). However, previous attempts to include these materials showed cracking and spalling of the oxide layer due to poor bonding. Current research at NASA's Marshall Space Flight Center (MSFC) has generated unique, high temperature material options for in-space thruster designs that are capable of up to 2500 C operating temperatures. The research is focused on fabrication technologies to form low cost Iridium,qF_.henium (Ir/Re) components with a ceramic hot wall created as an integral, functionally graded material (FGM). The goal of this effort is to further de?celop proven technologies for embedding a protective ceramic coating within the Ir/Re liner to form a robust functional gradient material. Current work includes the fabrication and testing of subscale samples to evaluate tensile, creep, thermal cyclic/oxidation, and thermophysical material properties. Larger test articles have also being fabricated and hot-fire tested to demonstrate the materials in prototype thrusters at 1O0 lbf thrust levels.

Diamond-like carbon coatings with zirconium-containing interlayers for orthopedic implants.

PubMed

Choudhury, Dipankar; Lackner, Juergen; Fleming, Robert A; Goss, Josh; Chen, Jingyi; Zou, Min

2017-04-01

Six types of diamond-like carbon (DLC) coatings with zirconium (Zr)-containing interlayers on titanium alloy (Ti-6Al-4V) were investigated for improving the biotribological performance of orthopedic implants. The coatings consist of three layers: above the substrate a layer stack of 32 alternating Zr and ZrN sublayers (Zr:ZrN), followed by a layer comprised of Zr and DLC (Zr:DLC), and finally a N-doped DLC layer. The Zr:ZrN layer is designed for increasing load carrying capacity and corrosion resistance; the Zr:DLC layer is for gradual transition of stress, thus enhancing layer adhesion; and the N-doped DLC layer is for decreasing friction, squeaking noises and wear. Biotribological experiments were performed in simulated body fluid employing a ball-on-disc contact with a Si 3 N 4 ball and a rotational oscillating motion to mimic hip motion in terms of gait angle, dynamic contact pressures, speed and body temperature. The results showed that the Zr:DLC layer has a substantial influence on eliminating delamination of the DLC from the substrates. The DLC/Si 3 N 4 pairs significantly reduced friction coefficient, squeaking noise and wear of both the Si 3 N 4 balls and the discs compared to those of the Ti-6Al-4V/Si 3 N 4 pair after testing for a duration that is equivalent to one year of hip motion in vivo. Copyright © 2017 Elsevier Ltd. All rights reserved.

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.

Preparation of magnetron sputtered ZrO2 films on Si for gate dielectric application

NASA Astrophysics Data System (ADS)

Kondaiah, P.; Mohan Rao, G.; Uthanna, S.

2012-11-01

Zirconium oxide (ZrO2) thin films were deposited on to p - Si and quartz substrates by sputtering of zirconium target at an oxygen partial pressure of 4x10-2 Pa and sputter pressure of 0.4 Pa by using DC reactive magnetron sputtering technique. The effect of annealing temperature on structural, optical, electrical and dielectric properties of the ZrO2 films was systematically studied. The as-deposited films were mixed phases of monoclinic and orthorhombic ZrO2. As the annealing temperature increased to 1073 K, the films were transformed in to single phase orthorhombic ZrO2. Fourier transform infrared studies conform the presence of interfacial layer between Si and ZrO2. The optical band gap and refractive index of the as-deposited films were 5.82 eV and 1.81. As the annealing temperature increased to 1073 K the optical band gap and refractive index increased to 5.92 eV and 2.10 respectively. The structural changes were influenced the capacitance-voltage and current-voltage characteristics of Al/ZrO2/p-Si capacitors. The dielectric constant was increased from 11.6 to 24.5 and the leakage current was decreased from 1.65×10-7 to 3.30×10-9 A/ cm2 for the as-deposited and annealed at 1073 K respectively.

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

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

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.

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.

Microstructures and Properties of the C/Zr-O-Si-C Composites Fabricated by Polymer Infiltration and Pyrolysis

NASA Astrophysics Data System (ADS)

Ma, Yan; Chen, Zhaohui

2013-09-01

A way to improve the ablation properties of the C/SiC composites in an oxyacetylene torch environment was investigated by the precursor infiltration and pyrolysis route using three organic precursors (zirconium butoxide, polycarbosilane, and divinylbenzene). The ceramic matrix derived from the precursors at 1200 °C was mainly a mixture of SiC, ZrO2, and C. After annealing at 1600 °C for 1 h, ZrO2 partly transformed to ZrC because of the carbothermic reductions and completely transformed to ZrC at 1800 °C in 1 h. The mechanical properties of the composites decreased with increasing temperature, while the ablation resistance increased due to the increasing content of ZrC. Compared with C/SiC composites, the ablation resistance of the C/Zr-O-Si-C composites overwhelms because of the oxide films which formed on the ablation surfaces. And, the films were composed of two layers: the porous surface layer (the mixture of ZrO2 and SiO2) and the dense underlayer (SiO2).

Effects of Rapid Thermal Annealing on the Structural, Electrical, and Optical Properties of Zr-Doped ZnO Thin Films Grown by Atomic Layer Deposition.

PubMed

Wu, Jingjin; Zhao, Yinchao; Zhao, Ce Zhou; Yang, Li; Lu, Qifeng; Zhang, Qian; Smith, Jeremy; Zhao, Yongming

2016-08-13

The 4 at. % zirconium-doped zinc oxide (ZnO:Zr) films grown by atomic layer deposition (ALD) were annealed at various temperatures ranging from 350 to 950 °C. The structural, electrical, and optical properties of rapid thermal annealing (RTA) treated ZnO:Zr films have been evaluated to find out the stability limit. It was found that the grain size increased at 350 °C and decreased between 350 and 850 °C, while creeping up again at 850 °C. UV-vis characterization shows that the optical band gap shifts towards larger wavelengths. The Hall measurement shows that the resistivity almost keeps constant at low annealing temperatures, and increases rapidly after treatment at 750 °C due to the effect of both the carrier concentration and the Hall mobility. The best annealing temperature is found in the range of 350-550 °C. The ZnO:Zr film-coated glass substrates show good optical and electrical performance up to 550 °C during superstrate thin film solar cell deposition.

Effects of Rapid Thermal Annealing on the Structural, Electrical, and Optical Properties of Zr-Doped ZnO Thin Films Grown by Atomic Layer Deposition

PubMed Central

Wu, Jingjin; Zhao, Yinchao; Zhao, Ce Zhou; Yang, Li; Lu, Qifeng; Zhang, Qian; Smith, Jeremy; Zhao, Yongming

2016-01-01

The 4 at. % zirconium-doped zinc oxide (ZnO:Zr) films grown by atomic layer deposition (ALD) were annealed at various temperatures ranging from 350 to 950 °C. The structural, electrical, and optical properties of rapid thermal annealing (RTA) treated ZnO:Zr films have been evaluated to find out the stability limit. It was found that the grain size increased at 350 °C and decreased between 350 and 850 °C, while creeping up again at 850 °C. UV–vis characterization shows that the optical band gap shifts towards larger wavelengths. The Hall measurement shows that the resistivity almost keeps constant at low annealing temperatures, and increases rapidly after treatment at 750 °C due to the effect of both the carrier concentration and the Hall mobility. The best annealing temperature is found in the range of 350–550 °C. The ZnO:Zr film-coated glass substrates show good optical and electrical performance up to 550 °C during superstrate thin film solar cell deposition. PMID:28773816

Formation of freestanding ZrO{sub 2} nanotubes for Cr(VI) removal

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

Bashirom, Nurulhuda, E-mail: nurulhuda.usm2014@gmail.com; Ye, Beh Chin, E-mail: cyebeh@gmail.com; Razak, Khairunisak Abdul, E-mail: khairunisak@usm.my

2016-07-06

Freestanding ZrO{sub 2} nanotubes (ZNTs) were produced using a simple anodization method in fluorinated ethylene glycol electrolyte containing 1 ml 1 M K{sub 2}CO{sub 3}. The pH of the bath was kept constant at 8. The potassium carbonate (K{sub 2}CO{sub 3}) was added into electrolyte to promote the detachment of anodic ZrO{sub 2} film from the underlying zirconium (Zr) substrate. The poor adherence of ZNTs layer was due to generation of CO{sub 2} gas that was thought to occur between metal|oxide interfaces. The effect of anodization voltages towards the detachment of ZNTs layer was systematically studied at 20 V, 40more » V, 50 V and 60 V for 1 hour. The formation of CO{sub 2} gas is a function of anodization voltage, in which at 60 V, a good anodic film separation seen due to higher formation of CO{sub 2} gas. A preliminary study shown the capability of ZNTs in removing 5 ppm of Cr(VI) aqueous solution under illumination of UV light.« less

Forming mechanism of Te-based conductive-bridge memories

NASA Astrophysics Data System (ADS)

Mendes, M. Kazar; Martinez, E.; Marty, A.; Veillerot, M.; Yamashita, Y.; Gassilloud, R.; Bernard, M.; Renault, O.; Barrett, N.

2018-02-01

We investigated origins of the resistivity change during the forming of ZrTe/Al2O3 based conductive-bridge resistive random access memories. Non-destructive hard X-ray photoelectron spectroscopy was used to investigate redox processes with sufficient depth sensitivity. Results highlighted the reduction of alumina correlated to the oxidation of zirconium at the interface between the solid electrolyte and the active electrode. In addition the resistance switching caused a decrease of Zr-Te bonds and an increase of elemental Te showing an enrichment of tellurium at the ZrTe/Al2O3 interface. XPS depth profiling using argon clusters ion beam confirmed the oxygen diffusion towards the top electrode. A four-layer capacitor model showed an increase of both the ZrO2 and AlOx interfacial layers, confirming the redox process located at the ZrTe/Al2O3 interface. Oxygen vacancies created in the alumina help the filament formation by acting as preferential conductive paths. This study provides a first direct evidence of the physico-chemical phenomena involved in resistive switching of such devices.

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

Conduction mechanism of leakage current due to the traps in ZrO2 thin film

NASA Astrophysics Data System (ADS)

Seo, Yohan; Lee, Sangyouk; An, Ilsin; Song, Chulgi; Jeong, Heejun

2009-11-01

In this work, a metal-oxide-semiconductor capacitor with zirconium oxide (ZrO2) gate dielectric was fabricated by an atomic layer deposition (ALD) technique and the leakage current characteristics under negative bias were studied. From the result of current-voltage curves there are two possible conduction mechanisms to explain the leakage current in the ZrO2 thin film. The dominant mechanism is the space charge limited conduction in the high-electric field region (1.5-5.0 MV cm-1) while the trap-assisted tunneling due to the existence of traps is prevailed in the low-electric field region (0.8-1.5 MV cm-1). Conduction caused by the trap-assisted tunneling is found from the experimental results of a weak temperature dependence of current, and the trap barrier height is obtained. The space charge limited conduction is evidenced, for different temperatures, by Child's law dependence of current density versus voltage. Child's law dependence can be explained by considering a single discrete trapping level and we can obtain the activation energy of 0.22 eV.

The Chemical Composition and Structure of Supported Sulfated Zirconia with Regulated Size Nanoparticles

NASA Astrophysics Data System (ADS)

Kanazhevskiy, V. V.; Shmachkova, V. P.; Kotsarenko, N. S.; Kochubey, D. I.; Vedrine, J. C.

2007-02-01

A set of model skeletal isomerization catalysts — sulfated zirconia nanoparticles of controlled thickness anchored on different supports — was prepared using colloidal solutions of Zr salt on titania as support. The nanoparticles of zirconia (1-5 nm) are epitaxially connected to the support surface, with S/Zr ratio equals to 1.3-1.5. It was shown by EXAFS that nanoparticles of non-stoichiometric zirconium sulfate Zr(SO4)1+x, where x<0.5, are formed on the support surface. Its structure looks like half-period shifted counterdirected chains built-up by zirconium atoms linked by triangle pyramids of sulfate groups. Considering catalytic data of skeletal n-butane isomerisation at 150°C, one can suggest that these species behave as the active component of sulfated zirconia. They are formed in subsurface layers as zirconium hydroxide undergoes sulfation followed by thermal treatment.

