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Sample records for monoclinic zirconium oxide

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2014-01-01

    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

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

    Energy Technology Data Exchange (ETDEWEB)

    Platt, P., E-mail: Philip.Platt@manchester.ac.uk [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom); Frankel, P. [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom); Gass, M.; Howells, R. [AMEC, Walton House, Faraday Street, Birchwood Park, Risley, Warrington WA3 6GA (United Kingdom); Preuss, M. [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom)

    2014-11-15

    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.

  4. Raman spectroscopy study of the tetragonal-to-monoclinic transition in zirconium oxide scales and determination of overall oxygen diffusion by nuclear microanalysis of O18

    International Nuclear Information System (INIS)

    Godlewski, J.; Lambertin, M.; Gros, J.P.; Wadier, J.F.; Weidinger, H.

    1991-01-01

    This paper reports on two allotropic forms of zirconium oxide, monoclinic and tetragonal that have been identified in the scales formed on zirconium alloys. The transition from tetragonal to monoclinic has been followed by Z-ray measurements and Raman laser spectroscopy. Information on the average content of the tetragonal phase was obtained by X-ray diffraction, whereas Raman laser analyses on tapered sections revealed its distribution through the scale thickness. Oxidation exposures were made in an autoclave, using H 2 O 18 and D 2 O 18 to determine the overall diffusion coefficients. In particular, oxide scales have been studied on Zircaloy-4 with three different precipitate sizes, and on a Zr-1Nb alloy, after exposure in an autoclave for between 3 and 100 days. The specimens were analyzed in detail in the vicinity of the kinetics transition point, where the acceleration of corrosion occurs. Raman spectroscopy analyses enabled the crystallographic nature of the ZrO 2 to be determined. Close to the interface, the tetragonal phase content is about 40%, when after the transition the tetragonal phase is transformed into monoclinic. The O 18 diffusion treatment was carried out in an autoclave at 400 degrees C under pressure on specimens previously oxidized for between 3 and 100 days in natural water vapor pressure. The diffusion profiles were determined by nuclear microanalysis using the O 18 (p, α) → N 15 reaction. Based on these profiles, the volume and grain boundary diffusion coefficients were calculated for each material and for each oxidation time

  5. Investigation of Zirconium Oxide Films in Different Dissolved Hydrogen Concentration

    International Nuclear Information System (INIS)

    Kim, Taeho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun

    2016-01-01

    It has been reported that in pre-transition zirconium oxide, the volume fraction of tetragonal zirconium oxide increased near the oxide/metal (O/M) interface, and the sub-stoichiometric zirconium oxide layer was observed. The diffusion of oxygen ion through the oxide layer is the rate-limiting process during the pre-transition oxidation process, and this diffusion mainly occurs in the grain boundaries. The two layered oxide structure is formed in pre-transition oxide for the zirconium alloy in high-temperature water environment. It is known that the corrosion rate is related to the volume fraction of zirconium oxide and the pores in the oxides; therefore, the aim of this paper is to investigate the oxidation behavior in the pre-transition zirconium oxide in high-temperature water chemistry. In this study, in situ Raman and TEM analysis were conducted for investigating the phase transformation of zirconium alloy in primary water. From this study, the following conclusions are drawn: 1. The zirconium alloy was oxidized in primary water chemistry for 100 d, and Raman and TEM were measured after 30, 50, 80, and 100 d from start-up. 2. TEM and FFT analysis showed that the zirconium oxide mostly consisted of the monoclinic phase. The tetragonal zirconium oxide was just found near the O/M interface

  6. A microstuctural study on accelerated zirconium alloy oxidation

    International Nuclear Information System (INIS)

    Sohn, Seung Bum; Oh, Seung Jun; Jang, Jung Nam; Kim, Yong Soo; Jung, Yong Hwan; Baek, Jong Hyuk; Park, Jung Yong

    2005-01-01

    It has been reported that the effect of thermal redistribution of hydrides across the zirconium metaloxide interface, coupled with thermal feedback on the metal-oxide interface, is a dominating factor in the accelerated oxidation in zirconium alloys cladding PWR fuel. Basically this influence determines characteristic of oxide layer. Influence estimation for corrosion oxide layer due to hydrogen / hydride carried out because of investigation on the kinetic on accelerated oxidation due to hydride precipitation was preceded. Generally, it is known that ZrO 2 tetragonal layer structures play an important role as a barrier layer. So analysing the ZrO 2 monoclinic and tetragonal structure distribution is our main aim. Especially, this study focused on the hydride effects. In other words, the difference of crystal structure distribution between pre-hydrided and without hydrided specimen is just expected results. Experimental results of microstructure at zirconium metal-oxide interface through TEM and EBSD analysis was confirmed

  7. In situ Raman Spectroscopy of Oxide Films on Zirconium Alloy in Simulated PWR Primary Water Condition

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Tae Ho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun [UNIST, Ulsan (Korea, Republic of)

    2016-05-15

    The two layered oxide structure is formed in pre-transition oxide for the zirconium alloy in high temperature water environment. It is known that the corrosion rate is related to the volume fraction of zirconium oxide and the pores in the oxides; therefore, the aim of this paper is to investigate the oxidation behavior in the pretransition zirconium oxide in high-temperature water chemistry. In this work, Raman spectroscopy was used for in situ investigations for characterizing the phase of zirconium oxide. In situ Raman spectroscopy is a well-suited technique for investigating in detail the characteristics of oxide films in a high-temperature corrosion environment. In previous studies, an in situ Raman system was developed for investigating the oxides on nickel-based alloys and low alloy steels in high-temperature water environment. Also, the early stage oxidation behavior of zirconium alloy with different dissolved hydrogen concentration environments in high temperature water was treated in the authors' previous study. In this study, a specific zirconium alloy was oxidized and investigated with in situ Raman spectroscopy for 100 d oxidation, which is close to the first transition time of the zirconium alloy oxidation. The ex situ investigation methods such as transmission electron microscopy (TEM) and energy dispersive X-ray spectroscopy (EDS) were used to further characterize the zirconium oxide structure. As oxidation time increased, the Raman peaks of tetragonal zirconium oxide were merged or became weaker. However, the monoclinic zirconium oxide peaks became distinct. The tetragonal zirconium oxide was just found near the O/M interface and this could explain the Raman spectra difference between the 30 d result and others.

  8. Thin zirconium oxides

    International Nuclear Information System (INIS)

    Oviedo, Cristina

    2000-01-01

    Polycrystalline Zr and two pure Zr single-crystal samples, one oriented with the normal to the surface parallel to the c-axis of the hcp structure (Z1) and the other with the normal perpendicular to c (Z2), were oxidised at 10 -8 , 10 -7 and 10 -6 Torr and room temperature. Oxidation kinetics, composition and thicknesses of the oxide films formed in each case were analyzed using XPS (X-ray Photoelectron Spectroscopy) as the main technique. The oxidation kinetics followed logarithmic laws in all cases. The deconvolution of XPS Zr3d peaks indicated the formation of two Zr-O compounds before the formation of ZrO 2 . Varying the photoelectrons take-off angle, the compound distribution inside the oxide films could be established. Thus, it was confirmed that the most external oxide, in contact with the gas, was ZrO 2 . The thickness of the films grown at the different pressures was determined. In the polycrystalline samples, thicknesses between 15 and 19 ± 2Angstroem were obtained for pressures between 10 -8 and 10 -6 Torr, in close coincidence with the determined ones for Z2. The thicknesses measured in Z1 were smaller, reaching 13 ± 2Angstroem for the oxidations performed at 10 -6 Torr. (author)

  9. In situ Investigation of Oxide Films on Zirconium Alloy in PWR Primary Water Chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Taeho; Choi, Kyoung Joon; Yoo, Seung Chang; Kim, Ji Hyun [Ulsan National Institute of Science and Technology, Ulsan (Korea, Republic of)

    2015-05-15

    Zirconium alloys are used as fuel cladding materials in nuclear power reactors, because these materials have a very low thermal neutron capture cross section as well as desirable mechanical properties. However, the Fukushima accident shows that the oxidation behavior of zirconium alloy is an important issue because the zirconium alloy functions as a shield of nuclear material (i.e., uranium, fission gas), and the degradation on zirconium cladding directly causes severe accident on nuclear power plant. Therefore, to ensure the safety of nuclear power reactors, the performance and sustainability of nuclear fuel should be understood. Currently, the water-metal interface is regarded as the rate-controlling site governing the rapid oxidation transition in high-burn-up fuels. Zirconium oxide is formed at the water-metal interface, and its structure and phase play an important role in determining its mechanical properties. In the early stage of the oxidation process, zirconium oxide with both tetragonal and monoclinic phases is formed. With an increase in the oxidation time to 150 h, the unstable tetragonal phase disappears and the monoclinic phase is dominant and possibly because of the stress relaxation according to previous and present results.

  10. Oxidation of zirconium alloys in steam: influence of tetragonal zirconia on oxide growth mechanism

    International Nuclear Information System (INIS)

    Godlewski, J.

    1990-07-01

    The oxidation of zirconium alloys in presence of steam, presents after a 'parabolic' growth law, an acceleration of the oxidation velocity. This phenomenon limits the use of zirconium alloys as nuclear fuel cladding element. In order to determine the physico-chemical process leading to this kinetic transition, two approaches have been carried out: the first one has consisted to determine the composition of the oxide layer and its evolution with the oxidation time; and the second one to determine the oxygen diffusion coefficients in the oxide layers of pre- and post-transition as well as their evolution with the oxidation time. The composition of the oxide layers has been determined by two analyses techniques: the X-ray diffraction and the laser Raman spectroscopy. This last method has allowed to confirm the presence of tetragonal zirconium oxide in the oxide layers. Analyses carried out by laser Raman spectroscopy on oxides oblique cuttings have revealed that the tetragonal zirconium oxide is transformed in monoclinic phase during the kinetic transition. A quantitative approach has allowed to corroborate the results obtained by these two techniques. In order to determine the oxygen diffusion coefficients in the oxides layers, two diffusion treatments have been carried out: 1)under low pressure with D 2 18 O 2 ) under high pressure in an autoclave with H 2 18 O. The oxygen 18 concentration profiles have been obtained by two analyses techniques: the nuclear microprobe and the secondary ions emission spectroscopy. The obtained profiles show that the mass transport is made by the volume and particularly by the grain boundaries. The corresponding diffusion coefficients have been calculated with the WHIPPLE and LE CLAIRE solution. The presence of tetragonal zirconium oxide, its relation with the kinetic transition, and the evolution of the diffusion coefficients with the oxidation time, are discussed in terms of internal stresses in the oxide layer and of the oxide layer

  11. Oxidized zirconium on ceramic; Catastrophic coupling.

    Science.gov (United States)

    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.

  12. Study for the chlorination of zirconium oxide

    International Nuclear Information System (INIS)

    Seo, E.S.M.; Takiishi, H.; Paschoal, J.O.A.; Andreoli, M.

    1990-12-01

    In the development of new ceramic and metallic materials the chlorination process constitutes step in the formation of several intermediate compounds, such as metallic chlorides, used for the production of high, purity raw materials. Chlorination studies with the aim of fabrication special zirconium-base alloys have been carried out at IPEN. Within this program the chlorination technique has been used for zirconium tetrachloride production from zirconium oxide. In this paper some relevant parameters such as: time and temperature of reaction, flow rate of chloride gas and percentage of the reducing agent which influence the efficiency of chlorination of zirconium oxide are evaluated. Thermodynamical aspects about the reactions involved in the process are also presented. (author)

  13. The effect of crystal textures on the anodic oxidization of zirconium in a boiling nitric acid solution

    International Nuclear Information System (INIS)

    Kato, Chiaki; Ishijima, Yasuhiro; Ueno, Fumiyoshi; Yamamoto, Masahiro

    2016-01-01

    to monoclinic ZrO_2. It is not well known why the cracks propagate along the (0002)_Z_r plane under the thick oxide film. As one assumption for the mechanism of crack initiation and propagation without an external stress, it is considered that the oxidizing zirconium hydrides precipitated in the (0002)_Z_r plane near the interface of the thick oxide film and the matrix. Then, the phase transformation from orthorhombic ZrO_2 to monoclinic ZrO_2 in the oxide layer causes the crack propagation in the (0002) plane. (author)

  14. Investigation of anodic oxide coatings on zirconium after heat treatment

    International Nuclear Information System (INIS)

    Sowa, Maciej; Dercz, Grzegorz; Suchanek, Katarzyna; Simka, Wojciech

    2015-01-01

    Highlights: • Oxide layers prepared via PEO of zirconium were subjected to heat treatment. • Surface characteristics were determined for the obtained oxide coatings. • Heat treatment led to the partial destruction of the anodic oxide layer. • Pitting corrosion resistance of zirconium was improved after the modification. - Abstract: Herein, results of heat treatment of zirconium anodised under plasma electrolytic oxidation (PEO) conditions at 500–800 °C are presented. The obtained oxide films were investigated by means of SEM, XRD and Raman spectroscopy. The corrosion resistance of the zirconium specimens was evaluated in Ringer's solution. A bilayer oxide coatings generated in the course of PEO of zirconium were not observed after the heat treatment. The resulting oxide layers contained a new sublayer located at the metal/oxide interface is suggested to originate from the thermal oxidation of zirconium. The corrosion resistance of the anodised metal was improved after the heat treatment

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

    Science.gov (United States)

    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...Zirconia-Oxide Materials 6. TITLE OF MATERIAL TO BE PUBLISHED OR PRESENTED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide...OBSOLETE 48. DATE Page 3 of 3 Pages Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials

  16. Traps in Zirconium Alloys Oxide Layers

    Directory of Open Access Journals (Sweden)

    Helmar Frank

    2005-01-01

    Full Text Available Oxide films long-time grown on tubes of three types of zirconium alloys in water and in steam were investigated, by analysing I-V characteristic measured at constant voltages with various temperatures. Using theoretical concepts of Rose [3] and Gould [5], ZryNbSn(Fe proved to have an exponential distribution of trapping centers below the conduction band edge, wheras Zr1Nb and IMP Zry-4 proved to have single energy trap levels.

  17. Zirconium oxide obtainment from brazilian zircon concentrate

    International Nuclear Information System (INIS)

    Ribeiro, S.; Martins, A.H.

    1991-01-01

    This work presents the experimental results of studies about alkaline melting, acid leaching and sulfation steps for obtention of zirconium oxide and partially stabilized zirconia by yttrium and rare-earth coprecipitation in chlorine medium, starting from the brazilian zircon concentrate. Using statistical methods of factorial design and the Packett-Burman approach, the results are discussed and the optimal conditions of the production steps were determined. (author)

  18. The effect of substrate texture and oxidation temperature on oxide texture development in zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Garner, A., E-mail: alistair.garner@manchester.ac.uk [Materials Performance Centre, University of Manchester, Grosvenor Street, Manchester, M17HS (United Kingdom); Frankel, P. [Materials Performance Centre, University of Manchester, Grosvenor Street, Manchester, M17HS (United Kingdom); Partezana, J. [Westinghouse Electric Company, 1332 Beulah Road, Pittsburgh, PA 15235 (United States); Preuss, M. [Materials Performance Centre, University of Manchester, Grosvenor Street, Manchester, M17HS (United Kingdom)

    2017-02-15

    During corrosion of zirconium alloys a highly textured oxide is formed, the degree of this preferred orientation has previously been shown to be an important factor in determining the corrosion behaviour of these alloys. Two distinct experiments were designed in order to investigate the origin of this oxide texture development on two commercial alloys. Firstly, sheet samples of Zircaloy-4 were oxidised between 500 and 800 °C in air. The resulting monoclinic oxide texture strength was observed to decrease with increasing oxidation temperature. In a second experiment, orthogonal faces of Low Tin ZIRLO{sub ™} were oxidised in 360 °C water, providing different substrate textures but identical microstructures. The substrate texture was observed to have a negligible effect on the corrosion performance whilst the major orientation of both oxide phases was found to be independent of substrate orientation. It is concluded that the main driving force for oxide texture development in single-phase zirconium alloys is the compressive stress caused by the Zr−ZrO{sub 2} transformation. - Highlights: • Substrate orientation does not significantly affect oxide texture development. • Corrosion performance is independent of substrate texture. • Monoclinic oxide texture strength decreases with increasing oxidation temperature. • The main driving force for texture development is the oxidation-induced stress.

  19. Diffusion of insoluble carbon in zirconium oxides

    CERN Document Server

    Vykhodets, V B; Koester, U; Kondrat'ev, V V; Kesarev, A G; Hulsen, C; Kurennykh, T E

    2011-01-01

    The diffusion coefficient of insoluble carbon in zirconium oxides has been obtained for the temperature range of 900-1000A degrees C. There are no published data on the diffusion of insoluble impurities; these data are of current interest for the diffusion theory and nuclear technologies. Tracer atoms 13C have been introduced into oxides by means of ion implantation and the kinetics of their emission from the samples in the process of annealing in air has been analyzed. The measurements have been performed using the methods of nuclear microanalysis and X-ray photoelectron spectroscopy. The diffusion activation energy is 2.7 eV and the carbon diffusion coefficient is about six orders of magnitude smaller than that for oxygen self-diffusion in the same systems. This result indicates the strong anomaly of the diffusion properties of carbon in oxides. As a result, zirconium oxides cannot be used in some nuclear technologies, in particular, as a material of sources for accelerators of short-lived carbon isotopes.