Thermally Induced Lateral Motion of α-Zirconium Phosphate Layers Intercalated with Hexadecylamines

NASA Astrophysics Data System (ADS)

Char, Kookheon

2005-03-01

Well-defined intercalated structure, either interdigitated layers or bilayers, of hexadecylamines (HDAs) in a confined space of a highly-functionalized layered material, α- zirconium phosphate (α-ZrP), was prepared and these two distinct intercalated structures can serve as model systems to investigate the interaction of the two monolayers whose amphiphilic tails are adjacent to each other. Acidic functional groups (-POH) on the α-ZrP are in well-ordered array and the number of functional group is quite high (i.e., cationic exchange capacity (CEC) = 664 mmole/100 g, area per one charge site = 0.24 nm^2) enough to realize the bilayers (i.e., discrete two monolayers) of HDAs within the α-ZrP interlayer. We employed the two-step intercalation mechanism for the preparation of well- ordered interdigitated layers as well as the bilayers of alkyl chains attached to both sides of the α-ZrP intergallery. An intriguing lateral motion of the α-ZrP sheets was observed with in-situ SAXS measurements for the interdigitated layer during heating and cooling cycle and verified with TEM. This lateral motion is believed to be due to the transition from the tilted to the untilted conformation of the interdigitated HDA chains and this transition is found to be thermally reversible.

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.

Interdiffusion behavior of U3Si2 with FeCrAl via diffusion couple studies

NASA Astrophysics Data System (ADS)

Hoggan, Rita E.; He, Lingfeng; Harp, Jason M.

2018-04-01

Uranium silicide (U3Si2) is a candidate to replace uranium oxide (UO2) as light water reactor (LWR) fuel because of its higher thermal conductivity and higher fissile density relative to the current standard, UO2. A class of Fe, Cr, Al alloys collectively known as FeCrAl alloys that have superior mechanical and oxidation resistance are being considered as an alternative to the standard Zirconium based LWR cladding. The interdiffusion behavior between FeCrAl and U3Si2 is investigated in this study. Commercially available FeCrAl, along with U3Si2 pellets were placed in diffusion couples. Individual tests were ran at temperatures ranging from 500 °C to 1000 °C for 30 h and 100 h. The interdiffusion was analyzed with an optical microscope, scanning electron microscope, and transmission electron microscope. Uniform and planar interdiffusion layers along the material interface were illustrated with backscatter electron micrographs and energy-dispersive X-ray spectroscopy. Electron diffraction was used to validate phases present in the system, including distinct U2Fe3Si/UFe2 and UFeSi layers at the material interface. U and Fe diffused far into the FeCrAl and U3Si2 matrix, respectively, in the higher temperature tests. No interaction was observed at 500 °C for 30 h.

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.

In-situ high-pressure powder X-ray diffraction study of α-zirconium phosphate.

PubMed

Readman, Jennifer E; Lennie, Alistair; Hriljac, Joseph A

2014-06-01

The high-pressure structural chemistry of α-zirconium phosphate, α-Zr(HPO4)2·H2O, was studied using in-situ high-pressure diffraction and synchrotron radiation. The layered phosphate was studied under both hydrostatic and non-hydrostatic conditions and Rietveld refinement carried out on the resulting diffraction patterns. It was found that under hydrostatic conditions no uptake of additional water molecules from the pressure-transmitting medium occurred, contrary to what had previously been observed with some zeolite materials and a layered titanium phosphate. Under hydrostatic conditions the sample remained crystalline up to 10 GPa, but under non-hydrostatic conditions the sample amorphized between 7.3 and 9.5 GPa. The calculated bulk modulus, K0 = 15.2 GPa, showed the material to be very compressible with the weak linkages in the structure of the type Zr-O-P.

Epitaxial growth of lead zirconium titanate thin films on Ag buffered Si substrates using rf sputtering

NASA Astrophysics Data System (ADS)

Wang, Chun; Laughlin, David E.; Kryder, Mark H.

2007-04-01

Epitaxial lead zirconium titanate (PZT) (001) thin films with a Pt bottom electrode were deposited by rf sputtering onto Si(001) single crystal substrates with a Ag buffer layer. Both PZT(20/80) and PZT(53/47) samples were shown to consist of a single perovskite phase and to have the (001) orientation. The orientation relationship was determined to be PZT(001)[110]‖Pt(001)[110]‖Ag(001)[110]‖Si(001)[110]. The microstructure of the multilayer was studied using transmission electron microscopy (TEM). The electron diffraction pattern confirmed the epitaxial relationship between each layer. The measured remanent polarization Pr and coercive field Ec of the PZT(20/80) thin film were 26μC /cm2 and 110kV/cm, respectively. For PZT(53/47), Pr was 10μC /cm2 and Ec was 80kV/cm.

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.

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.

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.

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.

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.

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.

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.

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.

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).

Atomic structure and composition of the yttria-stabilized zirconia (111) surface.

PubMed

Vonk, Vedran; Khorshidi, Navid; Stierle, Andreas; Dosch, Helmut

2013-06-01

Anomalous and nonanomalous surface X-ray diffraction is used to investigate the atomic structure and composition of the yttria-stabilized zirconia (YSZ)(111) surface. By simulation it is shown that the method is sensitive to Y surface segregation, but that the data must contain high enough Fourier components in order to distinguish between different models describing Y/Zr disorder. Data were collected at room temperature after two different annealing procedures. First by applying oxidative conditions at 10 - 5  mbar O 2 and 700 K to the as-received samples, where we find that about 30% of the surface is covered by oxide islands, which are depleted in Y as compared with the bulk. After annealing in ultrahigh vacuum at 1270 K the island morphology of the surface remains unchanged but the islands and the first near surface layer get significantly enriched in Y. Furthermore, the observation of Zr and oxygen vacancies implies the formation of a porous surface region. Our findings have important implications for the use of YSZ as solid oxide fuel cell electrode material where yttrium atoms and zirconium vacancies can act as reactive centers, as well as for the use of YSZ as substrate material for thin film and nanoparticle growth where defects control the nucleation process.

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.

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.

Layer Formation On Metal Surfaces In Lead-Bismuth At High Temperatures In Presence Of Zirconium

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

Loewen, Eric Paul; Yount, Hannah J.; Volk, Kevin

If the operating temperature lead–bismuth cooled fission reactor could be extended to 800 °C, they could produce hydrogen directly from water. A key issue for the deployment of this technology at these temperatures is the corrosion of the fuel cladding and structural materials by the lead–bismuth. Corrosion studies of several metals were performed to correlate the interaction layer formation rate as a function of time, temperature, and alloy compositions. The interaction layer is defined as the narrow band between the alloy substrate and the solidified lead–bismuth eutectic on the surface. Coupons of HT-9, 410, 316L, and F22 were tested atmore » 550 and 650 °C for 1000 h inside a zirconium corrosion cell. The oxygen potential ranged from approximately 10-22 to 10-19 Pa. Analyses were performed on the coupons to determine the depth of the interaction layer and the composition, at each time step (100, 300, and 1000 h). The thickness of the interaction layer on F22 at 550 °C was 25.3 µm, the highest of all the alloys tested, whereas at 650 °C, the layer thickness was only 5.6 µm, the lowest of all the alloys tested. The growth of the interaction layer on F22 at 650 °C was suppressed, owing to the presence of Zr (at 1500 wppm) in the LBE. In the case of 316L, the interaction layers of 4.9 and 10.6 µm were formed at 550 and 650 °C, respectively.« less

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.

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...

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...

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...

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...

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...

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.

Large-scale self-assembled zirconium phosphate smectic layers via a simple spray-coating process

NASA Astrophysics Data System (ADS)

Wong, Minhao; Ishige, Ryohei; White, Kevin L.; Li, Peng; Kim, Daehak; Krishnamoorti, Ramanan; Gunther, Robert; Higuchi, Takeshi; Jinnai, Hiroshi; Takahara, Atsushi; Nishimura, Riichi; Sue, Hung-Jue

2014-04-01

The large-scale assembly of asymmetric colloidal particles is used in creating high-performance fibres. A similar concept is extended to the manufacturing of thin films of self-assembled two-dimensional crystal-type materials with enhanced and tunable properties. Here we present a spray-coating method to manufacture thin, flexible and transparent epoxy films containing zirconium phosphate nanoplatelets self-assembled into a lamellar arrangement aligned parallel to the substrate. The self-assembled mesophase of zirconium phosphate nanoplatelets is stabilized by epoxy pre-polymer and exhibits rheology favourable towards large-scale manufacturing. The thermally cured film forms a mechanically robust coating and shows excellent gas barrier properties at both low- and high humidity levels as a result of the highly aligned and overlapping arrangement of nanoplatelets. This work shows that the large-scale ordering of high aspect ratio nanoplatelets is easier to achieve than previously thought and may have implications in the technological applications for similar materials.

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.

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.

Evaluation of coated metallic bipolar plates for polymer electrolyte membrane fuel cells

NASA Astrophysics Data System (ADS)

Yoon, Wonseok; Huang, Xinyu; Fazzino, Paul; Reifsnider, Kenneth L.; Akkaoui, Michael A.

Metallic bipolar plates for polymer electrolyte membrane (PEM) fuel cells typically require coatings for corrosion protection. Other requirements for the corrosion protective coatings include low electrical contact resistance, good mechanical robustness, low material and fabrication cost. The authors have evaluated a number of protective coatings deposited on stainless steel substrates by electroplating and physical vapor deposition (PVD) methods. The coatings are screened with an electrochemical polarization test for corrosion resistance; then the contact resistance test was performed on selected coatings. The coating investigated include Gold with various thicknesses (2 nm, 10 nm, and 1 μm), Titanium, Zirconium, Zirconium Nitride (ZrN), Zirconium Niobium (ZrNb), and Zirconium Nitride with a Gold top layer (ZrNAu). The substrates include three types of stainless steel: 304, 310, and 316. The results show that Zr-coated samples satisfy the DOE target for corrosion resistance at both anode and cathode sides in typical PEM fuel cell environments in the short-term, but they do not meet the DOE contact resistance goal. Very thin gold coating (2 nm) can significantly decrease the electrical contact resistance, however a relatively thick gold coating (>10 nm) with our deposition method is necessary for adequate corrosion resistance, particularly for the cathode side of the bipolar plate.

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.

Integrated atomic layer deposition and chemical vapor reaction for the preparation of metal organic framework coatings for solid-phase microextraction Arrow.

PubMed

Lan, Hangzhen; Salmi, Leo D; Rönkkö, Tuukka; Parshintsev, Jevgeni; Jussila, Matti; Hartonen, Kari; Kemell, Marianna; Riekkola, Marja-Liisa

2018-09-18

New chemical vapor reaction (CVR) and atomic layer deposition (ALD)-conversion methods were utilized for preparation of metal organic frameworks (MOFs) coatings of solid phase microextraction (SPME) Arrow for the first time. With simple, easy and convenient one-step reaction or conversion, four MOF coatings were made by suspend ALD iron oxide (Fe 2 O 3 ) film or aluminum oxide (Al 2 O 3 ) film above terephthalic acid (H 2 BDC) or trimesic acid (H 3 BTC) vapor. UIO-66 coating was made by zirconium (Zr)-BDC film in acetic acid vapor. As the first documented instance of all-gas phase synthesis of SPME Arrow coatings, preparation parameters including CVR/conversion time and temperature, acetic acid volume, and metal oxide film/metal-ligand films thickness were investigated. The optimal coatings exhibited crystalline structures, excellent uniformity, satisfactory thickness (2-7.5 μm), and high robustness (>80 times usage). To study the practical usefulness of the coatings for the extraction, several analytes with different chemical properties were tested. The Fe-BDC coating was found to be the most selective and sensitive for the determination of benzene ring contained compounds due to its highly hydrophobic surface and unsaturated metal site. UIO-66 coating was best for small polar, aromatic, and long chain polar compounds owing to its high porosity. The usefulness of new coatings were evaluated for gas chromatography-mass spectrometer (GC-MS) determination of several analytes, present in wastewater samples at three levels of concentration, and satisfactory results were achieved. Copyright © 2018 Elsevier B.V. All rights reserved.

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.

Solid State Research.

DTIC Science & Technology

1995-05-15

cooled to room temperature. Titanium isopropoxide and zirconium n-propoxide were then added (inside a glove box) to levels that correspond to the...ously patterned with a 200-nm-thick evaporated platinum film. In addition to the platinum there was a 40-nm titanium adhesion layer between the...an etch composed of buffered HF, HC1 and H20 [6]. By using a photoresist lift-off process, the top titanium -gold layer is formed, which provides the

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

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

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.

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.

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.

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

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

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.

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

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.

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.

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.

Low-temperature, solution-processed ZrO2:B thin film: a bifunctional inorganic/organic interfacial glue for flexible thin-film transistors.

PubMed

Park, Jee Ho; Oh, Jin Young; Han, Sun Woong; Lee, Tae Il; Baik, Hong Koo

2015-03-04

A solution-processed boron-doped peroxo-zirconium oxide (ZrO2:B) thin film has been found to have multifunctional characteristics, providing both hydrophobic surface modification and a chemical glue layer. Specifically, a ZrO2:B thin film deposited on a hydrophobic layer becomes superhydrophilic following ultraviolet-ozone (UVO) treatment, whereas the same treatment has no effect on the hydrophobicity of the hydrophobic layer alone. Investigation of the ZrO2:B/hydrophobic interface layer using angle-resolved X-ray photoelectron spectroscopy (AR XPS) confirmed it to be chemically bonded like glue. Using the multifunctional nature of the ZrO2:B thin film, flexible amorphous indium oxide (In2O3) thin-film transistors (TFTs) were subsequently fabricated on a polyimide substrate along with a ZrO2:B/poly-4-vinylphenol (PVP) dielectric. An aqueous In2O3 solution was successfully coated onto the ZrO2:B/PVP dielectric, and the surface and chemical properties of the PVP and ZrO2:B thin films were analyzed by contact angle measurement, atomic force microscopy (AFM), Fourier transform infrared (FT-IR) spectroscopy, and X-ray photoelectron spectroscopy (XPS). The surface-engineered PVP dielectric was found to have a lower leakage current density (Jleak) of 4.38 × 10(-8) A/cm(2) at 1 MV/cm, with no breakdown behavior observed up to a bending radius of 5 mm. In contrast, the electrical characteristics of the flexible amorphous In2O3 TFT such as on/off current ratio (Ion/off) and electron mobility remained similar up to 10 mm of bending without degradation, with the device being nonactivated at a bending radius of 5 mm. These results suggest that ZrO2:B thin films could be used for low-temperature, solution-processed surface-modified flexible devices.

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...

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...

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...

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...

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...

Electrical insulator assembly with oxygen permeation barrier

DOEpatents

Van Der Beck, R.R.; Bond, J.A.

1994-03-29

A high-voltage electrical insulator for electrically insulating a thermoelectric module in a spacecraft from a niobium-1% zirconium alloy wall of a heat exchanger filled with liquid lithium while providing good thermal conductivity between the heat exchanger and the thermoelectric module. The insulator has a single crystal alumina layer (SxAl[sub 2]O[sub 3], sapphire) with a niobium foil layer bonded thereto on the surface of the alumina crystal facing the heat exchanger wall, and a molybdenum layer bonded to the niobium layer to act as an oxygen permeation barrier to preclude the oxygen depleting effects of the lithium from causing undesirable niobium-aluminum intermetallic layers near the alumina-niobium interface. 3 figures.

[Determination of americium-241 in urine].

PubMed

Shvydko, N S; Mikhaĭlova, O A; Popov, D K

1988-01-01

A technique has been developed for the determination of americium 241 in urine by a radiochemical purification of the nuclide from uranium (upon co-precipitation of americium 241 with calcium and lanthanum), plutonium, thorium, and polonium 210 (upon co-precipitation of these radionuclides with zirconium iodate). alpha-Radioactivity was measured either in a thick layer of the americium 241 precipitate with a nonisotope carrier or in thin-layer preparations after electrolytic precipitation of americium 241 on a cathode.

Thermal barrier coating

DOEpatents

Bowker, Jeffrey Charles; Sabol, Stephen M.; Goedjen, John G.

2001-01-01

A thermal barrier coating for hot gas path components of a combustion turbine based on a zirconia-scandia system. A layer of zirconium scandate having the hexagonal Zr.sub.3 Sc.sub.4 O.sub.12 structure is formed directly on a superalloy substrate or on a bond coat formed on the substrate.

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

Synthesis, integration, and characterization of metal oxide films as alternative gate dielectric materials

NASA Astrophysics Data System (ADS)

Lin, You-Sheng

ZrO2 and HfO2 were investigated in this study to replace SiO2 as the potential gate dielectric materials in metal-oxide-semiconductor field effect transistors. ZrO2 and HfO2 films were deposited on p-type Si (100) wafers by an atomic layer chemical vapor deposition (ALCVD) process using zirconium (IV) t-butoxide and hafnium (IV) t-butoxide as the metal precursors, respectively. Oxygen was used alternatively with these metal alkoxide precursors into the reactor with purging and evacuation in between. The as-deposited ZrO2 and HfO2 films were stoichiometric and uniform based on X-ray photoemission spectroscopy and ellipsometry measurements. X-ray diffraction analysis indicated that the deposited films were amorphous, however, the high-resolution transmission electron microscopy showed an interfacial layer formation on the silicon substrate. Time-of-flight secondary ion mass spectrometry and medium energy ion scattering analysis showed significant intermixing between metal oxides and Si, indicating the formation of metal silicates, which were confirmed by their chemical etching resistance in HF solutions. The thermal stability of ZrO2 and HfO2 thin films on silicon was examined by monitoring their decomposition temperatures in ultra-high vacuum, using in-situ synchrotron radiation ultra-violet photoemission spectroscopy. The as-deposited ZrO2 and HfO2 thin films were thermally stable up to 880°C and 950°C in vacuum, respectively. The highest achieveable dielectric constants of as-deposited ZrO 2 and HfO2 were 21 and 24, respectively, which were slightly lower than the reported dielectric constants of bulk ZrO2 and HfO 2. These slight reductions in dielectric constants were attributed to the formation of the interfacial metal silicate layers. Very small hysteresis and interface state density were observed for both metal oxide films. Their leakage currents were a few orders of magnitude lower than that of SiO 2 at the same equivalent oxide thickness. NMOSFETs were also fabricated with the as-deposited metal oxide films, and reasonable ID-V D and IG-VG results were obtained. The electron mobilities were high from devices built using a plasma etching process to pattern the metal oxide films. However, they can be degraded if an HF wet etching process was used due to the large contact resistences. Upon oxygen annealing, the formation of SiOx at the interface improved the thermal stability of the as-deposited metal oxide films, however, lower overall dielectric constant and higher leakage current were observed. Upon ammonia annealing, the formation of SiOxNy improved not only the thermal stability but also reduced the leakage current. However, the overall dielectric constant of the film was still reduced due to the formation of the additional interfacial layer.

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.

A mediator-free glucose biosensor based on glucose oxidase/chitosan/α-zirconium phosphate ternary biocomposite.

PubMed

Liu, Li-Min; Wen, Jiwu; Liu, Lijun; He, Deyong; Kuang, Ren-yun; Shi, Taqing

2014-01-15

A novel glucose oxidase/chitosan/α-zirconium phosphate (GOD/chitosan/α-ZrP) ternary biocomposite was prepared by co-intercalating glucose oxidase (GOD) and chitosan into the interlayers of α-zirconium phosphate (α-ZrP) via a delamination-reassembly procedure. The results of X-ray diffraction, infrared spectroscopy, circular dichroism, and ultraviolet spectrum characterizations indicated not only the layered and hybrid structure of the GOD/chitosan/α-ZrP ternary biocomposite but also the recovered activity of the intercalated GOD improved by the co-intercalated chitosan. By depositing the GOD/chitosan/α-ZrP biocomposite film onto a glassy carbon electrode, the direct electrochemistry of the intercalated GOD was achieved with a fast electron transfer rate constant, k(s), of 7.48±3.52 s(-1). Moreover, this GOD/chitosan/α-ZrP biocomposite modified electrode exhibited a sensitive response to glucose in the linear range of 0.25-8.0 mM (R=0.9994, n=14), with a determination limit of 0.076 mM. Copyright © 2013 Elsevier Inc. All rights reserved.

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

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.

An Impact of Zirconium Doping of Zn-Al Braze on the Aluminum-Stainless Steel Joints Integrity During Aging

NASA Astrophysics Data System (ADS)

Yang, Jinlong; Xue, Songbai; Sekulic, Dusan P.

2017-01-01

This work offers an analysis of the microstructure and the growth rate of an intermetallic compound within the aged AA 6061 aluminum alloy-304 stainless steel joint brazed with Zn-15Al and Zn-15Al-0.2Zr filler metals. The effect of zirconium addition on mechanical integrity of the brazed joint was studied. The experimental results confirm that the thickness of the Fe-Al intermetallic layer formed at the brazed seam/stainless steel interface increases with the increase of the aging time. Furthermore, it is established that the growth rate of the intermetallic layer for the Zn-15Al-0.2Zr brazed joint was lower than that for Zn-15Al. The results also indicate that the shear strength of both Zn-15Al and Zn-15Al-0.2Zr brazed joints decreases monotonously during aging. The value of the strength after aging lasting for 800 h for Zn-15Al and Zn-15Al-0.2Zr has decreased by 20 and 17%, respectively. The fracture of joints occurred at the interface between the brazed seam and the Fe4Al13 intermetallic layer. The morphology of the surfaces exhibits a cleavage fracture.

Impact of lysozyme on stability mechanism of nanozirconia aqueous suspension

NASA Astrophysics Data System (ADS)

Szewczuk-Karpisz, Katarzyna; Wiśniewska, Małgorzata

2016-08-01

The effect of lysozyme (LSZ) presence on the zirconium(IV) oxide (ZrO2) aqueous suspension stability was examined. The applied zirconia contains mesopores (with a diameter about 30 nm) and its mean particle size is about 100 nm. To determine the stability mechanism of ZrO2 suspension in the biopolymer presence, the adsorption and electrokinetic (surface charge density and zeta potential) measurements were performed in the pH range 3-10. The lysozyme adsorption on the nanozirconia surface proceeds mainly through electrostatic forces. Under solid-polymer repulsion conditions, there is no adsorption of lysozyme (pH < 6, CNaCl 0.01 mol/dm3). The increase of solution ionic strength to 0.2 mol/dm3 causes screening of unfavourable forces and biopolymer adsorption becomes possible. The LSZ addition to the ZrO2 suspension influences its stability. At pH 3, 4.6 and 7.6, slight improvement of the system stability was obtained. In turn, at pH 9 considerable destabilization of nanozirconia particles covered by polymeric layers occurs.

Modeling of complex wear behavior associated with grid-to-rod fretting in light water nuclear reactors

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

Blau, P. J.; Qu, J.; Lu, R.

One significant concern in the operation of light water nuclear reactors is the fretting wear damage to fuel cladding from flow-induced vibrations. For years, research on the grid-to-rod fretting (GTRF) phenomena has been underway in countries where nuclear power production is a significant industry. Under the auspices of the U.S. Department of Energy Consortium for Advanced Simulation of Light Water Reactors, an effort has been underway to develop and test an engineering wear model for zirconium alloy fuel rod cladding against a supporting grid. Furthermore, the multi-stage model accounts for oxide layers and wear rate transitions. Our paper describes themore » basis for a GTRF engineering wear model, the physical significance of the wear factor it contains, and recent progress toward model validation based on a fretting wear testing apparatus that accounts for coolant temperature, pressure, and the presence of periodic impacts (gaps) in grid/rod contact.« less

Modeling of complex wear behavior associated with grid-to-rod fretting in light water nuclear reactors

DOE PAGES

Blau, P. J.; Qu, J.; Lu, R.