  20. Swelling of a Zirconium Oxide Film

    International Nuclear Information System (INIS)

    Henderson, Mark; Hawley, Adrian; White, John; Rennie, Adrian

    2005-01-01

    Full text: The structural changes that cause the change in the interlayer spacing of a surfactanttemplated zirconium oxide film have been studied using neutron diffractometry. We report that the film after drying on a glass substrate swells slightly through the addition of benzene by up to 4 Aangstroem on a lattice parameter of about 36 Aangstroem. The (001) and (002) diffraction peaks positions, widths and areas of a swollen film were then monitored by neutron diffraction as a function of benzene desorption. Disorder of the lamellar mesophase is considered as a cause of the observed effects on the diffraction signals. (authors)

  1. Swelling of a mesostructured zirconium oxide film

    Energy Technology Data Exchange (ETDEWEB)

    Henderson, M.J. [Research School of Chemistry, Australian National University, Canberra, ACT 0200 (Australia); Rennie, A.R. [Uppsala University, Studsvik Neutron Research Laboratory, S-611 82 Nykoeping (Sweden); Hawley, A.M. [Research School of Chemistry, Australian National University, Canberra, ACT 0200 (Australia); White, J.W. [Research School of Chemistry, Australian National University, Canberra, ACT 0200 (Australia)]. E-mail: jww@rsc.anu.edu.au

    2006-11-15

    The structural changes that cause the change in interlayer spacing of a surfactant-templated zirconium oxide film have been studied using neutron diffractometry. We report that the film after drying on a glass substrate swells slightly through the addition of benzene by up to 4 A on a lattice parameter of about 36 A. The (0 0 1) and (0 0 2) diffraction peak widths, positions and areas of a swollen film were monitored as a function of benzene desorption. Disorder of the lamellar mesophase is considered as a cause of the observed effects on the diffraction signals.

  2. Oxidation of zirconium-aluminum alloys

    International Nuclear Information System (INIS)

    Cox, B.

    1967-10-01

    Examination of the processes occurring during the oxidation of Zr-1% A1, Zr-3% A1, and Zr-1.5% A1-0.5% Mo alloys has shown that in steam rapid oxidation occurs predominantly around the Zr 3 A1 particles, which at low temperatures appear to be relatively unattacked. The unoxidised particles become incorporated in the oxide, and become fully oxidised as the film thickens. This rapid localised oxidation is preceded by a short period of uniform film growth, during which the oxide film thickness does not exceed ∼200A-o. Thus the high oxidation rates can probably be ascribed to aluminum in solution in the zirconium matrix, although its precise mode of operation has not been determined. Once the solubility limit of aluminum is exceeded, the size, distribution and number of intermetallic particles affects the oxidation rate merely by altering the distribution of regions of metal giving high oxidation rates. The controlling process during the early stages of oxidation is electron transport and not ionic transport. Thus, the aluminum in the oxide film is presumably increasing the ionic conductivity more than the electronic. The oxidation rates in atmospheric pressure steam are very high and their irregular temperature dependence suggests that the oxidation rate will be pressure dependent. This was confirmed, in part, by a comparison with oxidation in moist air. It was found that the rate of development of white oxide around intermetallic particles was considerably reduced by the decrease in the partial pressure of H 2 O; the incubation period was not much different, however. (author)

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

    Science.gov (United States)

    2016-05-12

    Capt Todd D. Church APPROVED: Translucency and Strength of High-Translucency Monolithic Zirconium -Oxide Materials C~t) Kraig/[ Vandewalle Date...copyrighted material in the thesis/dissertation manuscript entitled: "Translucency arid Strength of High-Translucency Monolithic Zirconium -Oxide...Translucency Monolithic Zirconium -Oxide Materials Abstract Dental materials manufacturers have developed more translucent monolithic zirconium oxide

  4. Characterization of zirconium alloy oxidation films by alternating current impedance

    International Nuclear Information System (INIS)

    Rosecrans, P.M.

    1984-01-01

    Kinetics of zirconium alloy oxidation are highly nonlinear. The results of electrochemical measurements and electron microscopy support the existence of porosity in oxide films formed on zirconium alloys in high temperature aqueous environments. Analytical treatment is presented relating oxidation kinetics to the thickness and distribution of nonporous elements within the oxide. This analysis illustrates that both the level and distribution of porosity within the oxide factor into oxidation kinetics. The barrier layer model can provide a basis for predicting the effect of environmental changes on oxidation rate. In addition, it demonstrates the need for further research into porosity generation mechanisms in oxide films

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

    Energy Technology Data Exchange (ETDEWEB)

    Kurpaska, L., E-mail: lukasz.kurpaska@ncbj.gov.pl [Laboratoire Roberval, UMR 7337, Université de Technologie de Compiègne, Centre de Recherche de Royallieu, CS 60319, 60203 Compiègne Cedex (France); National Center for Nuclear Research, St. A. Soltana 7/23, 05-400 Otwock-Swierk (Poland); Favergeon, J. [Laboratoire Roberval, UMR 7337, Université de Technologie de Compiègne, Centre de Recherche de Royallieu, CS 60319, 60203 Compiègne Cedex (France); Lahoche, L. [Laboratoire Roberval, UMR 7337, Université de Technologie de Compiègne, Centre de Recherche de Royallieu, CS 60319, 60203 Compiègne Cedex (France); Laboratoire des Technologies Innovantes, Université de Picardie Jules-Verne, EA 3899, Avenue des Facultés – Le Bailly, 80025 Amiens Cedex (France); El-Marssi, M. [Laboratoire de Physique de la Matière Condensée, Université de Picardie Jules-Verne, 33 rue St. Leu, 80039 Amiens Cedex (France); Grosseau Poussard, J.-L. [LaSIE UMR-CNRS 7356, Pole Sciences et Technologie, Universite de La Rochelle, av. M Crepeau, 17042 La Rochelle, Cedex (France); Moulin, G.; Roelandt, J.-M. [Laboratoire Roberval, UMR 7337, Université de Technologie de Compiègne, Centre de Recherche de Royallieu, CS 60319, 60203 Compiègne Cedex (France)

    2015-11-15

    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. - Highlights: • The oxide layer consists of a mixture of tetragonal and monoclinic phases, clearly distinguishable by Raman spectroscopy. • The layer located close to the metal/oxide interphase consists mainly of the tetragonal phase. • Small amount of tetragonal layer located in the external oxide scale have been observed. • Stabilization mechanism of the tetragonal phase located in the external part of the oxide have been proposed.

  6. Oxidation kinetics of some zirconium alloys in flowing carbon dioxide at high temperatures

    International Nuclear Information System (INIS)

    Kohli, R.

    1980-01-01

    The oxidation kinetics of three zirconium alloys (Zr-2.2 wt% Hf, Zr-2.5 wt% Nb, and Zr-3 wt% Nb-1 wt% Sn) have been measured in flowing carbon dioxide in the temperature range from 873 to 1173 K to 120 ks (2000 min). At all oxidation temperatures, Zr-2.5 Nb and Zr-3 Nb-1 Sn showed a transition to rapid linear kinetics after initial parabolic oxidation. The Zr-2.2 Hf showed this transition at temperatures in the range from 973 to 1173 K; at 873 K, no transition was observed within the oxidation times reported. The Zr-2.2 Hf showed the smallest weight gains, followed in order by Zr-2.5 Nb and Zr-3 Nb-1 Sn. Increased oxidation rates and shorter times-to-rate-transition of Zr-2.2 Nb and Zr-1 Sn as compared with Zr-2.2 Hf can be attributed to the presence of niobium, tin, and hafnium in the alloys. This is considered in terms of the Nomura-Akutsu model, according to which hafnium should delay the rate transition, while niobium and tin lead to shorter times-to-rate-transition. The scale on Zr-2.2 Hf was identified as monoclinic zirconia, while the tetragonal phase, 6ZrO 2 .Nb 2 O 5 , was contained in the monoclinic zirconia scales on both other alloys

  7. Characterization of zirconium alloy oxidation films by alternating current impedance

    International Nuclear Information System (INIS)

    Rosecrans, P.M.

    1983-11-01

    Kinetics of zirocnium alloy oxidation are highly nonlinear. The results of electrochemical measurements and electron microscopy support the existence of porosity in oxide films formed on zirconium alloys in high temperature aqueous environments. Analytical treatment is presented relating oxidation kinetics to the thickness and distribution of nonporous elements within the oxide. This analysis illustrates that both the level and distribution of porosity within the oxide factor into oxidation kinetics. The barrier layer model can provide a basis for predicting the effect of environmental changes on oxidation rate. In addition, it demonstrates the need for further research into porosity generation mechanisms in oxide films

  8. Microstructural aspects of the oxidation of zirconium alloys

    International Nuclear Information System (INIS)

    Proff, Ch.

    2011-01-01

    This thesis is focused on the microstructural characterisation of precipitates in the oxide of binary zirconium alloys (1 wt.% Fe, Cr or Ni or 0.6 wt.% Nb) under different oxidation conditions at 415 C. The samples were oxidised in autoclave in air and steam and in an environmental scanning electron microscope in water vapour. The microstructural evolution of the precipitates during oxidation was characterised using electron microscopy. The findings from the analysis are the following: -Two types of oxidation behaviour are observed for precipitates. -Pilling Bedworth ratio of precipitates is higher than that of the zirconium matrix. -Formation of pure iron oxide crystals on the surface for iron bearing precipitates close to or at the surface. From these observations it is concluded that the precipitate oxidation behaviour can be correlated to precipitate composition and oxidation tendency of the elements in the precipitates. Iron exhibits clearly different behaviour. (author)

  9. Enhanced low-temperature oxidation of zirconium alloys under irradiation

    International Nuclear Information System (INIS)

    Cox, B.; Fidleris, V.

    1989-01-01

    The linear growth of relatively thick (>300 nm) interference-colored oxide films on zirconium alloy specimens exposed in the Advanced Test Reactor (ATR) coolant at ≤55 o C was unexpected. Initial ideas were that this was a photoconduction effect. Experiments to study photoconduction in thin anodic zirconium oxide (ZrO 2 ) films in the laboratory were initiated to provide background data. It was found that, in the laboratory, provided a high electric field was maintained across the oxide during ultraviolet (UV) irradiation, enhanced growth of oxide occurred in the irradiated area. Similarly enhanced growth could be obtained on thin thermally formed oxide films that were immersed in an electrolyte with a high electric field superimposed. This enhanced growth was found to be caused by the development of porosity in the barrier oxide layer by an enhanced local dissolution and reprecipitation process during UV irradiation. Similar porosity was observed in the oxide films on the ATR specimens. Since it is not thought that a high electric field could have been present in this instance, localized dissolution of fast-neutron primary recoil tracks may be the operative mechanism. In all instances, the specimens attempt to maintain the normal barrier-layer oxide thickness, which causes the additional oxide growth. Similar mechanisms may have operated during the formation of thick loosely adherent, porous oxides in homogeneous reactor solutions under irradiation, and may be the cause of enhanced oxidation of zirconium alloys in high-temperature water-cooled reactors in some water chemistries. (author)

  10. Effect of boron oxide on the cubic-to-monoclinic phase transition in yttria-stabilized zirconia

    International Nuclear Information System (INIS)

    Florio, D.Z. de; Muccillo, R.

    2004-01-01

    Specimens of yttria fully stabilized zirconia with different amounts of boron oxide have been studied by X-ray diffraction at room temperature and at higher temperatures up to 1250 deg. C. A boron oxide-assisted cubic-to-monoclinic phase transformation was determined in the temperature range 800-1250 deg. C. In situ high temperature X-ray diffraction experiments gave evidences of the dependence of the phase transformation on the heating rate. The possibility of tuning the cubic-monoclinic phase ratio by suitable addition of boron oxide before pressing and sintering is proposed

  11. Standard Specification for Nuclear Grade Zirconium Oxide Pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2009-01-01

    1.1 This specification applies to pellets of stabilized zirconium oxide used in nuclear reactors. 1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.

  12. Influence of protecting gel film on oxidation of zirconium alloys

    Czech Academy of Sciences Publication Activity Database

    Frank, H.; Weishauptová, Zuzana; Vrtílková, V.

    2007-01-01

    Roč. 360, č. 3 (2007), s. 282-292 ISSN 0022-3115 R&D Projects: GA ČR GA106/04/0043 Institutional research plan: CEZ:AV0Z30460519 Keywords : fuel cladding * corrosion * Zirconium oxide Subject RIV: JF - Nuclear Energetics Impact factor: 1.643, year: 2007

  13. Synthesis and characterization of a mesoporous hydrous zirconium oxide used for arsenic removal from drinking water

    International Nuclear Information System (INIS)

    Bortun, Anatoly; Bortun, Mila; Pardini, James; Khainakov, Sergei A.; Garcia, Jose R.

    2010-01-01

    Powder (20-50 μm) mesoporous hydrous zirconium oxide was prepared from a zirconium salt granular precursor. The effect of some process parameters on product morphology, porous structure and adsorption performance has been studied. The use of hydrous zirconium oxide for selective arsenic removal from drinking water is discussed.

  14. KINETIC STUDY OF SELECTIVE GAS-PHASE OXIDATION OF ISOPROPANOL TO ACETONE USING MONOCLINIC ZRO2 AS A CATALYST

    Directory of Open Access Journals (Sweden)

    Mohammad Sadiq

    2015-08-01

    Full Text Available Zirconia was prepared by a precipitation method and calcined at 723 K, 1023 K, and 1253 K in order to obtain monoclinic zirconia. The prepared zirconia was characterized by XRD, SEM, EDX, surface area and pore size analyzer, and particle size analyzer. Monoclinic ZrO2 as a catalyst was used for the gas-phase oxidation of isopropanol to acetone in a Pyrex-glass-flow-type reactor with a temperature range of 443 K - 473 K. It was found that monoclinic ZrO2 shows remarkable catalytic activity (68% and selectivity (100% for the oxidation of isopropanol to acetone. This kinetic study reveals that the oxidation of isopropanol to acetone follows the L-H mechanism.

  15. Films of double oxides of zirconium and iron

    International Nuclear Information System (INIS)

    Kozik, V.V.; Borilo, L.P.; Shul'pekov, A.M.

    2000-01-01

    Films of double oxides of zirconium and iron were prepared by the method of precipitation from film-forming alcohol solutions of zirconium oxychloride and iron chloride with subsequent thermal treatment. Using the methods of X-ray phase and differential thermal analyses, conductometry and optical spectroscopy, basic chemical processes occurring in the film-forming solutions and during thermal treatment are studied alongside with phase composition and optical characteristics of the films prepared. The composition-property diagrams of the given system in a thin-film state are plotted [ru

  16. Study of the pelletizing process zirconium oxide and zircon sand

    International Nuclear Information System (INIS)

    Seo, E.S.M.; Paschoal, J.O.A.; Acevedo, M.T.P.

    1990-12-01

    The study of the process to obtain zirconium tetrachloride under development at IPEN, can be divide into two steps: pelletizing and chlorination. Pelletizing is an important step in the overall process as it facilitates greater contact between the particles and permits the production of pellets with dimensional uniformity and mechanical strength. In this paper, the results of the study of pelletizing zirconium oxide and zircon sand are presented. The influence of some variables related to the process and the equipment on the physical characteristics of the pellets are discussed. (author)

  17. Reaction of hydrogen peroxide with uranium zirconium oxide solid solution - Zirconium hinders oxidative uranium dissolution

    Science.gov (United States)

    Kumagai, Yuta; Takano, Masahide; Watanabe, Masayuki

    2017-12-01

    We studied oxidative dissolution of uranium and zirconium oxide [(U,Zr)O2] in aqueous H2O2 solution to estimate (U,Zr)O2 stability to interfacial reactions with H2O2. Studies on the interfacial reactions are essential for anticipating how a (U,Zr)O2-based molten fuel may chemically degrade after a severe accident. The fuel's high radioactivity induces water radiolysis and continuous H2O2 generation. Subsequent reaction of the fuel with H2O2 may oxidize the fuel surface and facilitate U dissolution. We conducted our experiments with (U,Zr)O2 powder (comprising Zr:U mole ratios of 25:75, 40:60, and 50:50) and quantitated the H2O2 reaction via dissolved U and H2O2 concentrations. Although (U,Zr)O2 reacted more quickly than UO2, the dissolution yield relative to H2O2 consumption was far less for (U,Zr)O2 compared to that of UO2. The reaction kinetics indicates that most of the H2O2 catalytically decomposed to O2 at the surface of (U,Zr)O2. We confirmed the H2O2 catalytic decomposition via O2 production (quantitative stoichiometric agreement). In addition, post-reaction Raman scattering spectra of the undissolved (U,Zr)O2 showed no additional peaks (indicating a lack of secondary phase formation). The (U,Zr)O2 matrix is much more stable than UO2 against H2O2-induced oxidative dissolution. Our findings will improve understanding on the molten fuels and provide an insight into decommissioning activities after a severe accident.

  18. MOCVD of zirconium oxide thin films: Synthesis and characterization

    International Nuclear Information System (INIS)

    Torres-Huerta, A.M.; Dominguez-Crespo, M.A.; Ramirez-Meneses, E.; Vargas-Garcia, J.R.

    2009-01-01

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO 2 thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  19. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atohuer@hotmail.com [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Dominguez-Crespo, M.A.; Ramirez-Meneses, E. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Vargas-Garcia, J.R. [ESIQIE, Departamento de Metalurgia y Materiales, Instituto Politecnico Nacional. A.P. 75-876, 07300 Mexico, D.F. (Mexico)

    2009-02-15

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO{sub 2} thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  20. Extraction of zirconium from raffinate stream of Zirconium Oxide Plant raffinate

    International Nuclear Information System (INIS)

    Pandey, Garima; Chinchale, R.; Renjith, A.U.; Mukhopadhyay, S.; Shenoy, K.T.; Ghosh, S.K.

    2013-01-01

    Recovery of metals from dilute streams is a major task in nuclear industry in the view of environmental remediation and value recovery. Presently solvent extraction process is employed on the commercial scale to recover nuclear pure zirconium using TBP as extractant. The waste stream of TBP extraction process contains about 1.2 gpl of Zirconium in nitrate form. At present there is no process to recover Zirconium from this raffinate stream. Hence, under the present study recovery of zirconium from the raffinate stream of Zirconium Oxide Plant Raffinate has been investigated. TBP, which is the most commonly used solvent in the nuclear industry is not suitable for the extraction of zirconium from lean solution at low acidity as its distribution coefficient is less than one. In search of a suitable extractant Mixed Alkyl Phosphine Oxide (MAPO) was investigated as potential carrier. Parametric batch studies for various equilibrium data like extractant concentration, strippant concentration, solvent reusability, equilibration time, acidity etc. were done to optimize the process condition. For the distribution studies, equal volumes of the raffinate and organic phase were shaken at room temperature in digital wrist action shaker for 10 minutes to ensure complete equilibrium. It was found that 0.1 M MAPO in 80:20 dodecane: isodecanol is suitable for extraction of Zr at 2 N acidity. 0.1 M MAPO gives distribution coefficient in the range of 12-15 for Zr. The slope of log-log plot between MAPO concentration and K, suggests involvement of 3 molecules of MAPO in the formation of extracting species. 0.2 M Oxalic acid was able to completely back extract Zr from the organic phase into aqueous phase. Also good regeneration capacity of MAPO projects its potential to be used as extractant for the process. Based on the equilibrium studies, Dispersion Liquid Membrane configuration in hollow fiber contactor was explored for the extraction of Zirconium from Zirconium Nitrate Pure

  1. Zirconium oxide crystal phase: The role of the pH and time to attain the final pH for precipitation of the hydrous oxide

    International Nuclear Information System (INIS)

    Srinivasan, R.; Harris, M.B.; Simpson, S.F.; De Angelis, R.J.; Davis, B.H.