2016-09-21

One significant concern in the operation of light water nuclear reactors is the fretting wear damage to fuel cladding from flow-induced vibrations. For years, research on the grid-to-rod fretting (GTRF) phenomena has been underway in countries where nuclear power production is a significant industry. Under the auspices of the U.S. Department of Energy Consortium for Advanced Simulation of Light Water Reactors, an effort has been underway to develop and test an engineering wear model for zirconium alloy fuel rod cladding against a supporting grid. Furthermore, the multi-stage model accounts for oxide layers and wear rate transitions. Our paper describes themore » basis for a GTRF engineering wear model, the physical significance of the wear factor it contains, and recent progress toward model validation based on a fretting wear testing apparatus that accounts for coolant temperature, pressure, and the presence of periodic impacts (gaps) in grid/rod contact.« less

Evidence for independent motional processes on the two interstitial sublattices of a layer-structured metal hydride: Hydrogen spin-lattice relaxation and motional narrowing in zirconium monohalide hemihydrides, ZrXH0.5

NASA Astrophysics Data System (ADS)

Hwang, T. Y.; Schoenberger, R. J.; Torgeson, D. R.; Barnes, R. G.

1983-01-01

We report the results of a proton-magnetic-resonance investigation of hydrogen location and motion in the hemihydrides ZrXH0.5 of the metallic layer-structured monohalides ZrX of zirconium (X=Br,Cl). Wide-line and pulsed NMR methods were employed to measure the temperature dependence of the linewidth and second moment and of the spin-lattice relaxation time in the laboratory and rotating frames. The results indicate that hydrogen forms an ordered structure on the tetrahedral (T) interstitial sublattice within the Zr metal bilayers, with some (small) random occupancy of octahedral (O) sites. Two stages of motional narrowing observed in the wide-line measurements and double minima found in the relaxation times are consistent with the occurrence of essentially independent hydrogen motional processes on the T and O interstitial sublattices. Hydrogen site occupancy probabilities, jump frequencies, activation energies for hydrogen diffusion, and conduction-electron contributions to the proton spin-lattice relaxation rate are deduced from the measurements.

Fabrication and Characterization of Nanoporous Niobia, and Nanotubular Tantala, Titania and Zirconia via Anodization

PubMed Central

Minagar, Sepideh; Berndt, Christopher C.; Wen, Cuie

2015-01-01

Valve metals such as titanium (Ti), zirconium (Zr), niobium (Nb) and tantalum (Ta) that confer a stable oxide layer on their surfaces are commonly used as implant materials or alloying elements for titanium-based implants, due to their exceptional high corrosion resistance and excellent biocompatibility. The aim of this study was to investigate the bioactivity of the nanostructures of tantala (Ta2O5), niobia (Nb2O5), zirconia (ZrO2) and titania (TiO2) in accordance to their roughness and wettability. Therefore, four kinds of metal oxide nanoporous and nanotubular Ta2O5, Nb2O5, ZrO2 and TiO2 were fabricated via anodization. The nanosize distribution, morphology and the physical and chemical properties of the nanolayers and their surface energies and bioactivities were investigated using SEM-EDS, X-ray diffraction (XRD) analysis and 3D profilometer. It was found that the nanoporous Ta2O5 exhibited an irregular porous structure, high roughness and high surface energy as compared to bare tantalum metal; and exhibited the most superior bioactivity after annealing among the four kinds of nanoporous structures. The nanoporous Nb2O5 showed a uniform porous structure and low roughness, but no bioactivity before annealing. Overall, the nanoporous and nanotubular layers of Ta2O5, Nb2O5, ZrO2 and TiO2 demonstrated promising potential for enhanced bioactivity to improve their biomedical application alone or to improve the usage in other biocompatible metal implants. PMID:25837724

pH-sensitive ion-selective field-effect transistor with zirconium dioxide film

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

Vlasov, Yu.G.; Bratov, A.V.; Tarantov, Yu.A.

1988-09-20

Miniature semiconductor pH sensors for liquid media, i.e., ion-selective field-effect transistors (ISFETs), are silicon field-effect transistors with a two-layer dielectric consisting of a passivating SiO/sub 2/ layer adjoining the silicon and a layer of pH-sensitive material in contact with the electrolyte solution to be tested. This study was devoted to the characteristics of pH-sensitive ISFETs with ZrO/sub 2/ films. The base was p-type silicon (KDB-10) with a (100) surface orientation. A ZrO/sub 2/ layer 10-50 nm thick was applied over the SiO/sub 2/ layer by electron-beam deposition. The measurements were made in aqueous KNO/sub 3/ or KCl solutions.

Electrical insulator assembly with oxygen permeation barrier

DOEpatents

Van Der Beck, Roland R.; Bond, James A.

1994-01-01

A high-voltage electrical insulator (21) for electrically insulating a thermoelectric module (17) in a spacecraft from a niobium-1% zirconium alloy wall (11) of a heat exchanger (13) filled with liquid lithium (16) while providing good thermal conductivity between the heat exchanger and the thermoelectric module. The insulator (21) has a single crystal alumina layer (SxAl.sub.2 O.sub.3, sapphire) with a niobium foil layer (32) bonded thereto on the surface of the alumina crystal (26) facing the heat exchanger wall (11), and a molybdenum layer (31) bonded to the niobium layer (32) to act as an oxygen permeation barrier to preclude the oxygen depleting effects of the lithium from causing undesirable niobium-aluminum intermetallic layers near the alumina-niobium interface.

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.

The study of the modes of Ta-Zr powder mixture non-vacuum electron-beam cladding on the surface of the cp-titanium plates

NASA Astrophysics Data System (ADS)

Samoylenko, V. V.; Lozhkina, E. A.; Polyakov, I. A.; Lenivtseva, O. G.; Ivanchik, I. S.; Matts, O. E.

2016-11-01

The effect of the modes of non-vacuum electron-beam cladding of Ta-Zr powder mixtures on the structure and properties of the layers formed on the surface of cp-titanium were studied. The mode of the electron-beam alloying of titanium with zirconium and tantalum, which ensured the formation of a defect-free layer with a high content of alloying elements was selected. Metallographic examination indicated the presence of a dendritic- and plate-type structure of cladded layers. The microhardness of the layers, formed at the optimum mode, was not changed in the cross section and was equal to 450 HV.

Effects of heat treatment on U-Mo fuel foils with a zirconium diffusion barrier

NASA Astrophysics Data System (ADS)

Jue, Jan-Fong; Trowbridge, Tammy L.; Breckenridge, Cynthia R.; Moore, Glenn A.; Meyer, Mitchell K.; Keiser, Dennis D.

2015-05-01

A monolith fuel design based on U-Mo alloy has been selected as the fuel type for conversion of the United States' high performance research reactors (HPRRs) from highly enriched uranium (HEU) to low-enriched uranium (LEU). In this fuel design, a thin layer of zirconium is used to eliminate the direct interaction between the U-Mo fuel meat and the aluminum-alloy cladding during irradiation. The co-rolling process used to bond the Zr barrier layer to the U-Mo foil during fabrication alters the microstructure of both the U-10Mo fuel meat and the U-Mo/Zr interface. This work studied the effects of post-rolling annealing treatment on the microstructure of the co-rolled U-Mo fuel meat and the U-Mo/Zr interaction layer. Microscopic characterization shows that the grain size of U-Mo fuel meat increases with the annealing temperature, as expected. The grain sizes were ∼9, ∼13, and ∼20 μm for annealing temperature of 650, 750, and 850 °C, respectively. No abnormal grain growth was observed. The U-Mo/Zr interaction-layer thickness increased with the annealing temperature with an Arrhenius constant for growth of 184 kJ/mole, consistent with a previous diffusion-couple study. The interaction layer thickness was 3.2 ± 0.5 μm, 11.1 ± 2.1 μm, 27.1 ± 0.9 μm for annealing temperature of 650, 750, to 850 °C, respectively. The homogeneity of Mo improves with post rolling annealing temperature and with U-Mo coupon homogenization. The phases in the Zr/U-Mo interaction layer produced by co-rolling, however, differ from those reported in the previous diffusion couple studies.

Effects of heat treatment on U–Mo fuel foils with a zirconium diffusion barrier

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

Jue, Jan-Fong; Trowbridge, Tammy L.; Breckenridge, Cynthia R.

A monolith fuel design based on U–Mo alloy has been selected as the fuel type for conversion of the United States’ high performance research reactors (HPRRs) from highly enriched uranium (HEU) to low-enriched uranium (LEU). In this fuel design, a thin layer of zirconium is used to eliminate the direct interaction between the U–Mo fuel meat and the aluminum-alloy cladding during irradiation. The co-rolling process used to bond the Zr barrier layer to the U–Mo foil during fabrication alters the microstructure of both the U–10Mo fuel meat and the U–Mo/Zr interface. This work studied the effects of post-rolling annealing treatmentmore » on the microstructure of the co-rolled U–Mo fuel meat and the U–Mo/Zr interaction layer. Microscopic characterization shows that the grain size of U–Mo fuel meat increases with the annealing temperature, as expected. The grain sizes were ~9, ~13, and ~20 μm for annealing temperature of 650, 750, and 850 °C, respectively. No abnormal grain growth was observed. The U–Mo/Zr interaction-layer thickness increased with the annealing temperature with an Arrhenius constant for growth of 184 kJ/mole, consistent with a previous diffusion-couple study. The interaction layer thickness was 3.2 ± 0.5 μm, 11.1 ± 2.1 μm, 27.1 ± 0.9 μm for annealing temperature of 650, 750, to 850 °C, respectively. The homogeneity of Mo improves with post rolling annealing temperature and with U–Mo coupon homogenization. The phases in the Zr/U–Mo interaction layer produced by co-rolling, however, differ from those reported in the previous diffusion couple studies.« less

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.

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.

Measurement station for interim inspections of Lightbridge metallic fuel rods at the Halden Boiling Water Reactor

NASA Astrophysics Data System (ADS)

Hartmann, C.; Totemeier, A.; Holcombe, S.; Liverud, J.; Limi, M.; Hansen, J. E.; Navestad, E. AB(; )

2018-01-01

Lightbridge Corporation has developed a new Uranium-Zirconium based metallic fuel. The fuel rods aremanufactured via a co-extrusion process, and are characterized by their multi-lobed (cruciform-shaped) cross section. The fuel rods are also helically-twisted in the axial direction. Two experimental fuel assemblies, each containing four Lightbridge fuel rods, are scheduled to be irradiated in the Halden Boiling Water Reactor (HBWR) starting in 2018. In addition to on-line monitoring of fuel rod elongation and critical assembly conditions (e.g. power, flow rates, coolant temperatures, etc.) during the irradiation, several key parameters of the fuel will be measured out-of-core during interim inspections. An inspection measurement station for use in the irradiated fuel handling compartment at the HBWR has therefore been developed for this purpose. The multi-lobed cladding cross section combined with the spiral shape of the Lightbridge metallic fuel rods requires a high-precision guiding system to ensure good position repeatability combined with low-friction guiding. The measurement station is equipped with a combination of instruments and equipment supplied from third-party vendors and instruments and equipment developed at Institute for Energy Technology (IFE). Two sets of floating linear voltage differential transformer (LVDT) pairs are used to measure swelling and diameter changes between the lobes and the valleys over the length of the fuel rods. Eddy current probes are used to measure the thickness of oxide layers in the valleys and on the lobe tips and also to detect possible surface cracks/pores. The measurement station also accommodates gamma scans. Additionally, an eddy-current probe has been developed at IFE specifically to detect potential gaps or discontinuities in the bonding layer between the metallic fuel and the Zirconium alloy cladding. Potential gaps in the bonding layer will be hidden behind a 0.5-1.0 mm thick cladding wall. It has therefore been necessary to perform a careful design study of the probe geometry. For this, finite element analysis (FEA) has been performed in combination with practical validation tests on representative fuel dummies with machined flaws to find the probe geometry that best detects a hidden flaw. Tests performed thus far show that gaps down to 25 μm thickness can be detected with good repeatability and good discrimination from lift-off signals.