    1988-01-01

    Precipitated hydrous zirconium oxide can be calcined to produce either a monoclinic or tetragonal product. It has been observed that the time taken to attain the final pH of the solution in contact with the precipitate plays a dominant role in determining the crystal structure of the zirconium oxide after calcination at 500 0 C. The dependence of crystal structure on the rate of precipitation is observed only in the pH range 7--11. Rapid precipitation in this pH range yields predominately monoclinic zirconia, whereas slow (8 h) precipitation produces the tetragonal phase. At pH of approximately 13.0, only the tetragonal phase is formed from both slowly and rapidly precipitated hydrous oxide. The present results, together with earlier results, show that both the pH of the supernatant liquid and the time taken to attain this pH play dominant roles in determining the crystal structure of zirconia that is formed after calcination of the hydrous oxide. The factors that determine the crystal phase are therefore imparted in a mechanism of precipitation that depends upon the pH, and it is inferred that it is the hydroxyl concentration that is the dominant factor

  2. Standard specification for nuclear-grade zirconium oxide powder

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 This specification defines the physical and chemical requirements for zirconium oxide powder intended for fabrication into shapes, either entirely or partially of zirconia, for use in a nuclear reactor core. 1.2 The material described herein shall be particulate in nature. 1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

  3. Zirconium

    Science.gov (United States)

    Bedinger, G.M.

    2013-01-01

    Zirconium is the 20th most abundant element in the Earth’s crust. It occurs in a variety of rock types and geologic environments but most often in igneous rocks in the form of zircon (ZrSiO4). Zircon is recovered as a coproduct of the mining and processing of heavy mineral sands for the titanium minerals ilmenite and rutile. The sands are formed by the weathering and erosion of rock containing zircon and titanium heavy minerals and their subsequent concentration in sedimentary systems, particularly in coastal environments. A small quantity of zirconium, less than 10 kt/a (11,000 stpy), compared with total world production of 1.4 Mt (1.5 million st) in 2012, was derived from the mineral baddeleyite (ZrO2), produced from a single source in Kovdor, Russia.

  4. Oxidation kinetics of zirconium nitride. I. Planar symmetry

    International Nuclear Information System (INIS)

    Desmaison, Jean; Billy, Michel

    1976-01-01

    The oxidation behavior of ZrNsub(0.93) plates was investigated at temperatures in the range 625-800 deg C in oxygen over the pressure range 10-730 torr. The reaction product consists of monoclinic zirconia accompanied with trace amounts of cubic or tetragonal zirconia. Although the kinetic results are well interpreted by a Prout and Tompkins type model. The morphological observations suggest a transformation governed by a phase boundary reaction, this being confirmed by the oxygen pressure dependence on the rate law [fr

  5. Obtainment of zirconium oxide and partially stabilized zirconium oxide with yttrium and rare earth oxides, from Brazilian zirconite, for ceramic aim

    International Nuclear Information System (INIS)

    Ribeiro, S.

    1991-05-01

    This work presents experimental results for processing of brazilian zirconite in order to obtain zirconium oxide with Yttrium and Rare Earth oxide by mutual coprecipitation for ceramics purposes. Due to analysis of experimental results was possible to obtain the optimum conditions for each one of technological route stage, such as: alkaline fusion; acid leaching; sulfactation and coprecipitation. (author)

  6. Growth and characterization of oxide layers on zirconium alloys

    International Nuclear Information System (INIS)

    Maroto, A.J.G.; Bordoni, R.; Villegas, M.; Blesa, M.A.; Olmedo, A.M.; Iglesias, A.; Rigotti, G.

    1997-01-01

    Corrosion behaviour in aqueous media at high temperature of zirconium alloys has been extensively studied in order to elucidate the corrosion mechanism and kinetics. The characterization of the morphology and microstructure of these oxides through the different stages of oxide growth may contribute to understand their corrosion mechanism. Argentina has initiated a research program to correlate long term in and out-reactor corrosion of these alloys. This paper reports a comparative study of out of pile oxidation of Zr-2.5Nb and Zry-4, which are structural materials of in-core components of nuclear power plants. Kinetic data at different temperatures and microstructural characterization of the oxide films are presented. (author). 25 refs, 18 figs, 1 tab

  7. Growth and characterization of oxide layers on zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Maroto, A J.G.; Bordoni, R; Villegas, M; Blesa, M A; Olmedo, A M; Iglesias, A; Rigotti, G [Comision Nacional de Energia Atomica, Buenos Aires (Argentina)

    1997-02-01

    Corrosion behaviour in aqueous media at high temperature of zirconium alloys has been extensively studied in order to elucidate the corrosion mechanism and kinetics. The characterization of the morphology and microstructure of these oxides through the different stages of oxide growth may contribute to understand their corrosion mechanism. Argentina has initiated a research program to correlate long term in and out-reactor corrosion of these alloys. This paper reports a comparative study of out of pile oxidation of Zr-2.5Nb and Zry-4, which are structural materials of in-core components of nuclear power plants. Kinetic data at different temperatures and microstructural characterization of the oxide films are presented. (author). 25 refs, 18 figs, 1 tab.

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

    Science.gov (United States)

    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.

  9. Swift heavy ion induced phase transformation and thermoluminescence properties of zirconium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Lokesha, H.S. [Physics R & D Centre, PES Institute of Technology, BSK 3rd Stage, Bangalore 560085 (India); Nagabhushana, K.R., E-mail: bhushankr@gmail.com [Physics R & D Centre, PES Institute of Technology, BSK 3rd Stage, Bangalore 560085 (India); Department of Physics, PES University, BSK 3rd Stage, Bangalore 560085 (India); Singh, Fouran [Inter University Accelerator Center, Aruna Asaf Ali Marg, New Delhi 110 067 (India)

    2016-07-15

    Zirconium oxide (ZrO{sub 2}) powder is synthesized by combustion technique. XRD pattern of ZrO{sub 2} shows monoclinic phase with average crystallite size 35 nm. Pellets of ZrO{sub 2} are irradiated with 100 MeV swift Si{sup 7+}, Ni{sup 7+} and 120 MeV swift Ag{sup 9+} ions in the fluence range 3 × 10{sup 10}–3 × 10{sup 13} ions cm{sup −2}. XRD pattern show the main diffraction peak correspond to monoclinic and tetragonal phase of ZrO{sub 2} in 2θ range 27–33°. Structural phase transformation is observed for Ni{sup 7+} and Ag{sup 9+} ion irradiated samples at a fluence 1 × 10{sup 13} ions cm{sup −2} and 3 × 10{sup 12} ions cm{sup −2} respectively, since the deposited electronic energy loss exceeds an effective threshold (>12 keV nm{sup −1}). Phase transition induced by Ag{sup 9+} ion is nearly 2.9 times faster than Ni{sup 7+} ion at 1 × 10{sup 13} ions cm{sup −2}. Ag{sup 9+} ion irradiation leads two ion impact processes. Thermoluminescence (TL) glow curves exhibit two glows, a well resolved peak at ∼424 K and unresolved peak at 550 K for all SHI irradiated samples. TL response is decreased with increase of ion fluence. Beyond 3 × 10{sup 12} ions cm{sup −2}, samples don’t exhibit TL due to annihilation of defects.

  10. Extensive Bone Reaction From Catastrophic Oxidized Zirconium Wear.

    Science.gov (United States)

    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.

  11. Zirconium metal-water oxidation kinetics. I. Thermometry

    International Nuclear Information System (INIS)

    Cathcart, J.V.; McElroy, D.L.; Pawel, R.E.; Perkins, R.A.; Williams, R.K.; Yurek, G.J.

    1976-02-01

    A description is given of the thermometry techniques used in the Zirconium Metal--Water Oxidation Kinetics Program. Temperature measurements in the range 900 to 1500 0 C are made in three experimental systems: two oxidation apparatuses and the annealing furnace used in a corollary study of the diffusion of oxygen in β-Zircaloy. Carefully calibrated Pt vs Pt--10 percent Rh thermocouples are employed in all three apparatuses, while a Pt--6 percent Rh vs Pt-- 30 percent Rh thermocouple and an optical pyrometer are used in addition in the annealing furnace. Features of the experimental systems pertaining to thermocouple installation, temperature control, emf measurements, etc. are described, and potential temperature-measurement error sources are discussed in detail. The accuracy of the temperature measurements is analyzed

  12. Oxidized zirconium: a potentially longer lasting hip implant

    International Nuclear Information System (INIS)

    Good, V.; Widding, K.; Hunter, G.; Heuer, D.

    2005-01-01

    Because younger, more active patients are receiving total hip replacements, it is necessary to develop materials, which would increase the life span of the implants and challenge their wear potential under adverse conditions. Oxidized zirconium (OxZr) is a metal with the surface transformed to ceramic by oxidation that offers low fracture risk and excellent abrasion resistance. This study compared wear of polyethylene (non-irradiated and highly crosslinked) with OxZr and CoCr heads under smooth and rough (clinically relevant) conditions. Wear was up to 15-fold less and up to 4-fold fewer particles were produced when coupled with OxZr than with CoCr, demonstrating that OxZr heads should increase clinical implant longevity

  13. Variation on wettability of anodic zirconium oxide nanotube surface

    International Nuclear Information System (INIS)

    Wang, Lu-Ning; Shen, Chen; Shinbine, Alyssa; Luo, Jing-Li

    2013-01-01

    The present study reports the effect of fabrication conditions and environmental conditions, such as anodization voltage and aging period, on the wetting of zirconium dioxide nanotube (ZrNT) surfaces. Comparing with intact zirconium foil, which was inherently less hydrophilic, possessing an approximate contact angle of 60–70°, the as-formed ZrNT surfaces were much hydrophilic with an approximate contact angle of 18°. However, the hydrophilicity of the surfaces exhibited a decrease when the nanotubular opening diameters decreased while maintaining the nanotubular layer thickness. This phenomenon was attributed to the balance of capillary force and force generated by compressed air in the ZrNTs. The annealing treatment further increased the hydrophilic property of the ZrNTs. In addition, it was found that the wettability of ZrNTs, when aged in air over a period of 105 days, demonstrated a decrease in hydrophilic characteristics and exhibited, to some extent, an increase in hydrophobic characteristics. It was believed that the surface wettability was able to be changed due to the decreasing content of hydroxyl groups in ambient atmosphere. This work can provide guidelines for improving the structural and environmental conditions responsible for changing surface wettability of ZrNT surfaces for biomedical application. - Highlights: ► Wettability of zirconium oxide nanotubes (ZrNTs) was observed and characterized. ► Increasing of nanotubular diameter decreased the hydrophilicity of ZrNTs. ► Annealing processes enhanced the hydrophilicity of ZrNTs. ► Long term aging resulted in the hydrophobicity of ZrNTs

  14. Synthesis of amorphous zirconium oxide with luminescent characteristics

    International Nuclear Information System (INIS)

    Barrera S, M.; Chavez G, M.; Soto E, A.M.; Velasquez O, C.; Garcia S, M.A.; Olvera T, L.; Rivera M, T.

    2004-01-01

    It was prepared zirconium oxide, ZrO 2 , by means of hydrolysis-condensation reactions (sol-gel method), using zirconium propoxide, Zr(C 3 H 7 O) 4 , as precursor and nitric acid, HNO 3 , as catalyst of the hydrolysis reaction. In this synthesis it was used a molar ratio water-alkoxide, r=n H2O /n Zr (C 3 H 7 0) 4 , high, similar to 200, so that the hydrolysis happens quickly and the nucleation and growth are completed in very little time. The solid was characterized with Ftir spectrophotometry, Differential thermal analysis (Dta), Thermal gravimetric analysis (T G), X-ray diffraction of powders, Scanning electron microscopy (Sem) and X-ray Dispersion energy (EDX). The ZrO 2 obtained by this way is amorphous even to 300 C and it consists of big aggregates. The amorphous ZrO 2 , presents thermoluminescent behavior, after it was irradiated with UV radiation and beta particles of 90 Sr/ 90 Y and it was thermally stimulated. (Author)

  15. Experimental investigation and thermodynamic simulation of the uranium oxide-zirconium oxide-iron oxide system in air

    Czech Academy of Sciences Publication Activity Database

    Petrov, Y. B.; Udalov, Y. P.; Šubrt, Jan; Bakardjieva, Snejana; Sázavský, P.; Kiselová, M.; Selucký, P.; Bezdička, Petr; Joumeau, C.; Piluso, P.

    2011-01-01

    Roč. 37, č. 2 (2011), s. 212-229 ISSN 1087-6596 Institutional research plan: CEZ:AV0Z40320502 Keywords : uranium oxide * zirconium oxide * iron oxide * fusibility curve * oxygen partial pressure * crystallization * phase composition Subject RIV: CA - Inorganic Chemistry Impact factor: 0.492, year: 2011

  16. Ligand exchange chromatography of free amino acids and proteins on porous microparticulate zirconium oxide

    International Nuclear Information System (INIS)

    Blackwell, J.A.; Carr, P.W.

    1992-01-01

    The Lewis acid sites present on the underlying zirconium oxide particles are responsible for the unusual elution sequence for amino acids on copper loaded, phosphated zirconium oxide supports reported in an earlier study. To more thoroughly examine the effect of these strong Lewis acid sites in this paper. The authors have studied ligand exchange chromatography on copper loaded zirconium oxide particles. It is shown here that carboxylate functional groups on amino acid solutes strongly interact with surface Lewis acid sites. Addition of competing hard Lewis bases to the eluent attenuates these specific interactions. The result is a chromatographic system with high selectivity which is also suitable for ligand exchange chromatography of proteins

  17. Hydrogenation and high temperature oxidation of Zirconium claddings

    International Nuclear Information System (INIS)

    Novotny, T.; Perez-Feró, E.; Horváth, M.

    2015-01-01

    In the last few years a new series of experiments started for supporting the new LOCA criteria, considering the proposals of US NRC. The effects which can cause the embrittlement of VVER fuel claddings were reviewed and evaluated in the framework of the project. The purpose of the work was to determine how the fuel cladding’s hydrogen uptake under normal operating conditions, effect the behavior of the cladding under LOCA conditions. As a first step a gas system equipment with gas valves and pressure gauge was built, in which the zirconium alloy can absorb hydrogen under controlled conditions. In this apparatus E110 (produced by electrolytic method, currently used at Paks NPP) and E110G (produced by a new technology) alloys were hydrogenated to predetermined hydrogen contents. According the results of ring compression tests the E110G alloys lose their ductility above 3200 ppm hydrogen content. This limit can be applied to determine the ductile-brittle transition of the nuclear fuel claddings. After the hydrogenation, high temperature oxidation experiments were carried out on the E110G and E110 samples at 1000 °C and 1200 °C. 16 pieces of E110G and 8 samples of E110 with 300 ppm and 600 ppm hydrogen content were tested. The oxidation of the specimens was performed in steam, under isothermal conditions. Based on the ring compression tests load-displacement curves were recorded. The main objective of the compression tests was to determine the ductile-brittle transition. These results were compared to the results of our previous experiments where the samples did not contain hydrogen. The original claddings showed more ductile behavior than the samples with hydrogen content. The higher hydrogen content resulted in a more brittle mechanical behavior. However no significant difference was observed in the oxidation kinetics of the same cladding types with different hydrogen content. The experiments showed that the normal operating hydrogen uptake of the fuel claddings

  18. Sulphur mustard degradation on zirconium doped Ti-Fe oxides

    Energy Technology Data Exchange (ETDEWEB)

    Stengl, Vaclav, E-mail: stengl@iic.cas.cz [Department of Solid State Chemistry, Institute of Inorganic Chemistry AS CR v.v.i 250 68 Husinec-Rez (Czech Republic); Grygar, Tomas Matys [Department of Solid State Chemistry, Institute of Inorganic Chemistry AS CR v.v.i 250 68 Husinec-Rez (Czech Republic); Oplustil, Frantisek; Nemec, Tomas [Military Technical Institute of Protection Brno Veslarska 230, 628 00 Brno (Czech Republic)

    2011-09-15

    Highlights: {yields} New stechiometric materials for sulphur mustard degradation. {yields} High degree of degradation, more then 95% h{sup -1}. {yields} One-pot synthesis procedure. - Abstract: Zirconium doped mixed nanodispersive oxides of Ti and Fe were prepared by homogeneous hydrolysis of sulphate salts with urea in aqueous solutions. Synthesized nanodispersive metal oxide hydroxides were characterised as the Brunauer-Emmett-Teller (BET) surface area and Barrett-Joiner-Halenda porosity (BJH), X-ray diffraction (XRD), infrared (IR) spectroscopy, scanning electron microscopy (SEM) with energy-dispersive X-ray (EDX) microanalysis, and acid-base titration. These oxides were taken for an experimental evaluation of their reactivity with sulphur mustard (chemical warfare agent HD or bis(2-chloroethyl)sulphide). The presence of Zr{sup 4+} dopant tends to increase both the surface area and the surface hydroxylation of the resulting doped oxides in such a manner that it can contribute to enabling the substrate adsorption at the oxide surface and thus accelerate the rate of degradation of warfare agents. The addition of Zr{sup 4+} to the hydrolysis of ferric sulphate with urea shifts the reaction route and promotes formation of goethite at the expense of ferrihydrite. We discovered that Zr{sup 4+} doped oxo-hydroxides of Ti and Fe exhibit a higher degradation activity towards sulphur mustard than any other yet reported reactive sorbents. The reaction rate constant of the slower parallel reaction of the most efficient reactive sorbents is increased with the increasing amount of surface base sites.