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.

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...

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)

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.

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.

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

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.

Improved electrical properties of atomic layer deposited tin disulfide at low temperatures using ZrO2 layer

NASA Astrophysics Data System (ADS)

Lee, Juhyun; Lee, Jeongsu; Ham, Giyul; Shin, Seokyoon; Park, Joohyun; Choi, Hyeongsu; Lee, Seungjin; Kim, Juyoung; Sul, Onejae; Lee, Seungbeck; Jeon, Hyeongtag

2017-02-01

We report the effect of zirconium oxide (ZrO2) layers on the electrical characteristics of multilayered tin disulfide (SnS2) formed by atomic layer deposition (ALD) at low temperatures. SnS2 is a two-dimensional (2D) layered material which exhibits a promising electrical characteristics as a channel material for field-effect transistors (FETs) because of its high mobility, good on/off ratio and low temperature processability. In order to apply these 2D materials to large-scale and flexible electronics, it is essential to develop processes that are compatible with current electronic device manufacturing technology which should be conducted at low temperatures. Here, we deposited a crystalline SnS2 at 150 °C using ALD, and we then annealed at 300 °C. X-ray diffraction (XRD) and Raman spectroscopy measurements before and after the annealing showed that SnS2 had a hexagonal (001) peak at 14.9° and A1g mode at 313 cm-1. The annealed SnS2 exhibited clearly a layered structure confirmed by the high resolution transmission electron microscope (HRTEM) images. Back-gate FETs with SnS2 channel sandwiched by top and bottom ZrO2 on p++Si/SiO2 substrate were suggested to improve electrical characteristics. We used a bottom ZrO2 layer to increase adhesion between the channel and the substrate and a top ZrO2 layer to improve contact property, passivate surface, and protect from process-induced damages to the channel. ZTZ (ZrO2/SnS2/ZrO2) FETs showed improved electrical characteristics with an on/off ratio of from 0.39×103 to 6.39×103 and a mobility of from 0.0076 cm2/Vs to 0.06 cm2/Vs.

The Preparation and Microstructure of Nanocrystal 3C-SiC/ZrO2 Bilayer Films

PubMed Central

Ye, Chao; Ran, Guang; Zhou, Wei; Qu, Yazhou; Yan, Xin; Cheng, Qijin; Li, Ning

2017-01-01

The nanocrystal 3C-SiC/ZrO2 bilayer films that could be used as the protective coatings of zirconium alloy fuel cladding were prepared on a single-crystal Si substrate. The corresponding nanocrystal 3C-SiC film and nanocrystal ZrO2 film were also dividedly synthesized. The microstructure of nanocrystal films was analyzed by grazing incidence X-ray diffraction (GIXRD) and cross-sectional transmission electron microscopy (TEM). The 3C-SiC film with less than 30 nm crystal size was synthesized by Plasma Enhanced Chemical Vapor Deposition (PECVD) and annealing. The corresponding formation mechanism of some impurities in SiC film was analyzed and discussed. An amorphous Zr layer about 600 nm in width was first deposited by magnetron sputtering and then oxidized to form a nanocrystal ZrO2 layer during the annealing process. The interface characteristics of 3C-SiC/ZrO2 bilayer films prepared by two different processes were obviously different. SiZr and SiO2 compounds were formed at the interface of 3C-SiC/ZrO2 bilayer films. A corrosion test of 3C-SiC/ZrO2 bilayer films was conducted to qualitatively analyze the surface corrosion resistance and the binding force of the interface. PMID:29168782

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.

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.

Steep-slope hysteresis-free negative capacitance MoS2 transistors

NASA Astrophysics Data System (ADS)

Si, Mengwei; Su, Chun-Jung; Jiang, Chunsheng; Conrad, Nathan J.; Zhou, Hong; Maize, Kerry D.; Qiu, Gang; Wu, Chien-Ting; Shakouri, Ali; Alam, Muhammad A.; Ye, Peide D.

2018-01-01

The so-called Boltzmann tyranny defines the fundamental thermionic limit of the subthreshold slope of a metal-oxide-semiconductor field-effect transistor (MOSFET) at 60 mV dec-1 at room temperature and therefore precludes lowering of the supply voltage and overall power consumption1,2. Adding a ferroelectric negative capacitor to the gate stack of a MOSFET may offer a promising solution to bypassing this fundamental barrier3. Meanwhile, two-dimensional semiconductors such as atomically thin transition-metal dichalcogenides, due to their low dielectric constant and ease of integration into a junctionless transistor topology, offer enhanced electrostatic control of the channel4-12. Here, we combine these two advantages and demonstrate a molybdenum disulfide (MoS2) two-dimensional steep-slope transistor with a ferroelectric hafnium zirconium oxide layer in the gate dielectric stack. This device exhibits excellent performance in both on and off states, with a maximum drain current of 510 μA μm-1 and a sub-thermionic subthreshold slope, and is essentially hysteresis-free. Negative differential resistance was observed at room temperature in the MoS2 negative-capacitance FETs as the result of negative capacitance due to the negative drain-induced barrier lowering. A high on-current-induced self-heating effect was also observed and studied.

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.

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.

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.

Physicochemical analysis of urinary stones from Dharmapuri district

NASA Astrophysics Data System (ADS)

Aslin Shamema, A.; Thanigai Arul, K.; Senthil Kumar, R.; Narayana Kalkura, S.

2015-01-01

Nephrolithiasis is a common disease caused by the multifactorial components such as geographical location, bacterial infection, low urine volume, and low intake of water. This disease induces severe metabolic abnormalities in the human body. As the prevalence of this disease was high in Dharmapuri district located in Tamil Nadu, urinary stones removed from the patients pertaining to this district were collected and to identify the toxic elements present in the stones. The presence of functional groups and phases of the stones were analyzed using X-ray diffraction (XRD), Fourier transform Raman spectroscopy and Fourier transform infrared spectroscopy (FT-IR). The majority of stones were found to be calcium oxalate monohydrate (COM) and mixed stones having minor existence of struvite and uric acid. Hexagonal shaped COM crystals, needle shaped uric acid crystals and layered arrangement of struvite crystals in the core region were revealed by Scanning Electron Microscopy (SEM). Thermo Gravimetric Analysis (TGA) was used to determine the thermal stability and the hardness of the stone which was measured using Vickers hardness (HV). The presence of toxic elements in stones such as zirconium and mercury was identified using Energy Dispersive X-ray Spectroscopy (EDS). The EDS analysis showed higher concentration of zirconium in the core region compared to the periphery. The percentage of zirconium was relatively high compared to other toxic elements in the stones. The Vickers hardness results indicated that high HV values in the core region than the periphery and this might be due to the presence of zirconium.

METHOD OF FORMING A FUEL ELEMENT FOR A NUCLEAR REACTOR

DOEpatents

Layer, E.H. Jr.; Peet, C.S.

1962-01-23

A method is given for preparing a fuel element for a nuclear reactor. The method includes the steps of sandblasting a body of uranium dioxide to roughen the surface thereof, depositing a thin layer of carbon thereon by thermal decomposition of methane, and cladding the uranium dioxide body with zirconium by gas pressure bonding. (AEC)

FUEL ELEMENT AND METHOD OF PREPARATION

DOEpatents

Kingston, W.E.

1961-04-25

A nuclear fuel element in the form of a wire is reported. A bar of uranium is enclosed in a thin layer of aluminum and the composite is sheathed in beryllium, zirconium, or stainnless steel. The sheathed article is then drawn to wire form, heated to alloy the aluminum with both uranium and sheath, and finally cold worked.

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.

Novel approach to Zr powder production by smooth ZrCl4 bubbling through molten salt

NASA Astrophysics Data System (ADS)

Bae, Hyun-Na; Choi, Mi-Seon; Lee, Go-Gi; Kim, Seon-Hyo

2016-01-01

A reduction process using ZrCl4 bubbles as a reactant was investigated to produce zirconium metals. ZrCl4 vapor was bubbled through the lance in the bath, in which Mg melt and MgCl2 salt were separated. Zr powder was formed by a reduction of ZrCl4 bubbles in magnesium layer. However, the lance was clogged by the aggregate of zirconium occurred during ZrCl4 vapor injecting leading to interruption of ZrCl4 supply into the bath. This phenomenon could be caused by the presence of magnesium at the lance tip, which passes through MgCl2 salt during bubbling, and then zirconium was formed in the forms of intermetallic compounds with aluminum. In this study, the effect of molten salt on the troubled phenomena was investigated and it was verified that CaCl2 with relatively low Weber number meaning relatively high surface tension as molten salt is effective in inhibiting the lance clogging phenomena. Then, a few micrometer-sized Zr powder with the high purity of 91.6 wt% was obtained smoothly without the formation of intermetallic compound.

Adsorption Behavior of Rare Earth Metal Cations in the Interlayer Space of γ-ZrP.

PubMed

Takei, Takahiro; Iidzuka, Kiyoaki; Miura, Akira; Yanagida, Sayaka; Kumada, Nobuhiro; Magome, Eisuke; Moriyoshi, Chikako; Kuroiwa, Yoshihiro

2016-10-04

Adsorption competencies of rare earth metal cations in γ-zirconium phosphate were examined by ICP, synchrotron X-ray diffraction (SXRD), and ab initio simulation. The adsorption amounts are around 0.06-0.10 per zirconium phosphate. From the SXRD patterns of the adsorbed samples, the basal spacing estimated by c sin β increased linearly with an increasing ionic radius of rare earth metal cation, though a and b lattice constants show no change. These SXRD patterns can be classified into four groups that have different super lattices. The four superlattices have multiplicities of x131, x241, and x221 for the xabc axis, and the location of the rare earth metal cation in the original unit cell changes depending on the superlattice cell. In the x131 superlattice, Yb and Er occupied the site near the zirconium phosphate layer, though La and Ce in the x221 superlattice remained in the center position between the phosphate sheet. For the ab initio simulation of γ-ZrP with the typical rare earth metal cations (Tb, Eu, Dy, and La), the results of simulation show a similar tendency of the position estimated by SXRD refinements.

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.

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.

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

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

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.

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.

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

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.

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)

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

Experimental study of high-temperature properties of zirconium carbide as a protective material for nuclear power and aerospace technologies (from 2000 to 5000 K)

NASA Astrophysics Data System (ADS)

Savvatimskiy, A. I.; Onufriev, S. V.; Muboyadzhyan, S. A.; Seredkin, N. N.

2017-11-01

The temperature dependences of the thermal and electro physical properties of the zirconium carbide ZrC + C and ZrCa0.95 were studied in the temperature range 2000-5000 K. The Zr+C specimens were in the form of thin layers sputtered on quarts substrate and ZrC0.95 specimens were in the form of plates cut off from the sintered block. The properties are measured: temperature and heat of fusion, enthalpy, specific heat and resistivity, referred to the initial dimensions. A steep increase in the specific heat of these substances before melting and a sharp decrease after melting were observed at a heating rate of ∼ 108 K/s, which is possibly due to the formation of Frenkel pair defects in the specimens.

Multilayer bioactive glass/zirconium titanate thin films in bone tissue engineering and regenerative dentistry

PubMed Central

Mozafari, Masoud; Salahinejad, Erfan; Shabafrooz, Vahid; Yazdimamaghani, Mostafa; Vashaee, Daryoosh; Tayebi, Lobat

2013-01-01

Surface modification, particularly coatings deposition, is beneficial to tissue-engineering applications. In this work, bioactive glass/zirconium titanate composite thin films were prepared by a sol-gel spin-coating method. The surface features of the coatings were studied by scanning electron microscopy, atomic force microscopy, and spectroscopic reflection analyses. The results show that uniform and sound multilayer thin films were successfully prepared through the optimization of the process variables and the application of carboxymethyl cellulose as a dispersing agent. Also, it was found that the thickness and roughness of the multilayer coatings increase nonlinearly with increasing the number of the layers. This new class of nanocomposite coatings, comprising the bioactive and inert components, is expected not only to enhance bioactivity and biocompatibility, but also to protect the surface of metallic implants against wear and corrosion. PMID:23641155

Influence of growth temperature on properties of zirconium dioxide films grown by atomic layer deposition

NASA Astrophysics Data System (ADS)

Kukli, Kaupo; Ritala, Mikko; Aarik, Jaan; Uustare, Teet; Leskela, Markku

2002-08-01

ZrO2 films were grown by atomic layer deposition from ZrCl4 and H2O or a mixture of H2O and H2O2 on Si(100) substrates in the temperature range of 180-600 degC. The films were evaluated in the as-deposited state, in order to follow the effect of deposition temperature on the film quality. The rate of crystal growth increased and the content of residual impurities decreased with increasing temperature. The zirconium-to-oxygen atomic ratio, determined by ion-beam analysis, corresponded to the stoichiometric dioxide regardless of the growth temperature. The effective permittivity of ZrO2 in Al/ZrO2/Si capacitor structures increased from 13-15 in the films grown at 180 degC to 19 in the films grown at 300-600 degC, measured at 100 kHz. The permittivity was relatively high in the crystallized films, compared to the amorphous ones, but rather insensitive to the crystal structure. The permittivity was higher in the films grown using water. The leakage current density tended to be lower and the breakdown field higher in the films grown using hydrogen peroxide.

Ca2+-exchange in layered zirconium orthophosphate, α-ZrP: Chemical study and potential application for zinc corrosion inhibition

NASA Astrophysics Data System (ADS)

Bouali, Imane; Rocca, Emmanuel; Veys-Renaux, Delphine; Rhouta, Benaissa; Khalil, Aziza; Aït Aghzzaf, Ahmed

2017-11-01

The control of the corrosion phenomenon occurring at the metal interface requires the development of new non-toxic anticorrosion additives. For this purpose, zirconium orthophosphate compounds (Zr(HPO4)2,H2O noted α-ZrP) were synthesized by both hydrothermal and refluxing methods The Ca2+-cationic exchange in the layered structure is kinetically favoured by low crystallinity of α-ZrP synthesized by refluxing process, and leads to the formation of CaZr(PO4)2,4H2O, noted Ca2+-ZrP. The H+/Ca2+ exchange mechanism is mainly triggered by acid-base considerations, and especially the pKa of α-ZrP/Ca2+-ZrP acid-base couple (evaluated to 2.5). Both compounds are acidic compounds by internal exchangeable H+ for α-ZrP and surface protons for Ca2+-ZrP, and can be used as potential inhibitors of zinc corrosion. Electrochemical measurements show that Ca2+-ZrP compounds dispersed in the NaCl electrolyte buffer the pH value over a long time and therefore allow controlling the corrosion rate of zinc.

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.

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.

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

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

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.

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

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.

High-intensity low energy titanium ion implantation into zirconium alloy

NASA Astrophysics Data System (ADS)

Ryabchikov, A. I.; Kashkarov, E. B.; Pushilina, N. S.; Syrtanov, M. S.; Shevelev, A. E.; Korneva, O. S.; Sutygina, A. N.; Lider, A. M.

2018-05-01

This research describes the possibility of ultra-high dose deep titanium ion implantation for surface modification of zirconium alloy Zr-1Nb. The developed method based on repetitively pulsed high intensity low energy titanium ion implantation was used to modify the surface layer. The DC vacuum arc source was used to produce metal plasma. Plasma immersion titanium ions extraction and their ballistic focusing in equipotential space of biased electrode were used to produce high intensity titanium ion beam with the amplitude of 0.5 A at the ion current density 120 and 170 mA/cm2. The solar eclipse effect was used to prevent vacuum arc titanium macroparticles from appearing in the implantation area of Zr sample. Titanium low energy (mean ion energy E = 3 keV) ions were implanted into zirconium alloy with the dose in the range of (5.4-9.56) × 1020 ion/cm2. The effect of ion current density, implantation dose on the phase composition, microstructure and distribution of elements was studied by X-ray diffraction, scanning electron microscopy and glow-discharge optical emission spectroscopy, respectively. The results show the appearance of Zr-Ti intermetallic phases of different stoichiometry after Ti implantation. The intermetallic phases are transformed from both Zr0.7Ti0.3 and Zr0.5Ti0.5 to single Zr0.6Ti0.4 phase with the increase in the implantation dose. The changes in phase composition are attributed to Ti dissolution in zirconium lattice accompanied by the lattice distortions and appearance of macrostrains in intermetallic phases. The depth of Ti penetration into the bulk of Zr increases from 6 to 13 μm with the implantation dose. The hardness and wear resistance of the Ti-implanted zirconium alloy were increased by 1.5 and 1.4 times, respectively. The higher current density (170 mA/cm2) leads to the increase in the grain size and surface roughness negatively affecting the tribological properties of the alloy.

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.

Zr-Containing 4,4'-ODA/PMDA Polyimide Composites. Parts 1 & 2

NASA Technical Reports Server (NTRS)

Illingsworth, M. L.; Betancourt, J. A.; Chen, Y.; Terschak, J. A.; Banks, B. A.; Rutledge, S. K.; Cales, M.; He, L.

2001-01-01

The objective of this research is to improve the atomic oxygen resistance of Kapton(TM), a polyimide (PI) made from pyromellitic acid dianhydride (PMDA) and 4,4'-oxydianiline (ODA), while retaining or enhancing the desirable properties of the pure polymer. Toward this end, zirconium-containing complexes and polymers were used to make composites and blends. Tetra(acetylacetonato)zirconium(IV), Zr(acac)4, which is commercially available, was identified as the best zirconium-containing complex for enhancing the atomic oxygen resistance of polyimide composites of the 10 complexes screened. Films prepared from the commercially available polyamic acid (PAA) of PMDA-ODA (DuPont) have good uniformity, flexibility, and tensile strength. A 24-layer 10% (mol) Zr(acac)4/PI composite film showed significant improvement (ca. 20 fold) of atomic oxygen resistance over the pure polyimide. However, 10% (mol) Zr(acac)4 represents an upper concentration limit, above which films undergo cracking upon thermal imidization. In order to increase the Zr complex concentration in PMDA-ODA PI films, while retaining good film properties, [Zr(adsp)2-PMDA]n coordination polymer [bis(4-amino-N,N'-disalicylidene- 1,2-phenylenediamino)zirconium(IV)-pyromellitic dianhydride] and [Zr(adsp)2-PMDA-ODA-PMDA]n terpolymer were synthesized and blended with commercial PAA, respectively. Several techniques were used to characterize the films made from the polymer containing Zr(acac)4. Plasma studies of films having 2% (mol) incremental concentrations of Zr in the Kapton up to 10% (mol) show that the overall rate of erosion is reduced about 75 percent.

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...

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.

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.

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.

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.

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

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.

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.

Hydrogenation behavior of Ti-implanted Zr-1Nb alloy with TiN films deposited using filtered vacuum arc and magnetron sputtering

NASA Astrophysics Data System (ADS)

Kashkarov, E. B.; Nikitenkov, N. N.; Sutygina, A. N.; Bezmaternykh, A. O.; Kudiiarov, V. N.; Syrtanov, M. S.; Pryamushko, T. S.

2018-02-01

More than 60 years of operation of water-cooled reactors have shown that local or general critical hydrogen concentration is one of the basic limiting criteria of zirconium-based fuel element claddings. During the coolant radiolysis, released hydrogen penetrates and accumulates in zirconium alloys. Hydrogenation of zirconium alloys leads to degradation of their mechanical properties, hydride cracking and stress corrosion cracking. In this research the effect of titanium nitride (TiN) deposition on hydrogenation behavior of Ti-implanted Zr-1Nb alloy was described. Ti-implanted interlayer was fabricated by plasma immersion ion implantation (PIII) at the pulsed bias voltage of 1500 V to improve the adhesion of TiN and reduce hydrogen penetration into Zr-1Nb alloy. We conducted the comparative analysis on hydrogenation behavior of the Ti-implanted alloy with sputtered and evaporated TiN films by reactive dc magnetron sputtering (dcMS) and filtered cathodic vacuum arc deposition (FVAD), respectively. The crystalline structure and surface morphology were investigated using X-ray diffraction (XRD) and scanning electron microscopy (SEM). The elemental distribution was analyzed using glow-discharge optical emission spectroscopy (GD-OES). Hydrogenation was performed from gas atmosphere at 350 °C and 2 atm hydrogen pressure. The results revealed that TiN films as well as Ti implantation significantly reduce hydrogen absorption rate of Zr-1Nb alloy. The best performance to reduce the rate of hydrogen absorption is Ti-implanted layer with evaporated TiN film. Morphology of the films impacted hydrogen permeation through TiN films: the denser film the lower hydrogen permeation. The Ti-implanted interface plays an important role of hydrogen accumulation layer for trapping the penetrated hydrogen. No deterioration of adhesive properties of TiN films on Zr-1Nb alloy with Ti-implanted interface occurs under high-temperature hydrogen exposure. Thus, the fabrication of Ti-implanted layer with dense TiN films can be an effective way to protect Zr-1Nb alloy from hydrogen embrittlement.

Microstructures and properties of ceramic particle-reinforced metal matrix composite layers produced by laser cladding

NASA Astrophysics Data System (ADS)

Zhang, Qingmao; He, Jingjiang; Liu, Wenjin; Zhong, Minlin

2005-01-01

Different weight ratio of titanium, zirconium, WC and Fe-based alloy powders were mixed, and cladded onto a medium carbon steel substrate using a 3kW continuous wave CO2 laser, aiming at producing Ceramic particles- reinforced metal matrix composites (MMCs) layers. The microstructures of the layers are typical hypoeutectic, and the major phases are Ni3Si2, TiSi2, Fe3C, FeNi, MC, Fe7Mo3, Fe3B, γ(residual austenite) and M(martensite). The microstructure morphologies of MMCs layers are dendrites/cells. The MC-type reinforcements are in situ synthesis Carbides which main compositions consist of transition elements Zr, Ti, W. The MC-type particles distributed within dendrite and interdendritic regions with different volume fractions for single and overlapping clad layers. The MMCs layers are dense and free of cracks with a good metallurgical bonding between the layer and substrate. The addition ratio of WC in the mixtures has the remarkable effect on the microhardness of clad layers.

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.

The sol-gel route: A versatile process for up-scaling the fabrication of gas-tight thin electrolyte layers

NASA Astrophysics Data System (ADS)

Viazzi, Céline; Rouessac, Vincent; Lenormand, Pascal; Julbe, Anne; Ansart, Florence; Guizard, Christian

2011-03-01

Sol-gel routes are often investigated and adapted to prepare, by suitable chemical modifications, submicronic powders and derived materials with controlled morphology, which cannot be obtained by conventional solid state chemistry paths. Wet chemistry methods provide attractive alternative routes because mixing of species occurs at the atomic scale. In this paper, ultrafine powders were prepared by a novel synthesis method based on the sol-gel process and were dispersed into suspensions before processing. This paper presents new developments for the preparation of functional materials like yttria-stabilized-zirconia (YSZ, 8% Y2O3) used as electrolyte for solid oxide fuel cells. YSZ thick films were coated onto porous Ni-YSZ substrates using a suspension with an optimized formulation deposited by either a dip-coating or a spin-coating process. The suspension composition is based on YSZ particles encapsulated by a zirconium alkoxide which was added with an alkoxide derived colloidal sol. The in situ growth of these colloids increases significantly the layer density after an appropriated heat treatment. The derived films were continuous, homogeneous and around 20 μm thick. The possible up-scaling of this process has been also considered and the suitable processing parameters were defined in order to obtain, at an industrial scale, homogeneous, crack-free, thick and adherent films after heat treatment at 1400 °C.