  19. The impact of zirconium oxide radiopacifier on the early hydration behaviour of white Portland cement.

    Science.gov (United States)

    Coleman, Nichola J; Li, Qiu

    2013-01-01

    Zirconium oxide has been identified as a candidate radiopacifying agent for use in Portland cement-based biomaterials. During this study, the impact of 20 wt.% zirconium oxide on the hydration and setting reactions of white Portland cement (WPC) was monitored by powder X-ray diffraction (XRD), (29)Si and (27)Al magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR), transmission electron microscopy (TEM) and Vicat apparatus. The presence of 20 wt.% zirconium oxide particles in the size-range of 0.2 to 5 μm was found to reduce the initial and final setting times of WPC from 172 to 147 min and 213 to 191 min, respectively. Zirconium oxide did not formally participate in the chemical reactions of the hydrating cement; however, the surface of the zirconium oxide particles presented heterogeneous nucleation sites for the precipitation and growth of the early C-S-H gel products which accelerated the initial setting reactions. The presence of zirconium oxide was found to have little impact on the development of the calcium (sulpho)aluminate hydrate phases. Copyright © 2012 Elsevier B.V. All rights reserved.

  20. Role of temperature and energy density in the pulsed laser deposition of zirconium oxide thin film

    International Nuclear Information System (INIS)

    Mittra, Joy; Abraham, G.J.; Viswanadham, C.S.; Kulkarni, U.D.; Dey, G.K.

    2011-01-01

    Present work brings out the effects of energy density and substrate temperature on pulsed laser deposition of zirconium oxide thin film on Zr-base alloy substrates. The ablation of sintered zirconia has been carried out using a KrF excimer laser having 30 ns pulse width and 600 mJ energy at source at 10 Hz repetition rate. To comprehend effects of these parameters on the synthesized thin film, pure zirconia substrate has been ablated at two different energy densities, 2 J.cm -2 and 5 J.cm -2 , keeping the substrate at 300 K, 573 K and 873 K, respectively. After visual observation, deposited thin films have been examined using Raman Spectroscopy (RS) and X-ray Photo-electron Spectroscopy (XPS). It has been found that the oxide deposited at 300 K temperature does not show good adherence with the substrate and deteriorates further with the reduction in energy density of the incident laser. The oxide films, deposited at 573 K and 873 K, have been found to be adherent with the substrate and appear lustrous black. These indicate that the threshold for adherence of the zirconia film on the Zr-base alloy substrate lies in between 300 K and 573 K. Analysis of Raman spectra has indicated that thin films of zirconia, deposited using pulsed laser, on the Zr-base metallic substrate are initially in amorphous state. Experimental evidence has indicated a strong link among the degree of crystallinity of the deposited oxide film, the substrate temperature and the energy density. It also has shown that the crystallization of the oxide film is dependent on the substrate temperature and the duration of holding at high temperature. The O:Zr ratios of the films, analyzed from the XPS data, have been found to be close to but less than 2. This appears to explain the reason for the transformation of amorphous oxide into monoclinic and tetragonal phases, below 573 K, and not into cubic phase, which is reported to be more oxygen deficient. (author)

  1. Preparation and Characterization of Hydrous Zirconium Oxide Formed by Homogeneous Precipitation

    Directory of Open Access Journals (Sweden)

    Silva G.L.J.P. da

    2002-01-01

    Full Text Available This paper reports on the preparation, characterization and study of the ion exchange behavior of hydrous zirconium oxides formed by homogeneous precipitation from zirconium oxychloride. The precipitants used were obtained by thermal decomposition of urea, sodium nitrite or ammonium carbonate. Seven compounds were prepared and characterized by thermal analysis, X-ray diffractometry and by surface area measurements. Amorphous forms were obtained in each case, a result that agrees with those obtained by conventional gel precipitation methodology. All these materials present surface area values of >148 m².g-1, determined after heat treatment at 50 °C. The ion exchange behavior of each hydrous zirconium oxide prepared was studied using K+ as the exchanged species and the results compared with those obtained for hydrous zirconium oxide originally precipitated by the sol gel method.

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

    Energy Technology Data Exchange (ETDEWEB)

    Fidan, S.; Muhaffel, F. [Department of Metallurgical and Materials Engineering, Istanbul Technical University, Sariyer, 34469 Istanbul (Turkey); Riool, M. [Department of Medical Microbiology, Center for Infection and Immunity Amsterdam (CINIMA), Academic Medical Center, University of Amsterdam, Meibergdreef 15, 1105, AZ, Amsterdam (Netherlands); Cempura, G. [International Centre of Electron Microscopy for Materials Science, AGH University of Science and Technology, PL, 30-059 Kraków (Poland); Boer, L. de; Zaat, S.A.J. [Department of Medical Microbiology, Center for Infection and Immunity Amsterdam (CINIMA), Academic Medical Center, University of Amsterdam, Meibergdreef 15, 1105, AZ, Amsterdam (Netherlands); Filemonowicz, A. Czyrska - [International Centre of Electron Microscopy for Materials Science, AGH University of Science and Technology, PL, 30-059 Kraków (Poland); Cimenoglu, H., E-mail: cimenogluh@itu.edu.tr [Department of Metallurgical and Materials Engineering, Istanbul Technical University, Sariyer, 34469 Istanbul (Turkey)

    2017-02-01

    The aim of this study was to cover the surfaces of zirconium (Zr) with an antimicrobial layer for biomedical applications. For this purpose, the micro-arc oxidation (MAO) process was employed in a sodium silicate and sodium hydroxide containing base electrolyte with and without addition of silver acetate (AgC{sub 2}H{sub 3}O{sub 2}). In general, synthesized MAO layers were composed of zirconium oxide (ZrO{sub 2}) and zircon (ZrSiO{sub 4}). Addition of AgC{sub 2}H{sub 3}O{sub 2} into the base electrolyte caused homogenous precipitation of silver-containing particles in the MAO layer, which exhibited excellent antibacterial efficiency against methicillin-resistant Staphylococcus aureus (MRSA) as compared to the untreated and MAO-treated Zr. - Highlights: • Micro-arc oxidation process was applied on zirconium in an electrolyte containing silver acetate. • Silver incorporated in the oxide layer in the form of nanoparticles. • 0.45 wt.% silver incorporation provided excellent antibacterial activity.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

    The aim of this study was to cover the surfaces of zirconium (Zr) with an antimicrobial layer for biomedical applications. For this purpose, the micro-arc oxidation (MAO) process was employed in a sodium silicate and sodium hydroxide containing base electrolyte with and without addition of silver acetate (AgC 2 H 3 O 2 ). In general, synthesized MAO layers were composed of zirconium oxide (ZrO 2 ) and zircon (ZrSiO 4 ). Addition of AgC 2 H 3 O 2 into the base electrolyte caused homogenous precipitation of silver-containing particles in the MAO layer, which exhibited excellent antibacterial efficiency against methicillin-resistant Staphylococcus aureus (MRSA) as compared to the untreated and MAO-treated Zr. - Highlights: • Micro-arc oxidation process was applied on zirconium in an electrolyte containing silver acetate. • Silver incorporated in the oxide layer in the form of nanoparticles. • 0.45 wt.% silver incorporation provided excellent antibacterial activity.

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

    Science.gov (United States)

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

    2017-02-01

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

  5. Zirconium oxide based ceramic solid electrolytes for oxygen detection

    International Nuclear Information System (INIS)

    Caproni, Erica

    2007-01-01

    Taking advantage of the high thermal shock resistance of zirconia-magnesia ceramics and the high oxide ion conductivity of zirconia-yttria ceramics, composites of these ceramics were prepared by mixing, pressing and sintering different relative concentrations of ZrO 2 : 8.6 mol% MgO and ZrO 2 : 3 mol% Y 2 O 3 solid electrolytes. Microstructural analysis of the composites was carried out by X-ray diffraction and scanning electron microscopy analyses. The thermal behavior was studied by dilatometric analysis. The electrical behavior was evaluated by the impedance spectroscopy technique. An experimental setup was designed for measurement the electrical signal generated as a function of the amount of oxygen at high temperatures. The main results show that these composites are partially stabilized (monoclinic, cubic and tetragonal) and the thermal behavior is similar to that of ZrO 2 : 8.6 mol% MgO materials used in disposable high temperature oxygen sensors. Moreover, the results of analysis of impedance spectroscopy show that the electrical conductivity of zirconia:magnesia is improved with zirconia-yttria addition and that the electrical signal depends on the amount of oxygen at 1000 deg C, showing that the ceramic composites can be used in oxygen sensors. (author)

  6. Oxidation kinetics and auger microprobe analysis of some oxidized zirconium alloys

    International Nuclear Information System (INIS)

    Ploc, R.A.

    1989-01-01

    Oxidation kinetics at 300 o C in dry oxygen of 0.5 wt% binary alloys of iron, nickel, and chromium in zirconium were determined for several surface preparations. Further, chemical profiles of the oxides as they existed on the matrix and on the precipitates were obtained by sputtering and Auger electron analysis. The appearance of 'breakaway' oxidation was controlled by the surface finish of the alloy, a variable that could be used to eliminate the phenomenon for all alloys except the Zr/Ni binary, which required β-quenching to accomplish the same purpose. (author)

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

    Energy Technology Data Exchange (ETDEWEB)

    Aktuğ, Salim Levent, E-mail: saktug@gtu.edu.tr [The Department of Materials Science and Engineering, Gebze Technical University, Gebze, Kocaeli 41400 (Turkey); Durdu, Salih, E-mail: durdusalih@gmail.com [The Department of Industrial Engineering, Giresun University, Merkez, Giresun 28200 (Turkey); Yalçın, Emine, E-mail: emine.yalcin@giresun.edu.tr [The Department of Biology, Giresun University, Merkez, Giresun 28200 (Turkey); Çavuşoğlu, Kültigin, E-mail: kultigin.cavusoglu@giresun.edu.tr [The Department of Biology, Giresun University, Merkez, Giresun 28200 (Turkey); Usta, Metin, E-mail: ustam@gtu.edu.tr [The Department of Materials Science and Engineering, Gebze Technical University, Gebze, Kocaeli 41400 (Turkey); Materials Institute, Marmara Research Center, TUBITAK, Gebze, Kocaeli 41470 (Turkey)

    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 28 days. 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 0.370 A/cm{sup 2} was minimum compared to uncoated zirconium coated at 0.260 and 0.292 A/cm{sup 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. - Highlights: • Hydroxyapatite was formed on zirconium at different current densities by single-step plasma electrolytic oxidation. • The amount of hydroxyapatite and calcium-based phases increased with

  8. Fabrication of NiO/zirconium oxide nanofibers by electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Sundarrajan, Subramanian, E-mail: sundarnus1@gmail.com [Department of Mechanical Engineering, NUS, 117576 (Singapore); Venkatesan, Arunachalam; Agarwal, Satya R.; Shaik Anwar Ahamed, Nabeela Nasreen [Department of Mechanical Engineering, NUS, 117576 (Singapore); Ramakrishna, Seeram, E-mail: seeram@nus.edu.sg [Department of Mechanical Engineering, NUS, 117576 (Singapore); King Saud University, Riyadh 11451 (Saudi Arabia); Institute of Materials Research and Engineering, 117602 (Singapore)

    2014-12-01

    The electrospinning technique has been used to fabricate 1D inorganic–organic composite nanofibers from solutions containing poly(vinyl alcohol) (PVA) and suitable aqueous precursors of nickel and zirconium ions. Upon calcination, nickel oxide/zirconia nanofibers retained the original morphological features of as-spun nanofibers. X-ray diffraction was used to identify the crystalline nature of the final product and analytical tools such as Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and atomic force microscopy (AFM) were employed to elucidate the pathway of ceramic phase formation and the systematic evolution of morphological features in the as-spun and calcined fibers. These fibers will find potential applications in biomedical field. - Highlights: • PVA/NiO/zirconia composite nanofibers were synthesized via electrospinning. • Green processing of nanofibers using only water as solvent. • Calcination of composite nanofibers to yield ceramic nanofibers. • High aspect ratio nanofibers with diameters 106 ± 25 nm • The application of these fibers as dental composites and bone tissue engineering.

  9. Analysis of zirconium and nickel based alloys and zirconium oxides by relative and internal monostandard neutron activation analysis methods

    International Nuclear Information System (INIS)

    Shinde, Amol D.; Acharya, Raghunath; Reddy, Annareddy V. R.

    2017-01-01

    The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples

  10. Analysis of zirconium and nickel based alloys and zirconium oxides by relative and internal monostandard neutron activation analysis methods

    Energy Technology Data Exchange (ETDEWEB)

    Shinde, Amol D.; Acharya, Raghunath; Reddy, Annareddy V. R. [Bhabha Atomic Research Centre, Mumbai (India)

    2017-04-15

    The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

  11. Calcium Oxide Supported on Monoclinic Zirconia as a Highly Active Solid Base Catalyst

    NARCIS (Netherlands)

    Frey, A.M.; Haasterecht, van T.; Jong, de K.P.; Bitter, J.H.

    2013-01-01

    Calcium oxide supported on ZrO2 is a highly active catalyst for base-catalyzed reactions such as aldol-type reactions and transesterification reactions. The role of key parameters during preparation, that is, impregnation versus precipitation, heat treatment, and metal oxide loading on the basicity

  12. Study of the production of Zirconium tetracheoride by chlorination of its oxide

    International Nuclear Information System (INIS)

    Seo, E.S.M.; Abrao, A.

    1987-08-01

    This work describes the studies carried out on the production of zirconium tetrachloride by chlorianation of pure zirconium oxide with (a) carbon tetrachloride and (b) chlorine in the presence of carbon. In the process of chlorination with carbon tetrachloride it has been determined that efficiency increases with the rising of temperature between 450 and 750 0 C. The flow rate of the carbon tetrachloride vapour used was 1.50L/min. For the zirconium oxide chlorination in the presence of carbon, the study has been carried out at temperatures between 700 and 850 0 C and the flow rate of the chlorine gas used in the process was 0,50/Lmin. Pure zirconium oxide chlorination as well as zirconium oxide-carbon mixture chlrorination have been studied in connection with the time of reaction at different temperatures and the apparent rate constants, the activation energies, the order of reaction in relation to the concentration of the gases (CCl 4 and Cl 2 ) and the content of carbon in the pellet have all been determined. (Author) [pt

  13. Study of the production of zirconium tetrachloride by chlorination of its oxide

    International Nuclear Information System (INIS)

    Seo, E.S.M.

    1983-01-01

    The studies carried out on the production of zirconium tetrachloride by chlorination of pure zirconium oxide with carbon tetrachloride and chlorine in the presence of carbon. In the process of chlorination with carbon tetrachloride, the chlorination efficiency increases with the rise in temperature at intervals between 450 and 750 0 C. The flow of the carbon tetrachloride vapour was 1.50l/min. Higher temperatures of 700 to 850 0 C were used for the zirconium oxide chlorination in the presence of carbon, and the flowrate of the chlorine gas used in the process was 0.50 l/min. Pure zirconium oxide chlorination as well as zirconium oxide - carbon misture chlorination have been studied in connection with the time of reaction at different temperatures and the apparent rate constant, the activation energies, the order of reaction in relation to the concentration of the gases (CCl 4 and Cl 2 ) and the content of carbon in the pellet have all been determined. (Author) [pt

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

    Science.gov (United States)

    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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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. The 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

  16. Separation of sup(99m)Tc from 99Mo through a hydrous zirconium oxide column

    International Nuclear Information System (INIS)

    Mengatti, J.

    1980-01-01

    The preparation of 99 Mo-,sup(99m)Tc generator based on the adsorption of 99 Mo on hydrous zirconium oxide column, employing the in exchange technique, is described. The adsorption of 99 Mo on hydrous zirconium oxide (HZO) and the separation of sup(99m)Tc, generated by the decay of 99 Mo with saline solution, are analised. The sup(99m)Tc separation yield, pH of the eluted solution, aspect of the elution curve and the adsorption of 99 Mo on hydrous zirconium oxide calcined at 800 0 C are studied. The chemical and radioactive purities of the final product are analysed and the variation of the elution yield for successive elutions is studied. (Author) [pt

  17. The impact of zirconium oxide radiopacifier on the early hydration behaviour of white Portland cement

    International Nuclear Information System (INIS)

    Coleman, Nichola J.; Li, Qiu

    2013-01-01

    Zirconium oxide has been identified as a candidate radiopacifying agent for use in Portland cement-based biomaterials. During this study, the impact of 20 wt.% zirconium oxide on the hydration and setting reactions of white Portland cement (WPC) was monitored by powder X-ray diffraction (XRD), 29 Si and 27 Al magic angle spinning nuclear magnetic resonance spectroscopy (MAS NMR), transmission electron microscopy (TEM) and Vicat apparatus. The presence of 20 wt.% zirconium oxide particles in the size-range of 0.2 to 5 μm was found to reduce the initial and final setting times of WPC from 172 to 147 min and 213 to 191 min, respectively. Zirconium oxide did not formally participate in the chemical reactions of the hydrating cement; however, the surface of the zirconium oxide particles presented heterogeneous nucleation sites for the precipitation and growth of the early C-S-H gel products which accelerated the initial setting reactions. The presence of zirconium oxide was found to have little impact on the development of the calcium (sulpho)aluminate hydrate phases. - Highlights: ► This is the first study of Portland cement-based biomaterials by 27 Al and 29 Si NMR. ► 20 wt.% ZrO 2 radiopacifier accelerates the early cement hydration reactions. ► Extent of hydration after 6 h is increased from 5.7% to 15% in the presence of ZrO 2 . ► Initial and final setting times are reduced by 25 and 22 min, respectively. ► ZrO 2 provides nucleation sites for the precipitation of early hydration products.

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

    Science.gov (United States)

    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.

  19. The air oxidation behavior of lanthanum ion implanted zirconium at 500 deg. C

    CERN Document Server

    Peng, D Q; Chen, X W; Zhou, Q G

    2003-01-01

    The beneficial effect of lanthanum ion implantation on the oxidation behavior of zirconium at 500 deg. C has been studied. Zirconium specimens were implanted by lanthanum ions using a MEVVA source at energy of 40 keV with a fluence range from 1x10 sup 1 sup 6 to 1x10 sup 1 sup 7 ions/cm sup 2 at maximum temperature of 130 deg. C, The weight gain curves were measured after being oxidized in air at 500 deg. C for 100 min, which showed that a significant improvement was achieved in the oxidation behavior of zirconium ion implanted with lanthanum compared with that of the as-received zirconium. The valence of the oxides in the scale was analyzed by X-ray photoemission spectroscopy; and then the depth distributions of the elements in the surface of the samples were obtained by Auger electron spectroscopy. Glancing angle X-ray diffraction at 0.3 deg. incident angles was employed to examine the modification of its phase transformation because of the lanthanum ion implantation in the oxide films. It was obviously fou...

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

    Science.gov (United States)

    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 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

  1. Effect of carbon on the oxidation of zirconium; Influence du carbone sur l'oxygenation du zirconium a haute temperature

    Energy Technology Data Exchange (ETDEWEB)

    Chauvin, G; Boudouresques, B; Coriou, H; Hure, J [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1959-07-01

    The study of specimens contaminated by different amounts of carbon shows a deleterious effect of this element in the resistance of zirconium to high temperature oxidation (700 to 900 deg. C). We drew the following results: a) the white spots or 'pimples' observed by numerous authors seem to be caused by the oxidation of precipitated carbides. We suggest a mechanism of formation and growth of these pimples; b) for a certain carbon content, the resistance to oxidation is increased by an uniform dispersion of the carbide phase and decreased, for instance, by extrusion textures. In this case, for the more marked textures, the more oriented corrosion was observed; c) by burning of the carbide phase it can result a second reaction increasing the corrosion rate; d) thin zirconium foils undergoes dimensional changes when scaling in oxygen. This unusual feature is also subordinated to carbon content and specially to the carbide phase dispersion. (author) [French] L'etude d'echantillons differemment contamines par le carbone nous a permis de mettre en evidence l'action particulierement nocive de cet element sur la resistance du zirconium a la corrosion par l'oxygene a haute temperature (700 a 900 deg. C). Nous avons pu degager les resultats essentiels suivants: a) l'origine des pustules d'oxyde blanc signalees par de nombreux auteurs doit etre recherchee dans l'oxydation des carbures precipites. Nous suggerons un mecanisme de formation et de croissance de ces pustules, b) la tenue du metal est d'autant meilleure que, pour une meme teneur en carbone, la phase 'carbure' est plus uniformement dispersee. En consequence, si la dispersion est mauvaise, on observe selon l'axe des textures de filage, par exemple, une corrosion preferentielle d'autant plus accentuee que les textures sont plus marquees, c) la combustion de la phase 'carbure' peut engendrer une reaction secondaire susceptible d'accroitre la cinetique de corrosion, d) l'expansion des grandes faces d

  2. Change in the work function of zirconium by oxidation at high temperatures and low oxygen pressures

    International Nuclear Information System (INIS)

    Maeno, Yutaka; Yamamoto, Masahiro; Naito, Shizuo; Mabuchi, Mahito; Hashino, Tomoyasu

    1991-01-01

    Changes in the work function of zirconium on oxidation are measured at oxygen pressures of 3.0 x 10 -6 - 3.0 x 10 -4 Pa and at temperatures in the range 426-775 K. The work function first decreases then increases until a final saturation stage is reached. Use of secondary-ion mass spectroscopy (SIMS) shows that the changes correspond to oxygen adsorption, oxide nucleation and oxide growth, respectively. The initial decrease in work function is interpreted by the incorporation of oxygen adatoms into the subsurface. The oxygen adsorption potential of zirconium is evaluated by an effective medium theory, and the physical origin of the incorporation of oxygen adatoms is discussed. The positive change in the work function caused by oxide formation and the temperature and pressure dependences of the change in the work function by oxidation are explained qualitatively. (author)

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

    Science.gov (United States)

    2013-12-01

    and compliance issues associated with the use of zinc phosphate and chromate/ chrome containing conversion coatings while maintaining military...safety, and occupational health risks associated with the use of zinc phosphate and chromate/ chrome -containing conversion coatings. There is a need to...zirconium-based pretreatment will be shown to be both environmentally acceptable (no hazardous air pollutants or heavy metals such as hexavalent chromium

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

    Science.gov (United States)

    Al-Thobity, Ahmad M

    2016-06-01

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

  5. Long-time corrosion and high-temperature oxidation of zirconium alloys applied on NPP like fuel elements cover

    International Nuclear Information System (INIS)

    Vrtilkova, V.; Novotny, L.; Lingart, S.; Doukha, R.; Yarosh, Ya.; Kolenchik, Ya.

    2007-01-01

    Zirconium is applying in nuclear energy since 50-th of last century in capacity of material for cover production for fuel elements, reactor fuel and structural parts, and mainly due to both corrosion stability and low effective cross section for thermal neutrons capture. Impurities in doping elements form and alloy production technology has influence on mechanical and corrosion properties of finite alloy. Long-time corrosion tests for several zirconium alloys in forcing autoclave under different reaction conditions were carried out. After that process kinetics was studied, mass increase, hydrogen formation, zirconium hydride forming morphology, zirconium oxide layer thickness have been determined as well

  6. The oxidation kinetics of zirconium alloys applicable to loss-of-coolant accidents

    International Nuclear Information System (INIS)

    Parsons, P.D.; Miller, W.N.

    1977-10-01

    A review is presented of the available published measurements of the rate of reaction between zirconium alloys and steam and, in some cases, oxygen. Attempts are made to define from all the experimental data a suitable rate equation which is appropriate over the range of temperatures relevant to LOCA conditions. The data reviewed encompass a temperature range 910 0 C to the melting point of zirconium, 1852 0 C. It can be concluded that within 910 to 1577 0 C, Zircaloy-2, Zircaloy-4 and Zr/2 1/2%Nb alloys have the same response to oxidation. (author)

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

    Science.gov (United States)

    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

  8. Fabrication and formation of bioactive anodic zirconium oxide nanotubes containing presynthesized hydroxyapatite via alternative immersion method

    International Nuclear Information System (INIS)

    Wang Luning; Luo Jingli

    2011-01-01

    Hydroxyapatite (HA) coating has been widely applied on metallic biomedical implants to enhance their biocompatibility. It has been reported that HA coating can be formed on annealed zirconium with anodic zirconium oxide nanotubular arrays after immersion in simulated biological fluid (SBF) for about 14 days. In the present study, we apply an alternative immersion method (AIM) to form presynthesized HA on ZrO 2 nanotubes. The AIM-treated specimen was then moved to the SBF to evaluate the capability for the formation of HA on it. The HA coating formed after only 2 days immersion and thickened after 5 days in the SBF. The HA coating is the carbonated HA with a ratio of Ca to P of about 1.4, similar to the physiological HA containing other minor elements such as Mg and Na. The results demonstrate that the AIM treatment is indeed suitable for the zirconium oxide nanotubes and highly accelerates the formation of HA coating in comparison with the existing methods, i.e. the annealing of the as-formed zirconium oxide nanotubular arrays.

  9. Preparation and characterization of sugar cane bagasse fiber modified with nanoparticles of zirconium oxide

    International Nuclear Information System (INIS)

    Carvalho, K.C.C. de; Mulinari, D.R.; Voorwald, H.C.J.; Cioffi, M.O.H.

    2010-01-01

    The sugar cane bagasse fiber are renewable materials and have great application potential when used as reinforcement in a polymer matrix to give rise to composite materials and as supports for adsorption of heavy metals. This paper therefore describes the preparation and characterization of bleached and hydrated zirconium oxide modified sugar cane bagasse fiber by conventional precipitation method. Through the technique of electron microscopy we observed the presence of oxide nanoparticles on the fiber surface, proving the efficiency of the conventional precipitation method. With the X-ray diffraction analysis it was determined a decrease of 6.2% in the crystallinity index of modified fibers when compared to the bleached fibers showing the deposition of amorphous zirconium oxide on the fiber surface. (author)

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

    International Nuclear Information System (INIS)

    Stengl, Vaclav; Houskova, Vendula; Bakardjieva, Snejana; Murafa, Nataliya; Marikova, Monika; Oplustil, Frantisek; Nemec, Tomas

    2010-01-01

    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 4+ dopant can increase both the surface area and the surface hydroxylation of the resulting 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 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.

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

    Energy Technology Data Exchange (ETDEWEB)

    Stengl, Vaclav, E-mail: stengl@uach.cz [Institute of Inorganic Chemistry AS CR v.v.i., 250 68 Rez (Czech Republic); Houskova, Vendula; Bakardjieva, Snejana; Murafa, Nataliya; Marikova, Monika [Institute of Inorganic Chemistry AS CR v.v.i., 250 68 Rez (Czech Republic); Oplustil, Frantisek; Nemec, Tomas [Military Technical Institute of Protection Brno, Veslarska 230, 628 00 Brno (Czech Republic)

    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 resulting 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.

  12. Methods of studying oxide scales grown on zirconium alloys in autoclaves and in a PWR

    International Nuclear Information System (INIS)

    Blank, H.; Bart, G.; Thiele, H.

    1992-01-01

    The analysis of water-side corrosion of zirconium alloys has been a field of research for more than 25 years, but the details of the mechanisms involved still cannot be put into a coherent picture. Improved methods are required to establish the details of the microstructure of the oxide scales. A new approach has been made for a general analysis of oxide specimens from scales grown on the zirconium-based cladding alloys of PWR rods in order to analyse the morphology of these scales, the topography of the oxide/metal interface and the crystal structures close to this interface: a) Instead of using the conventional pickling solutions, the Zr-alloys are dissolved using a 'softer' solution (Br 2 in an organic solvent) in order to avoid damage to the oxide at the oxide/metal interface to be analysed by SEM (scanning electron microscopy). A second advantage of this method is easy etching of the grain structure of Zr-alloys for SEM analysis; b) By using the particular properties of the oxide scales, the corrosion-rate-determining innermost part of the oxide layer at the oxide/metal interface can be separated from the rest of the oxide scale and then analysed by SEM, STEM (scanning transmission electron microscopy), TEM (transmission electron microscopy) and electron diffraction after dissolution of the alloy. Examples are given from oxides grown on Zr-alloys in a pressurized water reactor and in autoclaves. (author) 8 figs., 3 tabs., 9 refs

  13. Photoelectrochemical properties and band structure of oxide films on zirconium-transition metal alloys

    International Nuclear Information System (INIS)

    Takahashi, Kazuo; Uno, Masayoshi; Okui, Mihoko; Yamanaka, Shinsuke

    2006-01-01

    The microalloying effects of 4d and 5d transition metals, M (M: Nb, Mo, Ta, W) on the photoelectrochemical properties, the flat band potential (U fb ) and the band gap energy (E g ), for zirconium oxide films were investigated by photoelectrochemical measurements and band calculation. Button ingots of zirconium-5 mol% M (M: Nb, Mo, Ta, W) were made from high-purity metals (99.9% purity) by arc melting in a purified argon atmosphere. These plate specimens were sealed into silica tubes in vacuum, and then homogenized at 1273 K for 24 h. Subsequently, these specimens were oxidized up to 1173 K. The photocurrent of each specimen was evaluated at room temperature under the irradiation of Xe lamp (500 W) through grating monochrometer and cut-off filter. 0.1 M Na 2 SO 4 solution was used as the electrolyte. The value of the flat band potential was higher and the value of the band gap energy was smaller than that of pure zirconium oxide film in all sample. It was found from the calculation by CASTEP code that the decreases in band gap energy of these oxide films was due to formation of 4d or 5d orbital of transition metals

  14. Cation incorporation into zirconium oxide in LiOH, NaOH, and KOH solutions

    International Nuclear Information System (INIS)

    Jeong, Y.H.; Kim, K.H.; Baek, J.H.

    1999-01-01

    To investigate the cation incorporation into zirconium oxide, SIMS analysis was performed on the specimens prepared to have an equal oxide thickness in LiOH, NaOH, and KOH solutions. Even though they have an equal oxide thickness in LiOH, NaOH, and KOH solutions, the penetration depth of cation into the oxide decreased with an increase in the ionic radius of cation. The cation is considered to control the corrosion in alkali hydroxide solutions and its effect is dependent on the concentration of alkali and the oxide thickness. The slight enhancement of the corrosion rate at a low concentration is thought to be caused by cation incorporation into oxide, while the significant acceleration at a high concentration is due to the transformation of oxide microstructures that would be also induced by cation incorporation into oxide. (orig.)

  15. Synthesis of mesoporous cerium-zirconium mixed oxides by hydrothermal templating method

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

    Mesoporous cerium-zirconium mixed oxides were prepared by hydrothermal method using cetyl trimethyl ammonium bromide (CTAB) as template.The effects of amount of template,pH value of solution and hydrothermal temperature on mesostructure of samples were systematically investigated.The final products were characterized by XRD,TEM,FT-IR,and BET.The results indicate that all the cerium-zirconium mixed oxides present a meso-structure.At molar ratio of n(CTAB)/n((Ce)+(Zr))=0.15,pH value of 9,and hydrothermal temperature of 120 ℃,the samples obtained possess a specific surface area of 207.9 m2/g with pore diameter of 3.70 nm and pore volume of 0.19 cm3/g.

  16. Development of wear resistant zirconium oxide thin films on stainless steel substrates

    International Nuclear Information System (INIS)

    Then, I.K.; Mujahid, M.; Zhang, B.

    2005-01-01

    The present work deals specifically with the development of zirconium oxide thin film coatings on the stainless steel orthodontic bracket system by sputtering technique. Thin films of zirconium oxide have been deposited on injection molded stainless steel substrates using sputtering under controlled temperature and environment conditions. The deposited films, 1.5 μm in thickness, were found to have a predominantly tetragonal structure with grain size of about 5 nm. The grain size was found to increase only slightly with increasing heat treatment time at 650 C. It has been shown that thin-film zirconia coatings with stable structure and good adhesion along with very low friction coefficient could be produced. (orig.)

  17. Development of wear resistant zirconium oxide thin films on stainless steel substrates

    Energy Technology Data Exchange (ETDEWEB)

    Then, I.K.; Mujahid, M. [School of Materials Engineering, Nanyang Technological Univ. (Singapore); Zhang, B. [Dou Yee Technologies Pte Ltd, Bedok Industrial Park C (Singapore)

    2005-07-01

    The present work deals specifically with the development of zirconium oxide thin film coatings on the stainless steel orthodontic bracket system by sputtering technique. Thin films of zirconium oxide have been deposited on injection molded stainless steel substrates using sputtering under controlled temperature and environment conditions. The deposited films, 1.5 {mu}m in thickness, were found to have a predominantly tetragonal structure with grain size of about 5 nm. The grain size was found to increase only slightly with increasing heat treatment time at 650 C. It has been shown that thin-film zirconia coatings with stable structure and good adhesion along with very low friction coefficient could be produced. (orig.)

  18. Rheological and technological properties of zirconium suspensions stabilized with various amounts of calcium oxide

    International Nuclear Information System (INIS)

    Shulik, I.G.; Usatikov, I.F.; Alekseenko, A.S.

    1987-01-01

    A complex research of properties of zirconium dioxide-based suspensions with various amounts of calcium oxide up to calcium zirconate is carried out. Aqueous suspensions are used when preparing a complex form of ZrO 2 -based ceramics by the method of slip casting. Phase composition effect on the nature of rheologic curves ie found. The role of organic alcohol additions in the improvement of suspension flowability and reduction of casting porosity is noted

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

    Science.gov (United States)

    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 zirconium oxide restorations. © 2011 John Wiley & Sons A/S.

  20. Study of diffusion processes in the oxide layer of zirconium alloys

    Directory of Open Access Journals (Sweden)

    Sialini P.

    2016-03-01

    Full Text Available In the active zone of a nuclear reactor where zirconium alloys are used as a coating material, this material is subject to various harmful impacts. During water decomposition reactions, hydrogen and oxygen are evolved that may diffuse through the oxidic layer either through zirconium dioxide (ZrO2 crystals or along ZrO2 grains. The diffusion mechanism can be studied using the Ion Beam Analysis (IBA method where nuclear reaction 18O(p,α15N is used. A tube made of zirconium alloy E110 (with 1 wt. % of Nb was used for making samples that were pre-exposed in UJP PRAHA a.s. and subsequently exposed to isotopically cleansed environment of H2 18O medium in an autoclave. The samples were analysed with gravimetric methods and IBA methods performed at the electrostatic particle accelerator Tandetron 4130 MC in the Nucler Physics Institute of the CAS, Řež. With IBA methods, the overall thicknesses of corrosion layers on the samples, element composition of the alloy and distribution of oxygen isotope 18O in the corrosion layer and its penetration in the alloy were identified. The retrieved data shows at the oxygen diffusion along ZrO2 grains because there are two peaks of 18O isotope concentrations in the corrosion layer. These peaks occur at the environment-oxide and oxide-metal interface. The element analysis identified the presence of undesirable hafnium.

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

    Science.gov (United States)

    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 (pcement with 20% zirconium oxide as the radiopacifier showed low cytotoxicity as a promising material to be exploited for root-end filling.

  2. In-situ electrochemical impedance spectroscopy measurements of zirconium alloy oxide conductivity: Relationship to hydrogen pickup

    International Nuclear Information System (INIS)

    Couet, Adrien; Motta, Arthur T.; Ambard, Antoine; Livigni, Didier

    2017-01-01

    Highlights: • In-situ electrochemistry on zirconium alloys in 360 °C pure water show oxide layer resistivity changes during corrosion. • A linear relationship is observed between oxide resistivity and instantaneous hydrogen pickup fraction. • The resistivity of the oxide layer formed on Zircaloy-4 (and thus its hydrogen pickup fraction) is higher than on Zr-2.5Nb. - Abstract: Hydrogen pickup during nuclear fuel cladding corrosion is a critical life-limiting degradation mechanism for nuclear fuel. Following a program dedicated to zirconium alloys, corrosion, it has been hypothesized that oxide electronic resistivity determines hydrogen pickup. In-situ electrochemical impedance spectroscopy experiments were performed on Zircaloy-4 and Zr-2.5Nb alloys in 360 °C water. The oxide resistivity was measured as function of time. The results show that as the oxide resistivity increases so does the hydrogen pickup fraction. The resistivity of the oxide layer formed on Zircaloy-4 is higher than on Zr-2.5Nb, resulting in a higher hydrogen pickup fraction of Zircaloy-4, compared to Zr-2.5Nb.