Surface derivatization strategy for combinatorial analysis of cell response to mixtures of protein domains.

PubMed

Chiang, Chunyi; Karuri, Stella W; Kshatriya, Pradnya P; Schwartz, Jeffrey; Schwarzbauer, Jean E; Karuri, Nancy W

2012-01-10

We report a robust strategy for conjugating mixtures of two or more protein domains to nonfouling polyurethane surfaces. In our strategy, the carbamate groups of polyurethane are reacted with zirconium alkoxide from the vapor phase to give a surface-bound oxide that serves as a chemical layer that can be used to bond organics to the polymer substrate. A hydroxyalkylphosphonate monolayer was synthesized on this layer, which was then used to covalently bind primary amine groups in protein domains using chloroformate-derived cross-linking. The effectiveness of this synthesis strategy was gauged by using an ELISA to measure competitive, covalent bonding of cell-binding (III(9-10)) and fibronectin-binding (III(1-2)) domains of the cell adhesion protein fibronectin. Cell adhesion, spreading, and fibronectin matrix assembly were examined on surfaces conjugated with single domains, a 1:1 surface mixture of III(1-2) and III(9-10), and a recombinant protein "duplex" containing both domains in one fusion protein. The mixture performed as well as or better than the other surfaces in these assays. Our surface activation strategy is amenable to a wide range of polymer substrates and free amino group-containing protein fragments. As such, this technique may be used to create biologically specific materials through the immobilization of specific protein groups or mixtures thereof on a substrate surface.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

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.

Electrochemical Behavior Assessment of As-Cast Mg-Y-RE-Zr Alloy in Phosphate Buffer Solutions (X Na3PO4 + Y Na2HPO4) Using Electrochemical Impedance Spectroscopy and Mott-Schottky Techniques

NASA Astrophysics Data System (ADS)

Fattah-alhosseini, Arash; Asgari, Hamed

2018-05-01

In the present study, electrochemical behavior of as-cast Mg-Y-RE-Zr alloy (RE: rare-earth alloying elements) was investigated using electrochemical tests in phosphate buffer solutions (X Na3PO4 + Y Na2HPO4). X-ray diffraction techniques and Scanning electron microscopy equipped with energy dispersive x-ray spectroscopy were used to investigate the microstructure and phases of the experimental alloy. Different electrochemical tests such as potentiodynamic polarization (PDP), electrochemical impedance spectroscopy (EIS) and Mott-Schottky (M-S) analysis were carried out in order to study the electrochemical behavior of the experimental alloy in phosphate buffer solutions. The PDP curves and EIS measurements indicated that the passive behavior of the as-cast Mg-Y-RE-Zr alloy in phosphate buffer solutions was weakened by an increase in the pH, which is related to formation of an imperfect and less protective passive layer on the alloy surface. The presence of the insoluble zirconium particles along with high number of intermetallic phases of RE elements mainly Mg24Y5 in the magnesium matrix can deteriorate the corrosion performance of the alloy by disrupting the protective passive layer that is formed at pH values over 11. These insoluble zirconium particles embedded in the matrix can detrimentally influence the passivation. The M-S analysis revealed that the formed passive layers on Mg-Y-RE-Zr alloy behaved as an n-type semiconductor. An increase in donor concentration accompanying solutions of higher alkalinity is thought to result in the formation of a less resistive passive layer.

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.

High rate buffer layer for IBAD MgO coated conductors

DOEpatents

Foltyn, Stephen R [Los Alamos, NM; Jia, Quanxi [Los Alamos, NM; Arendt, Paul N [Los Alamos, NM

2007-08-21

Articles are provided including a base substrate having a layer of an oriented material thereon, and, a layer of hafnium oxide upon the layer of an oriented material. The layer of hafnium oxide can further include a secondary oxide such as cerium oxide, yttrium oxide, lanthanum oxide, scandium oxide, calcium oxide and magnesium oxide. Such articles can further include thin films of high temperature superconductive oxides such as YBCO upon the layer of hafnium oxide or layer of hafnium oxide and secondary oxide.

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.

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.

Actinide oxide photodiode and nuclear battery

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

Sykora, Milan; Usov, Igor

Photodiodes and nuclear batteries may utilize actinide oxides, such a uranium oxide. An actinide oxide photodiode may include a first actinide oxide layer and a second actinide oxide layer deposited on the first actinide oxide layer. The first actinide oxide layer may be n-doped or p-doped. The second actinide oxide layer may be p-doped when the first actinide oxide layer is n-doped, and the second actinide oxide layer may be n-doped when the first actinide oxide layer is p-doped. The first actinide oxide layer and the second actinide oxide layer may form a p/n junction therebetween. Photodiodes including actinide oxidesmore » are better light absorbers, can be used in thinner films, and are more thermally stable than silicon, germanium, and gallium arsenide.« less

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.

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

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.

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

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.

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.

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.

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

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.

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.

Electrical characterization of doped strontium titanate thin films for semiconductor memories

NASA Astrophysics Data System (ADS)

Han, Jeong Hee

2002-08-01

Doped strontium titanate (ST) thin films were investigated for high-density memory applications. ST has become a promising candidate to replace conventional silicon oxide due to its high inherent dielectric constant, superior leakage characteristics, and good chemical stability. However, oxygen vacancies and the problems that arise as a result are one of the main drawbacks against this material. Resistance degradation is a serious reliability issue in perovskite titanate films and may be a result of oxygen vacancies. In this dissertation, an attempt to reduce the resistance degradation was made by doping the ST films with both niobium and lanthanum. Niobium is a B-site donor in the perovskite, whereas lanthanum is an A-site donor. Both have an extra valence charge than the atom which it replaces in the crystal structure. With a higher valence charge, the number of oxygen vacancies is hoped to be reduced and result in better electrical performance. Experimental results showed that the degradation rate is reduced by doping with either niobium or lanthanum. A bi-layer study was also performed to optimize the dielectric with the strengths of both doped and undoped strontium titanate and to distinguish the source of the oxygen vacancies. A study on the conduction mechanisms and dielectric dispersion was also performed. An additional study was made on the effect of iridium as a possible gate electrode for a MOS capacitor. Hafnium oxide was used as the high-permittivity oxide. The results observed showed that the capacitance was higher for iridium electrodes than those for platinum electrodes. However, both electrodes showed unacceptable frequency dispersion which may be caused by crude patterning techniques. A hysteresis review was also done for hafnium and zirconium oxides. It was observed that the hysteresis measured in the high-permittivity oxides are dependent on the accumulation sweep voltage due to the trapping and de-trapping of charge at the dielectric-silicon interface.

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.

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.

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:

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)

Method for bonding thin film thermocouples to ceramics

DOEpatents

Kreider, Kenneth G.

1993-01-01

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

Method for fabrication of ceramic dielectric films on copper foils

DOEpatents

Ma, Beihai; Narayanan, Manoj; Dorris, Stephen E.; Balachandran, Uthamalingam

2017-06-14

The present invention provides copper substrate coated with a lead-lanthanum-zirconium-titanium (PLZT) ceramic film, which is prepared by a method comprising applying a layer of a sol-gel composition onto a copper foil. The sol-gel composition comprises a precursor of a ceramic material suspended in 2-methoxyethanol. The layer of sol-gel is then dried at a temperature up to about 250.degree. C. The dried layer is then pyrolyzed at a temperature in the range of about 300 to about 450.degree. C. to form a ceramic film from the ceramic precursor. The ceramic film is then crystallized at a temperature in the range of about 600 to about 750.degree. C. The drying, pyrolyzing and crystallizing are performed under a flowing stream of an inert gas.

Some observations on uranium carbide alloy/tungsten compatibility

NASA Technical Reports Server (NTRS)

Phillips, W. M.

1972-01-01

Chemical compatibility between both pure and thoriated tungsten and uranium carbide alloys was studied at 1800 C for up to 3300 hours. Alloying with zirconium carbide appeared to widen the homogeneity range of uranium carbide, making additional carbon available for reaction with the tungsten. Reaction layers were formed both by vapor phase reaction and by physical contact, producing either or both UWC2 and W2C, dependent upon the phases present in the starting fuel alloy. Formation of UWC2 results in slow growth of the reaction layer with time, while W2C reaction layers grow rapidly, allowing equilibrium to be reached in less than 2500 hours at 1800 C. The presence of a thermal gradient had no effect on the reactions observed nor did the presence of thoria in the tungsten clad.

Some observations on uranium carbide alloy/tungsten compatibility.

NASA Technical Reports Server (NTRS)

Phillips, W. M.

1972-01-01

Results of chemical compatibility tests between both pure tungsten and thoriated tungsten run at 1800 C for up to 3300 hours with uranium carbide alloys. Alloying with zirconium carbide appeared to widen the homogeneity range of uranium carbide, making additional carbon available for reaction with the tungsten. Reaction layers were formed both by vapor phase reaction and by physical contact, producing either or both UWC2 and W2C, depending upon the phases present in the starting fuel alloy. Formation of UWC2 results in slow growth of the reaction layer with time, while W2C reaction layers grow rapidly, allowing equilibrium to be reached in less than 2500 hours at 1800 C. Neither the presence of a thermal gradient nor the presence of thoria in the tungsten clad affect the reactions observed.

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.

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.

Oriented conductive oxide electrodes on SiO2/Si and glass

DOEpatents

Jia, Quanxi; Arendt, Paul N.

2001-01-01

A thin film structure is provided including a silicon substrate with a layer of silicon dioxide on a surface thereof, and a layer of cubic oxide material deposited upon the layer of silicon dioxide by ion-beam-assisted-deposition, said layer of cubic oxide material characterized as biaxially oriented. Preferably, the cubic oxide material is yttria-stabilized zirconia. Additional thin layers of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide are deposited upon the layer of yttria-stabilized zirconia. An intermediate layer of cerium oxide is employed between the yttria-stabilized zirconia layer and the lanthanum strontium cobalt oxide layer. Also, a layer of barium strontium titanium oxide can be upon the layer of biaxially oriented ruthenium oxide or lanthanum strontium cobalt oxide. Also, a method of forming such thin film structures, including a low temperature deposition of a layer of a biaxially oriented cubic oxide material upon the silicon dioxide surface of a silicon dioxide/silicon substrate is provided.

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

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.

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

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.

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.

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...

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.

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.

Synthesis and Exfoliation of Discotic Zirconium Phosphates to Obtain Colloidal Liquid Crystals

PubMed Central

Yu, Yi-Hsien; Wang, Xuezhen; Shinde, Abhijeet; Cheng, Zhengdong

2016-01-01

Due to their abundance in natural clay and potential applications in advanced materials, discotic nanoparticles are of interest to scientists and engineers. Growth of such anisotropic nanocrystals through a simple chemical method is a challenging task. In this study, we fabricate discotic nanodisks of zirconium phosphate [Zr(HPO4)2·H2O] as a model material using hydrothermal, reflux and microwave-assisted methods. Growth of crystals is controlled by duration time, temperature, and concentration of reacting species. The novelty of the adopted methods is that discotic crystals of size ranging from hundred nanometers to few micrometers can be obtained while keeping the polydispersity well within control. The layered discotic crystals are converted to monolayers by exfoliation with tetra-(n)-butyl ammonium hydroxide [(C4H9)4NOH, TBAOH]. Exfoliated disks show isotropic and nematic liquid crystal phases. Size and polydispersity of disk suspensions is highly important in deciding their phase behavior. PMID:27284765

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...

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...

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.

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.

Hydrogen permeation in FeCrAl alloys for LWR cladding application

NASA Astrophysics Data System (ADS)

Hu, Xunxiang; Terrani, Kurt A.; Wirth, Brian D.; Snead, Lance L.