  3. Formation and dissolution of the anodic oxide film on zirconium in alcoholic aqueous solutions

    International Nuclear Information System (INIS)

    Mogoda, A.S.

    1995-01-01

    The dissolution behavior of the anodic oxide film formed in alcoholic aqueous solutions was studied. Results indicated the dissolution mechanism of the duplex oxide film followed a zero-order rate equation. The increase in methanol concentration in the formation medium (phosphoric acid [H 3 PO 4 ]) resulted in formation of an oxide film that incorporated little phosphate ion and that dissolved at a low rate. The dissolution rate of the oxide film decreased with increasing methanol concentration in the dissolution medium. This was attributed to the increase in the viscosity of the medium, which led to a decrease in the diffusion coefficient of the dissolution product of the zirconium oxide film. Dissolution of the anodic oxide film also was investigated as a function of the chain length of alcohols

  4. Role of electrolyte composition on structural, morphological and in-vitro biological properties of plasma electrolytic oxidation films formed on zirconium

    International Nuclear Information System (INIS)

    M, Sandhyarani; T, Prasadrao; N, Rameshbabu

    2014-01-01

    Highlights: • Uniform oxide films were formed on zirconium by plasma electrolytic oxidation. • Silicate in electrolyte alter the growth of m-ZrO 2 from (1 ¯ 11) to (2 0 0) orientation. • Addition of KOH to electrolyte improved the corrosion resistance of oxide films. • Silicon incorporated oxide films showed higher surface roughness and wettability. • Human osteosarcoma cells were strongly adhered and spreaded on all the oxide films. - Abstract: Development of oxide films on metallic implants with a good combination of corrosion resistance, bioactivity and cell adhesion can greatly improve its biocompatibility and functionality. Thus, the present work is aimed to fabricate oxide films on metallic Zr by plasma electrolytic oxidation (PEO) in methodically varied concentrations of phosphate, silicate and KOH based electrolyte systems using a pulsed DC power source. The oxide films fabricated on Zr are characterized for its phase composition, surface morphology, chemical composition, roughness, wettability, surface energy, corrosion resistance, apatite forming ability and osteoblast cell adhesion. Uniform films with thickness varying from 6 to 11 μm are formed. XRD patterns of all the PEO films showed the predominance of monoclinic zirconia phase. The film formed in phosphate + KOH electrolyte showed superior corrosion resistance, which can be ascribed to its pore free morphology. The films formed in silicate electrolyte showed higher apatite forming ability with good cell adhesion and spreading over its surface which is attributed to its superior surface roughness and wettability characteristics. Among the five different electrolyte systems employed in the present study, the PEO film formed in an electrolyte system with phosphate + silicate + KOH showed optimum corrosion resistance, apatite forming ability and biocompatibility

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

    Science.gov (United States)

    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.

  6. Optical and electrical characteristics of zirconium oxide thin films deposited on silicon substrates by spray pyrolysis

    International Nuclear Information System (INIS)

    Aguilar-Frutis, M.; Araiza, J.J.; Falcony, C.; Garcia, M.

    2002-01-01

    The optical and electrical characteristics of zirconium oxide thin films deposited by spray pyrolysis on silicon substrates are reported. The films were deposited from a spraying solution of zirconium acetylacetonate in N,N-dimethylformamide using an ultrasonic mist generator on (100) Si substrates. The substrate temperature during deposition was in the range of 400 to 600 grad C. Deposition rates up to 16 A/sec were obtained depending on the spraying solution concentration and on the substrate temperature. A refraction index of the order of 2.0 was measured on these films by ellipsometry. The electrical characteristics of the films were determined from the capacitance and current versus voltage measurements. The addition of water mist during the spraying deposition process was also studied in the characteristics of the films. (Authors)

  7. Preliminary radiation-oxidizing treatment influence on electrophysical properties of zirconium

    International Nuclear Information System (INIS)

    Garibov, A.A.; Aliyev, A.G.; Agayev, T.N.; Ismailov, S.S.; Aliyev, S.M.; Velibekova, G.Z.

    2004-01-01

    The dependences of resistivity (ρ), thermoelectromotive force (α) voltage-current characteristics of thin zirconium film 80-200 mkm of thick from adsorbed dose of γ-quantum have been investigated. It has been found out that when initial meanings of absorbed dose are insignificant (D ≤ 20 kGy) in Zr-ZrO 2 system ρ is decreased at the expense of formation of point defects (biographic protective oxide film). The further increase of absorbed dose (up to definite value) leads to radiation-heterogeneous processes of protective oxide film formation with high vacancy concentration that is accompanied with ρ increase. (author)

  8. Growth and characterization of oxide layers on zirconium alloys

    International Nuclear Information System (INIS)

    Maroto, A.J.G.; Bordoni, R.; Villegas, M.; Olmedo, A.M.; Blesa, M.A.; Iglesias, A.; Koenig, P.

    1996-01-01

    In the range 265-435 C Zr-2.5Nb corrosion takes place in two stages, as opposed to the cyclic behaviour of Zry-4. The Zry-4 corrosion stages are described by a single equation, in terms of the dense oxide layer thickness that decreases sharply at each transition. Tetragonal zirconia is present in the oxide layers of both alloys. In Zry-4, its volume fraction decreases as the oxide grows; it is barely discernible in Zr-2.5Nb in films below 1 μm, to later increase up to the transition. In both alloys, compressive stresses are developed associated with the oxide growth. Their relaxation at the transition correlates with the transformation of ZrO 2 (t) to ZrO 2 (m) and with the decrease of the dense oxide layer. In Zr-2.5Nb, oxide ridges form on the β-Zr phase filaments, at the very onset of film growth. The cyclic behaviour associated with the periodical breakdown of the dense oxide layer is therefore blurred, although optical microscopy shows that the scale retains the multilayered structure typical of Zry-4. (orig.)

  9. Zirconium Micro-Arc Oxidation as a Method for Producing Heat Insulation Elements in Spacecraft

    Directory of Open Access Journals (Sweden)

    V. K. Shatalov

    2014-01-01

    Full Text Available Application of coatings on the surface of materials as well as their composition and structure control in the near-surface layer enables us to use properties of base material and modified layers in the most rational and profitable way and save expensive and rare metals and alloys.The space telescope of T-170M will be the main tool of the international space observatory "Spektr-UF".It is being understood that the main mirror shade, which is in the outer space and has a considerable height will act as a radiator cooling a unit (cage of the main mirror. Therefore it is necessary to create heat insulation between the shade of the main mirror and the frame of the main mirror unit. From the thermal calculations a detail to provide heat insulation must possess thermal conductivity, at most, 2,5 and a conditional limit of fluidity for compression, at least, 125 MPas to ensure that the shade diaphragms position of the main mirror is stable with respect to the optical system of telescope.Considering that oxide of zirconium possesses one of the lowest thermal conductivities among oxides of metals, it is offered to use zirconium, as a material of base, and to put the MAO-covering (micro-arc oxide on its surface.As a result of studying the features of MAO-coverings on zirconium it is:1 found that the composite material consisting of zirconium and MAO-covering on it, has low thermal conductivity (less than 2 , and thus, because of small oxide layer thickness against the thickness of base material, possesses the mechanical properties which are slightly different from the pure zirconium ones;2 found that the composite material possesses the low gas release, allowing its use in the outer space conditions; the material processed in two electrolytes i.e. phosphate and acid ones has the lowest gas release;3 found that with growing thickness of MAO-covering its porosity decreases, thus the average pore diameter grows thereby leading to increasing thermal

  10. Oxidation behaviour of zirconium alloys and their precipitates – A mechanistic study

    International Nuclear Information System (INIS)

    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.

  11. Phase stability of zirconium oxide films during focused ion beam milling

    Science.gov (United States)

    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.

  12. Sulphur mustard degradation on zirconium doped Ti-Fe oxides

    Czech Academy of Sciences Publication Activity Database

    Štengl, Václav; Matys Grygar, Tomáš; Opluštil, F.; Němec, T.

    2011-01-01

    Roč. 192, č. 3 (2011), s. 1491-1504 ISSN 0304-3894 Institutional research plan: CEZ:AV0Z40320502 Keywords : warfare agents * nanodispersive oxides * homogeneous hydrolysis * urea Subject RIV: CA - Inorganic Chemistry Impact factor: 4.173, year: 2011

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

    Science.gov (United States)

    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 zirconium oxide core-resin cement-titanium base, and the lowest was recorded for the polycarboxylate cement-zirconium oxide core (p zirconium are all important factors that determine the final shade of zirconia cores in implant-supported FPDs. © 2015 by the American College of Prosthodontists.

  14. Physicochemical study of zirconium oxides and of the alumina-zirconia dispersoid

    International Nuclear Information System (INIS)

    Orlans, Patrick

    1987-01-01

    This research thesis reports the physicochemical characterization of different zirconium oxides, but also their synthesis in laboratory by using a gel precipitation method. Various techniques are used to characterize gels and powders: electro-kinetic potential measurement, study of rheological properties, granulometry, chemical analysis, X-ray diffraction, thermo-luminescence, differential thermal analysis, specific surface measurements, scanning electronic microscopy. This process is then extended to the synthesis of an alumina-zirconia dispersoid. The measurement of mechanical properties allowed the synthesis to be modulated in order to obtain powders with properties as close as possible to defined properties [fr

  15. Characterization of the sorption behavior of trivalent actinides on zirconium(IV) oxide

    Energy Technology Data Exchange (ETDEWEB)

    Eibl, Manuel; Huittinen, Nina [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Surface Processes; Virtanen, S.; Merilaeinen, S.; Lehto, J. [Helsinki Univ. (Finland); Rabung, T. [Karlsruhe Institute of Technology (KIT), Karlsruhe (Germany). Inst. for Nuclear Waste Disposal

    2017-06-01

    The uptake of trivalent Eu and Cm on zirconium(IV) oxide was investigated in batch sorption and TRLFS studies, respectively. Sorption of Eu{sup 3+} was found to start at a pH-value of 4. Based on TRLFS results, sorption of Cm{sup 3+} was assigned to occur through innersphere complex formation at the zirconia surface. A deconvolution of the TRLFS emission spectra gave three different sorption species with strong red-shifts of the peak positions (600.3 nm, 604.3 nm and 608.2 nm) compared to similar systems.

  16. Investigation of anodizing parameter effect on barrier layer of anodic zirconium oxide

    International Nuclear Information System (INIS)

    Kharchenko, Eh.P.

    1979-01-01

    Effect of fluoride concentration and forming direction upon kinetics of barrier layer transformations in the process of preparation of phase anodic zirconium oxide in acid fluorine-containing solutions is considered. Suppositions are made on the mechanism of barrier layer transformation under the effect of the parameters mentioned. The thickness of the barrier layer is determined by two methods and it is shown that coefficient of the layer thickess growth at the voltage increase by 1 V is much lower than during formation of the barrier films in non-agressive electrolytes

  17. Contribution of in situ acoustic emission analysis coupled with thermogravimetry to study zirconium alloy oxidation

    International Nuclear Information System (INIS)

    Al Haj, O.; Peres, V.; Serris, E.; Cournil, M.; Grosjean, F.; Kittel, J.; Ropital, F.

    2015-01-01

    Zirconium alloy (zircaloy-4) corrosion behavior under oxidizing atmosphere at high temperature was studied using thermogravimetric experiment associated with acoustic emission analysis. Under a mixture of oxygen and air in helium, an acceleration of the corrosion is observed due to the detrimental effect of nitrogen which produces zirconium nitride. The kinetic rate increases significantly after a kinetic transition (breakaway). This acceleration is accompanied by an acoustic emission (AE) activity. Most of the acoustic emission bursts were recorded after the kinetic transition or during the cooling of the sample. Acoustic emission signals analysis allows us to distinguish different populations of cracks in the ZrO 2 layer. These cracks have also been observed by SEM on post mortem cross section of oxidized samples and by in-situ microscopy observations on the top surface of the sample during oxidation. The numerous small convoluted thin cracks observed deeper in the zirconia scale are not detected by the AE technique. From these studies we can conclude that mechanisms as irreversible mechanisms, as cracks initiation and propagation, generate AE signals

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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

  20. High performance solution processed zirconium oxide gate dielectric appropriate for low temperature device application

    Energy Technology Data Exchange (ETDEWEB)

    Hasan, Musarrat; Nguyen, Manh-Cuong; Kim, Hyojin; You, Seung-Won; Jeon, Yoon-Seok; Tong, Duc-Tai; Lee, Dong-Hwi; Jeong, Jae Kyeong; Choi, Rino, E-mail: rino.choi@inha.ac.kr

    2015-08-31

    This paper reports a solution processed electrical device with zirconium oxide gate dielectric that was fabricated at a low enough temperature appropriate for flexible electronics. Both inorganic dielectric and channel materials were synthesized in the same organic solvent. The dielectric constant achieved was 13 at 250 °C with a reasonably low leakage current. The bottom gate transistor devices showed the highest mobility of 75 cm{sup 2}/V s. The device is operated at low voltage with high-k dielectric with excellent transconductance and low threshold voltage. Overall, the results highlight the potential of low temperature solution based deposition in fabricating more complicated circuits for a range of applications. - Highlights: • We develop a low temperature inorganic dielectric deposition process. • We fabricate oxide semiconductor channel devices using all-solution processes. • Same solvent is used for dielectric and oxide semiconductor deposition.

  1. Experimental and numerical study of the effects of a nanocrystallisation treatment on high-temperature oxidation of a zirconium alloy

    International Nuclear Information System (INIS)

    Panicaud, B.; Retraint, D.; Grosseau-Poussard, J.-L.; Li, L.; Guérain, M.; Goudeau, P.; Tamura, N.; Kunz, M.

    2012-01-01

    Highlights: ► SMAT leads to a modification of surface properties of an M5 zirconium alloy (grain size and roughness. ► SMAT induces a change in the oxidation kinetics during high temperature oxidation. ► A diffusion model is able to reproduce kinetics and emphasise the consequences of SMAT on dissolution of oxygen in Zr. - Abstract: In the present work, the effects of a nanocrystallisation treatment on the high-temperature oxidation of a zirconium alloy are investigated. Surface Mechanical Attrition Treatment is a recent process designed to nanocrystallise the surface of materials. The particular effects of this treatment on an M5 zirconium alloy are studied using different experimental techniques at several scales. This material is of considerable interest, especially to the nuclear industry where very stringent conditions apply. High temperature oxidation was performed in order to show the benefits of this type of nanocrystallisation on the corrosion resistance of the alloy concerned. Microstructure development mechanisms, which improve the oxidation resistance of zirconium alloys have been identified during high-temperature corrosion. Those mechanisms have been discussed in further detail in relation to numerical calculations concerning the oxidation kinetics.

  2. Removal of methylene blue and rhodamine B from water by zirconium oxide/graphene

    Directory of Open Access Journals (Sweden)

    Sumita Rani

    2016-04-01

    Full Text Available Methylene blue (MB and rhodamine B dyes (RB were degraded from water using zirconium oxide (ZrO2 and zirconium oxide/graphene composites (ZrO2/GR as photocatalyst. The photocatalytic efficiency was calculated from absorption spectra obtained using UV–visible spectroscopy. It has been observed that photodegradation time as well as photocatalytic efficiency increase with the concentration of catalyst up to a certain limit after which effect was reversed. The degradation was studied as a function of pH also. It was found that photocatalytic efficiency was more in alkaline medium than acidic medium. Degradation of RB takes place at higher value of pH as compared to MB. The degradation time for MB was 1 h using ZrO2 which get reduced to 32 min using ZrO2/GR composite and for RB it reduced to 40 min (using ZrO2/GR from 80 min (ZrO2.

  3. Thermoluminescence of magnesium doped zirconium oxide (ZrO2:Mg) UV irradiated

    International Nuclear Information System (INIS)

    Rivera Montalvo, Teodoro; Furetta, Claudio

    2008-01-01

    Full text: The monitoring of ultraviolet radiation (UVR) different thermoluminescent (TL) materials have been used to measure UVR. UV dosimetry using thermoluminescence phenomena has been suggested in the past by several authors. This technique has an advantage over others methods due to the readout of the samples. Other advantages of these phosphors are their small size, portability, lack of any power requirements, linear response to increasing radiation dose and high sensitivity. Zirconium oxide, recently received full attention in view of their possible use as thermoluminescent dosimeter (TLD), if doped with suitable activators, in radiation dosimetry. In the present investigation thermoluminescent (TL) properties of magnesium doped zirconium oxide (ZrO 2 :Mg) under ultraviolet radiation (UVR) were studied. The ZrO 2 :Mg powder of size 30-40 nm, having mono clinical structure, exhibit a thermoluminescent glow curve with one peak centered at 180 C degrees. The TL response of ZrO 2 :Mg as a function ultraviolet radiation exhibits four maxima centered at 230, 260, 310 and 350 nmn. TL response of ZrO 2 :Mg as a function of spectral irradiance of UV Light was linear in a wide range. Fading and reusability of the phosphor were also studied. The results showed that ZrO 2 :Mg nano powder has the potential to be used as a UV dosemeter in UVR dosimetry. (author)

  4. Kinetic study of Cs+ and Eu3+ ions sorption by zirconium oxide powder

    International Nuclear Information System (INIS)

    Hanafi, H.A.; Hassan, H.S.; Hamed, M.M.

    2009-01-01

    Full text: Zirconium oxide powder was chemically synthesized by sol-gel method and characterized using infrared spectra and x-ray diffraction. The sorptive removal of cesium and europium ions from aqueous waste solution using synthetic zirconium oxide powder was investigated using batch technique. Experiments were carried out as a function of pH, time and temperature. The uptake of europium was found to be greater than that of cesium. A comparison of kinetic models applied to the sorption process of each ion was evaluated for the pseudo first order, the pseudo second order, and homogeneous particle diffusion kinetic models, respectively. The results showed that both the pseudo second order and the homogeneous particle diffusion models (HPDM) were found to best correlate the experimental rate data. The numerical values of the rate constants and particle diffusion coefficients were determined from the graphical representation of the proposed models. Activation energy (Ea) and entropy (Δ S*) of activation for each sorption process were also calculated from the linearized form of Arrhenius equation. (author)

  5. Analysis of the deconvolution of the thermoluminescent curve of the zirconium oxide doped with graphite

    International Nuclear Information System (INIS)

    Salas C, P.; Estrada G, R.; Gonzalez M, P.R.; Mendoza A, D.

    2003-01-01

    In this work, we present a mathematical analysis of the behavior of the thermoluminescent curve (Tl) induced by gamma radiation in samples made of zirconium oxide doped with different amounts of graphite. In accordance with the results gamma radiation induces a Tl curve with two maximum of emission localized in the temperatures at 139 and 250 C, the area under the curve is increasing as a function of the time of exposition to the radiation. The analysis of curve deconvolution, in accordance with the theory which indicates that this behavior must be obey a Boltzmann distribution, we found that each one of them has a different growth velocity as the time of exposition increase. In the same way, we observed that after the irradiation was suspended each one of the maximum decrease with different velocity. The behaviour observed in the samples is very interesting because the zirconium oxide has attracted the interest of many research groups, this material has demonstrated to have many applications in thermoluminescent dosimetry and it can be used in the quantification of radiation. (Author)

  6. Determination of the composition of surface optical layers prepared with the use of rare earth and zirconium oxides

    International Nuclear Information System (INIS)

    Mishchenko, V.T.; Shilova, L.P.; Shkol'nikova, T.M.

    1991-01-01

    Simple titrimetric and gravimetric methods for determination of optical oxide layers (rare earth and zirconium oxides), sputtered on glass or quartz sublayer, have been developed. The minimal determined oxide mass in surface layers is equal to 0.01 mg in titrimetric determination and 0.1 mg - in gravimetric one. It is shown that composition of films and pellets, used for film sputtering, is identical

  7. High-resolution characterization of oxidation mechanism of zirconium nuclear fuel cladding alloys

    International Nuclear Information System (INIS)

    Hu, J.; Lozano-Perez, S.; Grovenor, C.

    2015-01-01

    Full text of publication follows. Zirconium alloys are used extensively as cladding materials in modern light water reactors to separate the uranium dioxide (UO 2 ) fuel rods and the coolant water in order to prevent the escape of radioactive fission products whilst maintaining heat transfer to the coolant. With increasing demand for high burn-up in modern nuclear reactors, environmental degradation of these alloys is now the life limiting factor for fuel assemblies. As part of the MUZIC-2 collaboration studying oxidation and hydrogen pickup in Zr alloys, several high resolution analysis techniques have been used to study the microstructure of a range of commercial and developmental Zr alloys. The sample used for this investigation was prepared from a Westinghouse TM developmental alloy with composition of Zr-0.9Nb-0.01Sn-0.08Fe (wt %) in the recrystallized condition. The sample was oxidised in an autoclave at EDF Energy under simulated PWR water conditions at 360 C. degrees for 360 days. Using Transmission Electron Microscope (TEM), we have studied the development of the equiaxed-columnar-equiaxed grain structure, and observe that the columnar grains are both longer and show a stronger preferred texture in more corrosion-resistant alloys. Fresnel imaging revealed the existence of both parallel interconnected pores and some vertically interconnected pores along the columnar oxide grain boundaries, which become more disconnected near the metal-oxide interface. Electron Energy Loss Spectroscopy (EELS) provided accurate quantitative analysis of the oxygen concentration across the interface, identifying the existence of local regions of stoichiometric ZrO and Zr 3 O 2 with varying thickness. These observations will be discussed in the context of current models for oxidation in zirconium alloys. (authors)

  8. Irradiation effects of the zirconium oxidation and the uranium diffusion in zirconia; Effets d'irradiation sur l'oxydation du zirconium et la diffusion de l'uranium dans la zircone

    Energy Technology Data Exchange (ETDEWEB)

    Bererd, N

    2003-07-01

    The context of this study is the direct storage of spent fuel assemblies after operation in reactor. In order to obtain data on the capacities of the can as the uranium diffusion barrier, a fundamental study has been carried out for modelling the internal cladding surface under and without irradiation. The behaviour of zirconium in reactor conditions has at first been studied. A thin uranium target enriched with fissile isotope has been put on a zirconium sample, the set being irradiated by a thermal neutrons flux leading to the fission of the deposited uranium. The energetic history of the formed fission products has revealed two steps: 1)the zirconium oxidation and 2)the diffusion of uranium in the zirconia formed at 480 degrees C. A diffusion coefficient under irradiation has been measured. Its value is 10{sup -15} cm{sup 2}.s{sup -1}. In order to be able to reveal clearly the effect of the irradiation by the fission products on the zirconium oxidation, measurements of thermal oxidation and under {sup 129}Xe irradiation have been carried out. They have shown that the oxidation is strongly accelerated by the irradiation and that the temperature is negligible until 480 degrees C. On the other hand, the thermal diffusion of the uranium in zirconium and in zirconia has been studied by coupling ion implantation and Rutherford backscattering spectroscopy. This study shows that the uranium diffuses in zirconium and is trapped in zirconia in a UO{sub 3} shape. (O.M.)

  9. In vitro adsorption of oxalic acid and glyoxylic acid onto activated charcoal, resins and hydrous zirconium oxide

    NARCIS (Netherlands)

    Scholtens, R.; Scholten, J.; de Koning, H. W.; Tijssen, J.; ten Hoopen, H. W.; Olthuis, F. M.; Feijen, J.

    1982-01-01

    Patients suffering from primary hyperoxaluria show elevated plasma concentrations of oxalic acid and glyoxylic acid. The in vitro adsorption of these compounds into activated charcoal, a series of neutral and ion exchange resins and onto hydrous zirconium oxide has been investigated. Hydrous

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

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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.

  12. Stress-induced breakdown during galvanostatic anodising of zirconium

    International Nuclear Information System (INIS)

    Van Overmeere, Q.; Proost, J.

    2010-01-01

    Although internal stress is frequently being suggested as a plausible reason for oxide breakdown during valve metal anodising, no direct quantitative evidence has been made available yet. In this work, we anodized sputtered zirconium thin films galvanostatically at room temperature in sulphuric acid until breakdown was observed, and simultaneously measured the internal stress evolution in the oxide in situ, using a high-resolution curvature setup. It was found that the higher the magnitude of the observed internal compressive stress in the oxide, the smaller the oxide thickness at which breakdown occurred. The moment of breakdown was identified from a slope change in the cell voltage evolution, indicative for a decrease in anodising efficiency. The latter presumably occurs as a result of oxygen evolution, initiated by the relative increase of the cubic or tetragonal zirconia phase content relative to the monoclinic one. This was evidenced in turn by comparing electron diffractograms, taken in a transmission electron microscope, before and after breakdown. The critical role of internal stress on oxide breakdown during zirconium anodising can therefore be associated with its promoting effect on the densifying phase transformation of monoclinic oxide.

  13. Critical assessment of finite element analysis applied to metal–oxide interface roughness in oxidising zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Platt, P., E-mail: Philip.Platt@manchester.ac.uk [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom); Frankel, P. [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom); Gass, M. [AMEC, Walton House, Faraday Street, Birchwood Park, Risley, Warrington WA3 6GA (United Kingdom); Preuss, M. [University of Manchester, School of Materials, Materials Performance Centre, Manchester M13 9PL (United Kingdom)

    2015-09-15

    As a nuclear fuel cladding material, zirconium alloys act as a barrier between the fuel and pressurised steam or lithiated water environment. Controlling degradation mechanisms such as oxidation is essential to extending the in-service lifetime of the fuel. At temperatures of ∼360 °C zirconium alloys are known to exhibit cyclical, approximately cubic corrosion kinetics. With acceleration in the oxidation kinetics occurring every ∼2 μm of oxide growth, and being associated with the formation of a network of lateral cracks. Finite element analysis has been used previously to explain the lateral crack formation by the development of localised out-of-plane tensile stresses at the metal–oxide interface. This work uses the Abaqus finite element code to assess critically current approaches to representing the oxidation of zirconium alloys, with relation to undulations at the metal–oxide interface and localised stress generation. This includes comparison of axisymmetric and 3D quartered modelling approaches, and investigates the effect of interface geometry and plasticity in the metal substrate. Particular focus is placed on the application of the anisotropic strain tensor used to represent the oxidation mechanism, which is typically applied with a fixed coordinate system. Assessment of the impact of the tensor showed that 99% of the localised tensile stresses originated from the out-of-plane component of the strain tensor, rather than the in-plane expansion as was previously thought. Discussion is given to the difficulties associated with this modelling approach and the requirements for future simulations of the oxidation of zirconium alloys.

  14. Recovery of sodium hydroxide and silica from zirconium oxide plant effluent of Nuclear Fuel Complex

    International Nuclear Information System (INIS)

    Bajpai, M.B.; Shenoi, M.R.K.; Keni, V.S.

    1994-01-01

    Sodium hydroxide (lye) and silica can be recovered in pure form from the alkaline sodium silicate waste of Nuclear Fuel Complex, Hyderabad. Electrolytic method was used to amalgamate the sodium present in an electrolyser with flowing mercury as cathode and nickel as anode. The amalgam is then denuded with water in a graphite packed tower to recover mercury for recycling to the electrolyser and sodium hydroxide lye. Sodium hydroxide lye can be recycled in the zirconium oxide plant. Silica is recovered from the spent electrolyte by ion exchange method using cation exchange resin. Both the process details are described in this paper, with experimental data useful for the scale up. The process converts waste to value products. (author)

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

    Science.gov (United States)

    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.

  16. Recovery of sodium hydroxide and silica from zirconium oxide plant effluent of Nuclear Fuel Complex

    Energy Technology Data Exchange (ETDEWEB)

    Bajpai, M B; Shenoi, M R.K.; Keni, V S [Chemical Engineering Division, Bhabha Atomic Research Centre, Mumbai (India)

    1994-06-01

    Sodium hydroxide (lye) and silica can be recovered in pure form from the alkaline sodium silicate waste of Nuclear Fuel Complex, Hyderabad. Electrolytic method was used to amalgamate the sodium present in an electrolyser with flowing mercury as cathode and nickel as anode. The amalgam is then denuded with water in a graphite packed tower to recover mercury for recycling to the electrolyser and sodium hydroxide lye. Sodium hydroxide lye can be recycled in the zirconium oxide plant. Silica is recovered from the spent electrolyte by ion exchange method using cation exchange resin. Both the process details are described in this paper, with experimental data useful for the scale up. The process converts waste to value products. (author). 3 figs., 2 tabs.

  17. Structural and microstructural changes in the zirconium-indium mixed oxide system during the thermal treatment

    Science.gov (United States)

    Štefanić, G.; Štefanić, I. I.; Musić, S.; Ivanda, M.

    2011-05-01

    The zirconium-indium mixed oxide systems on both the zirconium- and the indium-rich side of the concentration range were prepared by co-precipitation from aqueous solutions of the corresponding salts, followed by washing and heat-treatment. The thermal behavior (up to 1000 °C) of the dried samples was examined by X-ray powder diffraction, Raman spectroscopy, Fourier transform infrared spectroscopy, field emission scanning electron microscopy, energy dispersive X-ray spectrometry, differential thermal analysis and thermogravimetric measurements. The obtained results show that the increase in the amount of the second phase causes an increase of both the crystallization temperature of the amorphous precursors of ZrO 2, from 435 °C (0 mol.% of InO 1.5) to 476 °C (˜62 mol.% of InO 1.5), and of the topotactic transition temperature of cubic In(OH) 3 to cubic In 2O 3, from 259 °C (0 mol.% of ZrO 2) to 290 °C (˜25 mol.% of ZrO 2). The amorphous precursors of ZrO 2 phase exhibit an extended capability to incorporate In 3+ ions (more than 60 mol.%). With a rise in temperature the maximum solubility of In 3+ ions in the ZrO 2 lattice decreases from ˜55 mol.% in the crystallization products obtained after calcination at 400 °C to ˜10 mol.% after calcination at 1000 °C. The results of phase analysis indicate that the incorporation of In 3+ ions partially stabilized both the tetragonal and cubic ZrO 2 polymorphs. The maximum solubility of Zr 4+ ions in the starting In(OH) 3 lattice was estimated at ˜10 mol.%. Thermal treatment causes a small increase of Zr 4+ ion solubility limits, estimated at ˜15 mol.% in the cubic In 2O 3 lattice after calcination at 1000 °C. Precise lattice parameter measurements, by using Le Bail refinements of the powder diffraction patterns with added silicon as an internal standard, show that the incorporation of In 3+ ions caused a very small decrease of the cubic ZrO 2 lattice, while the incorporation of Zr 4+ ions had a negligible

  18. Microstructure refinement and strengthening mechanisms of a 9Cr oxide dispersion strengthened steel by zirconium addition

    International Nuclear Information System (INIS)

    Xu, Hai Jian; Lu, Zheng; Wang, Dong Mei; Liu, Chunming

    2017-01-01

    To study the effects of zirconium (Zr) addition on the microstructure, hardness and the tensile properties of oxide dispersion strengthened (ODS) ferritic-martensitic steels, two kinds of 9Cr-ODS ferritic-martensitic steels with nominal compositions (wt.%) of Fe-9Cr-2W-0.3Y_2O-3 and Fe-9Cr-2W-0.3Zr-0.3Y_2O_3 were fabricated by the mechanical alloying (MA) of premixed powders and then consolidated by hot isostatic pressing (HIP) techniques. The experimental results showed that the average grain size decreases with Zr addition. The trigonal δ-phase Y_4Zr_3O_1_2 oxides and body-centered cubic Y_2O_3 oxides are formed in the 9Cr-Zr-ODS steel and 9Cr non-Zr ODS steel, respectively, and the average size of Y_4Zr_3O_1_2 particles is much smaller than that of Y_2O_3. The dispersion morphology of the oxide particles in 9Cr-Zr-ODS steel is significantly improved and the number density is 1.1 x 10"2"3/m"3 with Zr addition. The 9Cr-Zr-ODS steel shows much higher tensile ductility, ultimate tensile strength and Vickers hardness at the same time

  19. Microstructure refinement and strengthening mechanisms of a 9Cr oxide dispersion strengthened steel by zirconium addition

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Hai Jian; Lu, Zheng; Wang, Dong Mei; Liu, Chunming [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang (China)

    2017-02-15

    To study the effects of zirconium (Zr) addition on the microstructure, hardness and the tensile properties of oxide dispersion strengthened (ODS) ferritic-martensitic steels, two kinds of 9Cr-ODS ferritic-martensitic steels with nominal compositions (wt.%) of Fe-9Cr-2W-0.3Y{sub 2}O-3 and Fe-9Cr-2W-0.3Zr-0.3Y{sub 2}O{sub 3} were fabricated by the mechanical alloying (MA) of premixed powders and then consolidated by hot isostatic pressing (HIP) techniques. The experimental results showed that the average grain size decreases with Zr addition. The trigonal δ-phase Y{sub 4}Zr{sub 3}O{sub 12} oxides and body-centered cubic Y{sub 2}O{sub 3} oxides are formed in the 9Cr-Zr-ODS steel and 9Cr non-Zr ODS steel, respectively, and the average size of Y{sub 4}Zr{sub 3}O{sub 12} particles is much smaller than that of Y{sub 2}O{sub 3}. The dispersion morphology of the oxide particles in 9Cr-Zr-ODS steel is significantly improved and the number density is 1.1 x 10{sup 23}/m{sup 3} with Zr addition. The 9Cr-Zr-ODS steel shows much higher tensile ductility, ultimate tensile strength and Vickers hardness at the same time.

  20. Preliminary radiation-oxidizing treatment influence on radiation-catalytic activity of zirconium during water decomposition process

    International Nuclear Information System (INIS)

    Garibov, A.A.; Aliyev, A.G.; Agayev, T.N.; Aliyev, S.M.; Velibekova, G.Z.

    2004-01-01

    The study of physical-chemical processes proceeding in contact of metal constructional materials nuclear reactors with water at simultaneous influence of temperature and radiation represents the large interest at the decision of problems material authority and safety of work of nuclear -power installations [1-2]. One of the widely widespread materials of active zone nuclear reactors is metal zirconium and its alloys. The influence of preliminary radiation processing on radiation, radiation -thermal and thermal processes of accumulation of molecular hydrogen and oxidation zirconium in contact with water is investigated at T=673 K and ρ=5mg/sm 3 [3-4]. Initial samples zirconium previously has been exposed by an irradiation in medium H 2 O 2 at D=20-410 kGy. The contribution of radiation processes in these contacts in process thermo-radiation decomposition of water and oxidation of materials of zirconium is revealed. It is established that the interaction of Zr metal, preliminary treated by radiation, with water at radiation -heterogeneous processes leads to passivity of a surface. The rate meanings of thermal, radiation -thermal processes and radiation-chemical yields of hydrogen are determined. It is revealed, that at radiation-heterogeneous processes in system Zr +H 2 O (ρ =5mg/sm 3 T=673 K) the increase of the absorbed doze up to 123 kGy results to reduction of a radiation -chemical yield of molecular hydrogen. The further increase of the absorbed doze results to increase of a radiation -chemical yield of hydrogen. The observable effect at the preliminary radiation of zirconium is connected to formation of oxide phase on a surface. The mechanism of radiation -heterogeneous processes proceeding in system Zr+H 2 O is suggested. (author)

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

    Science.gov (United States)

    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-Wzirconium-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

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

    Science.gov (United States)

    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

  3. Zr{sub 2}N{sub 2}Se. The first zirconium(IV) nitride selenide by the oxidation of zirconium(III) nitride with selenium

    Energy Technology Data Exchange (ETDEWEB)

    Lissner, Falk; Hack, Bettina; Schleid, Thomas [Institute for Inorganic Chemistry, University of Stuttgart (Germany); Lerch, Martin [Institute for Chemistry, Technical University of Berlin (Germany)

    2012-08-15

    The oxidation of zirconium(III) nitride (ZrN) with suitable amounts of selenium (Se) in the presence of sodium chloride (NaCl) as flux yields small yellow brownish platelets of the first zirconium(IV) nitride selenide with the composition Zr{sub 2}N{sub 2}Se. The new compound crystallizes in the hexagonal space group P6{sub 3}/mmc (no. 194) with a = 363.98(2) pm, c = 1316.41(9) pm (c/a = 3.617) and two formula units per unit cell. The crystallographically unique Zr{sup 4+} cations are surrounded by three selenide and four nitride anions in the shape of a capped trigonal antiprism. The Se{sup 2-} anions are coordinated by six Zr{sup 4+} cations as trigonal prism and the N{sup 3-} anions reside in tetrahedral surrounding of Zr{sup 4+} cations. These [NZr{sub 4}]{sup 13+} tetrahedra become interconnected via three edges each to form {sup 2}{sub ∞}{[(NZr_4_/_4)_2]"2"+} double layers parallel to the (001) plane, which are held together by monolayers of Se{sup 2-} anions. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  4. Diagnostic study of the roughness surface effect of zirconium on the third-order nonlinear-optical properties of thin films based on zinc oxide nanomaterials

    International Nuclear Information System (INIS)

    Bahedi, K.; Addou, M.; El Jouad, M.; Sofiani, Z.; Alaoui Lamrani, M.; El Habbani, T.; Fellahi, N.; Bayoud, S.; Dghoughi, L.; Sahraoui, B.; Essaidi, Z.