2015-06-01

FeCrAl, an advanced oxidation-resistant iron-based alloy class, is a highly prevalent candidate as an accident-tolerant fuel cladding material. Compared with traditional zirconium alloy fuel cladding, increased tritium permeation through FeCrAl fuel cladding to the primary coolant is expected, raising potential safety concerns. In this study, the hydrogen permeability of several FeCrAl alloys was obtained using a static permeation test station, which was calibrated and validated using 304 stainless steel. The high hydrogen permeability of FeCrAl alloys leads to concerns with respect to potentially significant tritium release when used for fuel cladding in LWRs. The total tritium inventory inside the primary coolant of a light water reactor was quantified by applying a 1-dimensional steady state tritium diffusion model to demonstrate the dependence of tritium inventory on fuel cladding type. Furthermore, potential mitigation strategies for tritium release from FeCrAl fuel cladding were discussed and indicate the potential for application of an alumina layer on the inner clad surface to serve as a tritium barrier. More effort is required to develop a robust, economical mitigation strategy for tritium permeation in reactors using FeCrAl clad fuel assemblies.

Joining of materials using laser heating

DOEpatents

Cockeram, Brian V.; Hicks, Trevor G.; Schmid, Glenn C.

2003-07-01

A method for diffusion bonding ceramic layers such as boron carbide, zirconium carbide, or silicon carbide uses a defocused laser beam to heat and to join ceramics with the use of a thin metal foil insert. The metal foil preferably is rhenium, molybdenum or titanium. The rapid, intense heating of the ceramic/metal/ceramic sandwiches using the defocused laser beam results in diffusive conversion of the refractory metal foil into the ceramic and in turn creates a strong bond therein.

Joining of Zirconium Diboride-Based Ceramic Composites to Metallic Systems for High-Temperature Applications

NASA Technical Reports Server (NTRS)

Asthana, R.; Singh, M.

2008-01-01

Three types of hot-pressed zirconium diboride (ZrB2)-based ultra-high-temperature ceramic composites (UHTCC), ZrB2-SiC (ZS), ZrB2-SiC-C (ZSC), and ZrB2-SCS9-SiC (ZSS), were joined to Cu-clad-Mo using two Ag-Cu brazes (Cusil-ABA and Ticusil, T(sub L) approx.1073-1173 K) and two Pd-base brazes (Palco and Palni, T(sub L) approx.1493-1513 K). Scanning Electron Microscopy (SEM) coupled with energy-dispersive spectroscopy (EDS) revealed greater chemical interaction in joints made using Pd-base brazes than in joints made using Ag-Cu based active brazes. The degree of densification achieved in hot pressed composites influenced the Knoop hardness of the UHTCC and the hardness distribution across the braze interlayer. The braze region in Pd-base system displayed higher hardness in joints made using fully-dense ZS composites than in joints made using partially-dense ZSS composites and the carbon-containing ZSC composites. Calculations indicate a small negative elastic strain energy and an increase in the UHTCC's fracture stress up to a critical clad layer thickness . Above this critical thickness, strain energy in the UHTCC is positive, and it increases with increasing clad layer thickness. Empirical projections show a reduction in the effective thermal resistance of the joints and highlight the potential benefits of joining the UHTCC to Cu-clad-Mo.

Substrate Structures For Growth Of Highly Oriented And/Or Epitaxial Layers Thereon

DOEpatents

Arendt, Paul N.; Foltyn, Stephen R.; Groves, James R.; Jia, Quanxi

2005-07-26

A composite substrate structure including a substrate, a layer of a crystalline metal oxide or crystalline metal oxynitride material upon the substrate, a layer of an oriented cubic oxide material having a rock-salt-like structure upon the crystalline metal oxide or crystalline metal oxynitride material layer is provided together with additional layers such as one or more layers of a buffer material upon the oriented cubic oxide material layer. Jc's of 2.3×106 A/cm2 have been demonstrated with projected Ic's of 320 Amperes across a sample 1 cm wide for a superconducting article including a flexible polycrystalline metallic substrate, an inert oxide material layer upon the surface of the flexible polycrystalline metallic substrate, a layer of a crystalline metal oxide or crystalline metal oxynitride material upon the layer of the inert oxide material, a layer of an oriented cubic oxide material having a rock-salt-like structure upon the crystalline metal oxide or crystalline metal oxynitride material layer, a layer of a buffer material upon the oriented cubic oxide material layer, and, a top-layer of a high temperature superconducting material upon the layer of a buffer material.

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...

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...

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.

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.

The impact of thermal treatment conditions on the formation of crystalline structure of Ce-Zr-oxide composite obtained by a modified sol-gel technique

NASA Astrophysics Data System (ADS)

Trusova, E. A.; Khrushcheva, A. A.; Shvorneva, L. I.

2012-02-01

We present the results of the modified sol-gel synthesis of ultrafine ceria-doped zirconia powder for medical ceramics (implants) and catalytic purposes (environmental catalysis and petrochemistry). Special attention has been paid to study the influence of thermal treatment on crystallite size and crystal lattice parameters of zirconia doped by ceria. Zirconyl chloride and cerium nitrate were used as metal sources, and tetraethylammonium hydroxide (TEAH) was used as a sol stabilizer at molar ratio TEAH/Σ (Ce + Zr) equal to 0.5. It was proved that zirconium and cerium practically completely were included in the obtained solid solutions, since their phase compositions fully correspond to initial quantities of cerium and zirconium in reaction mixture. It was shown that average crystallite size of the obtained powders did not exceed 75Å, and the powders were resistant to thermal treatment. It was established that stabilization of the crystal lattice of ZrO2 occurs through formation of a cubic ceria sublattice.

Particulate fuel bed tests

NASA Astrophysics Data System (ADS)

Horn, F. L.; Powell, J. R.; Savino, J. M.

Gas-cooled reactors using packed beds of small-diameter, coated fuel particles have been proposed for compact, high-power systems. To test the thermal-hydraulic performance of the particulate reactor fuel under simulated reactor conditions, a bed of 800-micrometer diameter particles was heated by its electrical resistance current and cooled by flowing helium gas. The specific resistance of the bed composed of pyrocarbon-coated particles was measured at several temperatures, and found to be 0.09 ohm-cm at 1273 K and 0.06 ohm-cm at 1600 K. The maximum bed power density reached was 1500 W/cu cm at 1500 K. The pressure drop followed the packed-bed correlation, typically 100,000 Pa/cm. The various frit materials used to contain the bed were also tested to 2000 K in helium and hydrogen to determine their properties and reactions with the fuel. Rhenium metal, zirconium carbide, and zirconium oxide appeared to be the best candidate materials, while tungsten and tungsten-rhenium lost mass and strength.

High Temperature Superconducting Thick Films

DOEpatents

Arendt, Paul N.; Foltyn, Stephen R.; Groves, James R.; Holesinger, Terry G.; Jia, Quanxi

2005-08-23

An article including a substrate, a layer of an inert oxide material upon the surface of the substrate, (generally the inert oxide material layer has a smooth surface, i.e., a RMS roughness of less than about 2 nm), a layer of an amorphous oxide or oxynitride material upon the inert oxide material layer, a layer of an oriented cubic oxide material having a rock-salt-like structure upon the amorphous oxide material layer is provided together with additional layers such as at least one layer of a buffer material upon the oriented cubic oxide material layer or a HTS top-layer of YBCO directly upon the oriented cubic oxide material layer. With a HTS top-layer of YBCO upon at least one layer of a buffer material in such an article, Jc's of 1.4×106 A/cm2 have been demonstrated with projected Ic's of 210 Amperes across a sample 1 cm wide.

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.

Anticorrosive Behavior and Porosity of Tricationic Phosphate and Zirconium Conversion Coating on Galvanized Steel

NASA Astrophysics Data System (ADS)

Velasquez, Camilo S.; Pimenta, Egnalda P. S.; Lins, Vanessa F. C.

2018-05-01

This work evaluates the corrosion resistance of galvanized steel treated with tricationic phosphate and zirconium conversion coating after painting, by using electrochemical techniques, accelerated and field corrosion tests. A non-uniform and heterogeneous distribution of zirconium on the steel surface was observed due to preferential nucleation of the zirconium on the aluminum-rich sites on the surface of galvanized steel. The long-term anti-corrosion performance in a saline solution was better for the phosphate coating up to 120 days. The coating capacitance registered a higher increase for the zirconium coatings than the phosphate coatings up to 120 days of immersion. This result agrees with the higher porosity of zirconium coating in relation to the phosphate coating. After 3840 h of accelerated corrosion test, and after 1 year of accelerated field test, zirconium-treated samples showed an average scribe delamination length higher than the phosphate-treated samples.

Anticorrosive Behavior and Porosity of Tricationic Phosphate and Zirconium Conversion Coating on Galvanized Steel

NASA Astrophysics Data System (ADS)

Velasquez, Camilo S.; Pimenta, Egnalda P. S.; Lins, Vanessa F. C.

2018-04-01

This work evaluates the corrosion resistance of galvanized steel treated with tricationic phosphate and zirconium conversion coating after painting, by using electrochemical techniques, accelerated and field corrosion tests. A non-uniform and heterogeneous distribution of zirconium on the steel surface was observed due to preferential nucleation of the zirconium on the aluminum-rich sites on the surface of galvanized steel. The long-term anti-corrosion performance in a saline solution was better for the phosphate coating up to 120 days. The coating capacitance registered a higher increase for the zirconium coatings than the phosphate coatings up to 120 days of immersion. This result agrees with the higher porosity of zirconium coating in relation to the phosphate coating. After 3840 h of accelerated corrosion test, and after 1 year of accelerated field test, zirconium-treated samples showed an average scribe delamination length higher than the phosphate-treated samples.

Analysis of the influence of the macro- and microstructure of dental zirconium implants on osseointegration: a minipig study.

PubMed

Mueller, Cornelia Katharina; Solcher, Philipp; Peisker, Andrè; Mtsariashvilli, Maia; Schlegel, Karl Andreas; Hildebrand, Gerhard; Rost, Juergen; Liefeith, Klaus; Chen, Jiang; Schultze-Mosgau, Stefan

2013-07-01

It was the aim of this study to analyze the influence of implant design and surface topography on the osseointegration of dental zirconium implants. Six different implant designs were tested in the study. Nine or 10 test implants were inserted in the frontal skull in each of 10 miniature pigs. Biopsies were harvested after 2 and 4 months and subjected to microradiography. No significant differences between titanium and zirconium were found regarding the microradiographically detected bone-implant contact (BIC). Cylindric zirconium implants showed a higher BIC at the 2-month follow-up than conic zirconium implants. Among zirconium implants, those with an intermediate Ra value showed a significantly higher BIC compared with low and high Ra implants 4 months after surgery. Regarding osseointegration, titanium and zirconium showed equal properties. Cylindric implant design and intermediate surface roughness seemed to enhance osseointegration. Copyright © 2013 Elsevier Inc. All rights reserved.

40 CFR 721.10152 - Oxirane, substituted silylmethyl-, hydrolysis products with alkanol zirconium(4+) salt and silica...

Code of Federal Regulations, 2010 CFR

2010-07-01

...-, hydrolysis products with alkanol zirconium(4+) salt and silica, acetates (generic). 721.10152 Section 721... Oxirane, substituted silylmethyl-, hydrolysis products with alkanol zirconium(4+) salt and silica... zirconium(4+) salt and silica, acetates (PMN P-07-674) is subject to reporting under this section for the...

Processing fissile material mixtures containing zirconium and/or carbon

DOEpatents

Johnson, Michael Ernest; Maloney, Martin David

2013-07-02

A method of processing spent TRIZO-coated nuclear fuel may include adding fluoride to complex zirconium present in a dissolved TRIZO-coated fuel. Complexing the zirconium with fluoride may reduce or eliminate the potential for zirconium to interfere with the extraction of uranium and/or transuranics from fission materials in the spent nuclear fuel.