    2009-01-01

    Zinc oxide (ZnO) and zirconium doped zinc oxide (ZnO:Zr) thin films were deposited by reactive chemical pulverization spray pyrolysis technique on heated glass substrates at 500 deg. C using zinc and zirconium chlorides as precursors. Effects of zirconium doping agent and surface roughness on the nonlinear optical properties were investigated in detail using atomic force microscopy (AFM) and third harmonic generation (THG) technique. The best value of nonlinear optical susceptibility χ (3) was obtained from the doped films with less roughness. A strong third order nonlinear optical susceptibility χ (3) = 20.12 x 10 -12 (esu) of the studied films was found for the 3% doped sample.

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

    OpenAIRE

    Felemban, Nayef H.; Ebrahim, Mohamed I.

    2017-01-01

    Background 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. Methods 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 di...

  6. Reactive removal of 2-chloroethyl ethyl sulfide vapors under visible light irradiation by cerium oxide modified highly porous zirconium (hydr) oxide

    Energy Technology Data Exchange (ETDEWEB)

    Mitchell, Joshua K.; Arcibar-Orozco, Javier A.; Bandosz, Teresa J., E-mail: tbandosz@ccny.cuny.edu

    2016-12-30

    Highlights: • Microporous zirconium-cerium (hydr) oxides were synthetized. • Ce presence narrowed the band gap of the materials. • The samples showed a high efficiency for removal of CEES vapors. • 1,2-Bis (ethyl thio) ethane and ethyl vinyl sulfide were the main reaction products. • 5% (Ce/Zr mol) addition of cerium oxide results in the best performing material. - Abstract: Highly porous cerium oxide modified Zr(OH){sub 4} samples were synthesized using a simple one stage urea precipitation method. The amorphicity level of zirconium hydroxide did not change upon addition of cerium oxide particles. A unique aspect of the cerium oxide-modified materials is the presence of both the oxide (CeO{sub 2}) and hydroxide (Zr(OH){sub 4}) phases resulting in a unique microporous structure of the final material. Extensive characterization using various chemical and physical methods revealed significant differences in the surface features. All synthesized materials were microporous and small additions of cerium oxide affected the surface chemistry. These samples were found as effective catalysts for a decontamination of mustard gas surrogate, 2-chloroethyl ethyl sulfide (CEES). Cerium oxide addition significantly decreased the band gap of zirconium hydroxide. Ethyl vinyl sulfide and 1,2-bis (Ethyl thio) ethane were identified as surface reaction products.

  7. Silica-gel modified with zirconium oxide as a novel 99Mo adsorbent 99mTc generators

    International Nuclear Information System (INIS)

    Salehi, H.; Mollarazi, E.; Abbasi, H.

    2010-01-01

    A new 99 Mo adsorbent has been prepared with modified silica gel with zirconium oxide (SiO 2 /ZrO 2 :Na 2 MoO 4 ) and used in technetium-99m generator. The adsorption behaviors of 99 Mo in the form of molybdate and 99m Tc in the form of pertechnetate on the new adsorbent was investigated showed that the adsorption capacity of molybdate on this generator was considerably higher than the usual generator with alumina column. Coating zirconium oxide on the surface of silica gel resulted in higher 99 Mo adsorption of this compound. 99m Tc is eluted with 0.9% NaCl, and the radionuclidic, radiochemical and chemical purities of the eluate were checked. This generator has a great potential as compared to the traditional alumina generators.

  8. Evolution of zirconium-based precipitates during oxidation and irradiation of Zr alloys (impact on the oxidation kinetics of Zr alloys)

    International Nuclear Information System (INIS)

    Pecheur, Dominique

    1993-01-01

    As the oxidation of the zircaloy sheath is one of the factors which limit the lifetime of nuclear fuel rods, this research thesis aims at a better knowledge of the involved oxidation mechanisms and to improve the oxidation resistance in order to increase rod lifetime. Oxidation test performed in autoclave to study zirconium alloy oxidation without irradiation showed that oxidation kinetics is significantly higher under irradiation. This difference is attributed to a different evolution of the sheath material under irradiation. Thus, this research focused on the role of precipitates in the oxidation process of zirconium alloys, and on the impact of their amorphization on this oxidation. After a detailed description of the context and of the various implemented experimental means, the author presents the results obtained on a reference material on the one hand, and on a material irradiated by ions or neutrons on the other hand. More particularly, the author studied in these both cases the introduction of precipitates in the oxide layer by transmission electronic microscopy, and oxidation kinetics obtained in autoclave on these two types of material. He reports the analysis of the introduction of precipitates in the oxide layer formed on the reference material. He proposes interpretations for the evolutions of structure and of chemical compositions of precipitates in the oxide layer. These observations are then correlated with oxidation kinetics in these alloys. Finally, the author discusses results of oxidation tests obtained on materials irradiated by ions and by neutrons [fr

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

    Science.gov (United States)

    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.

  10. Electrochemical oxidation of zirconium alloys in pre-transition and post-transition kinetic regimes at corrosion in electrolyte solutions

    International Nuclear Information System (INIS)

    Barkov, A.A.; Shavshin, V.M.

    1986-01-01

    With the aim of investigation on oxidation of zirconium alloys (Zr+2.5% Nb) the critical thickness of beginning of spalling of froming oxide films in HCl and NHO 3 aqueous solutions was evaluated by coulometry with accelerated procedure. Some variants of predeposition of modificated oxide coatings are proposed increase pre-transition regime time and to decrease corrosion during post-transition regime. Increase in agressivity of solutions (addition of 1 vol.% HF) and UV irradiation are found to increase 3-4 times pre-transition period

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

    Science.gov (United States)

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

    2016-06-29

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

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

    Directory of Open Access Journals (Sweden)

    Nor Monica Ahmad

    2016-06-01

    Full Text Available 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.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

    Highlights: • Magnetic zirconium-iron oxide nanoparticle (MZION) was successfully synthesized. • The removal of phosphate could be effectively fulfilled using MZION. • MZION could be conveniently separated by magnet after adsorption. • The Fe/Zr molar ratios played a key role in adsorption capacity and magnetic separation. - Abstract: In this study, magnetic zirconium-iron oxide nanoparticles (MZION) of different Fe/Zr molar ratios were successfully prepared using the co-precipitation method, and their performance for phosphate removal was systematically evaluated. The as-obtained adsorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential analyzer, Fourier transform infrared spectroscopy (FT-IR) and Brunauer Emmett Teller (BET) specific surface area analysis. The effects of pH, ionic strength, and co-existing ions (including Cl − , SO 4 2− , NO 3 − and HCO 3 − ) were measured to evaluate the adsorption performance in batch experiments. The results showed that decreasing the Fe/Zr molar ratios increased the specific surface area that was propitious to adsorption process, but the adsorption capacity enhanced with the decrease of Fe/Zr molar ratios. Phosphate adsorption on MZION could be well described by the Freundlich equilibrium model and pseudo-second-order kinetics. The adsorption of phosphate was highly pH dependent and decreased with increasing pH from 1.5 to 10.0. The adsorption was slightly affected by ionic strength. With the exception of HCO 3 − , co-existing anions showed minimum or no effect on their adsorption performance. After adsorption, phosphate on these MZION could be easily desorbed by 0.1 M NaOH solution. The phosphate adsorption mechanism of MZION followed the inner-sphere complexing mechanism, and the surface −OH groups played a significant role in the phosphate adsorption. Additionally, the main advantages of MZION consisted in its

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

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Chang, E-mail: zhangchang@hnu.edu.cn [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control (Hunan University), Ministry of Education, Changsha 410082 (China); Li, Yongqiu [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control (Hunan University), Ministry of Education, Changsha 410082 (China); Wang, Fenghua, E-mail: 952157786@qq.com [Institute of Physical Education, Xinjiang Normal University, Urumqi 830054 (China); Yu, Zhigang; Wei, Jingjing; Yang, Zhongzhu; Ma, Chi; Li, Zihao; Xu, ZiYi; Zeng, Guangming [College of Environmental Science and Engineering, Hunan University, Changsha 410082 (China); Key Laboratory of Environmental Biology and Pollution Control (Hunan University), Ministry of Education, Changsha 410082 (China)

    2017-02-28

    Highlights: • Magnetic zirconium-iron oxide nanoparticle (MZION) was successfully synthesized. • The removal of phosphate could be effectively fulfilled using MZION. • MZION could be conveniently separated by magnet after adsorption. • The Fe/Zr molar ratios played a key role in adsorption capacity and magnetic separation. - Abstract: In this study, magnetic zirconium-iron oxide nanoparticles (MZION) of different Fe/Zr molar ratios were successfully prepared using the co-precipitation method, and their performance for phosphate removal was systematically evaluated. The as-obtained adsorbents were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Zeta potential analyzer, Fourier transform infrared spectroscopy (FT-IR) and Brunauer Emmett Teller (BET) specific surface area analysis. The effects of pH, ionic strength, and co-existing ions (including Cl{sup −}, SO{sub 4}{sup 2−}, NO{sub 3}{sup −} and HCO{sub 3}{sup −}) were measured to evaluate the adsorption performance in batch experiments. The results showed that decreasing the Fe/Zr molar ratios increased the specific surface area that was propitious to adsorption process, but the adsorption capacity enhanced with the decrease of Fe/Zr molar ratios. Phosphate adsorption on MZION could be well described by the Freundlich equilibrium model and pseudo-second-order kinetics. The adsorption of phosphate was highly pH dependent and decreased with increasing pH from 1.5 to 10.0. The adsorption was slightly affected by ionic strength. With the exception of HCO{sub 3}{sup −}, co-existing anions showed minimum or no effect on their adsorption performance. After adsorption, phosphate on these MZION could be easily desorbed by 0.1 M NaOH solution. The phosphate adsorption mechanism of MZION followed the inner-sphere complexing mechanism, and the surface −OH groups played a significant role in the phosphate adsorption. Additionally, the main

  15. Behaviour of zirconium oxidation and is oxide films in alkali halide solutions as studied by electrochemical techniques

    International Nuclear Information System (INIS)

    Saleh, H.E.M.

    1996-01-01

    Study of the properties of Zr electrode and the oxide films that cover the metal surface is of extreme importance due to their wide applications in chemical and nuclear industry. In this thesis the electrochemical behaviour of Zr electrode in alkali halide solutions and with various surface conditions was studied, Also the galvanostatic oxidation of the metal in addition to the open circuit and impedance measurements were employed. Chapter I is a literature survey of the electrochemistry of Zr metal with particular emphasis on the stability and growth process of Zr in different media. Chapter II contains the experimental part, including details of the electrochemical techniques used in the measurements. The electrode impedance was always balanced as a series capacitance Cs and resistance Rs.Chapter III includes the experimental results and discussion. It is divide into sections, A and B. Section A includes the results of some experimental parameters which affect the reactivity of the oxide growth process on the zirconium surface, such as surface pre - treatment, electrolyte composition, the effect of different alkali halide anions, as well as the triiodide ion. 9 tabs.,26 figs.,67 refs

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

    Science.gov (United States)

    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.

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

    Science.gov (United States)

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

    2016-05-01

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

  18. Creep behavior under internal pressure of zirconium alloy cladding oxidized in steam at high temperature

    International Nuclear Information System (INIS)

    Chosson, Raphael

    2014-01-01

    During hypothetical Loss-Of-Coolant-Accident (LOCA) scenarios, zirconium alloy fuel cladding tubes creep under internal pressure and are oxidized on their outer surface at high temperature (HT). Claddings become stratified materials: zirconia and oxygen-stabilized α phase, called α(O), are formed on the outer surface of the cladding whereas the inner part remains in the β domain. The strengthening effect of oxidation on the cladding creep behavior under internal pressure has been highlighted at HT. In order to model this effect, the creep behavior of each layer had to be determined. This study focused on the characterization of the creep behavior of the α(O) phase at HT, through axial creep tests performed under vacuum on model materials, containing from 2 to 7 wt.% of oxygen and representative of the α(O) phase. For the first time, two creep flow regimes have been observed in this phase. Underlying physical mechanisms and relevant microstructural parameters have been discussed for each regime. The strengthening effect due to oxygen on the α(O) phase creep behavior at HT has been quantified and creep flow equations have been identified. A ductile to brittle transition criterion has been also suggested as a function of temperature and oxygen content. Relevance of the creep flow equations for each layer, identified in this study or from the literature, has been discussed. Then, a finite element model, describing the oxidized cladding as a stratified material, has been built. Based on this model, a fraction of the experimental strengthening during creep is predicted. (author) [fr

  19. Layer-by-layer deposition of zirconium oxide films from aqueous solutions for friction reduction in silicon-based microelectromechanical system devices

    International Nuclear Information System (INIS)

    Liu Junfu; Nistorica, Corina; Gory, Igor; Skidmore, George; Mantiziba, Fadziso M.; Gnade, Bruce E.

    2005-01-01

    This work reports layer-by-layer deposition of zirconium oxide on a Si surface from aqueous solutions using the successive ionic layer adsorption and reaction technique. The process consists of repeated cycles of adsorption of zirconium precursors, water rinse, and hydrolysis. The film composition was determined by X-ray photoelectron spectroscopy. The film thickness was determined by Rutherford backscattering spectrometry, by measuring the Zr atom concentration. The average deposition rate from a 0.1 M Zr(SO 4 ) 2 solution on a SiO 2 /Si surface is 0.62 nm per cycle. Increasing the acidity of the zirconium precursor solution inhibits the deposition of the zirconium oxide film. Atomic force microscopy shows that the zirconium oxide film consists of nanoparticles of 10-50 nm in the lateral dimension. The surface roughness increased with increasing number of deposition cycles. Friction measurements made with a microelectromechanical system device reveal a reduction of 45% in the friction coefficient of zirconium oxide-coated surfaces vs. uncoated surfaces in air

  20. Fabrication of a Biomass-Based Hydrous Zirconium Oxide Nanocomposite for Preferable Phosphate Removal and Recovery.

    Science.gov (United States)

    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.

  1. Thermoluminescence of zirconium oxide nanostructured to mammography X-ray beams

    Energy Technology Data Exchange (ETDEWEB)

    Palacios, L.L. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada-Legaria, IPN. Av. Legaria 694, 11500 Mexico D.F. (Mexico); Rivera, T., E-mail: trivera@ipn.mx [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada-Legaria, IPN. Av. Legaria 694, 11500 Mexico D.F. (Mexico); Roman, J. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada-Legaria, IPN. Av. Legaria 694, 11500 Mexico D.F. (Mexico); Azorin, J. [Universidad Autonoma Metropolitana-Iztapalapa. Av. San Rafael Atlixco 187, 09340 Mexico D.F. (Mexico); Gaona, E. [Universidad Autonoma Metropolitana-Xochimilco. Calz. Del Hueso 1100, 04960 Mexico D.F. (Mexico)

    2012-07-15

    In the present work thermoluminescent (TL) response of zirconium oxide (ZrO{sub 2}) nanostructured induced by mammography X-ray radiation was investigated. Measurements were made of the response per unit air kerma of ZrO{sub 2} with mammography equipment parameters (semiautomatic exposure control, 24 kVp and 108 mAs). The calibration curves were obtained by simultaneously irradiating ZrO{sub 2} samples and ion chamber. Samples of ZrO{sub 2} showed a linear response as a function of entrance skin air kerma. The observed results in TL properties suggest that ZrO{sub 2} nanostructured could be considered as an effective material for X-ray beams dosimetry if appropriate calibration procedures are performed. - Highlights: Black-Right-Pointing-Pointer X-ray low energy thermoluminescent of ZrO{sub 2} dosimeter is developed. Black-Right-Pointing-Pointer Air kerma measurements were made by thermoluminescent dosimeter ZrO{sub 2} using mammography equipment parameters. Black-Right-Pointing-Pointer Entrance surface skin doses were made using thermoluminescent dosimeter of ZrO{sub 2} to X-ray beam quality control.

  2. Thermoluminescence of zirconium oxide nanostructured to mammography X-ray beams

    International Nuclear Information System (INIS)

    Palacios, L.L.; Rivera, T.; Roman, J.; Azorín, J.; Gaona, E.

    2012-01-01

    In the present work thermoluminescent (TL) response of zirconium oxide (ZrO 2 ) nanostructured induced by mammography X-ray radiation was investigated. Measurements were made of the response per unit air kerma of ZrO 2 with mammography equipment parameters (semiautomatic exposure control, 24 kVp and 108 mAs). The calibration curves were obtained by simultaneously irradiating ZrO 2 samples and ion chamber. Samples of ZrO 2 showed a linear response as a function of entrance skin air kerma. The observed results in TL properties suggest that ZrO 2 nanostructured could be considered as an effective material for X-ray beams dosimetry if appropriate calibration procedures are performed. - Highlights: ► X-ray low energy thermoluminescent of ZrO 2 dosimeter is developed. ► Air kerma measurements were made by thermoluminescent dosimeter ZrO 2 using mammography equipment parameters. ► Entrance surface skin doses were made using thermoluminescent dosimeter of ZrO 2 to X-ray beam quality control.

  3. High Temperature Oxidation Behavior of Zirconium Alloy with Nano structured Oxide Layer in Air Environment

    International Nuclear Information System (INIS)

    Park, Y. J.; Kim, J. W.; Park, J. W.; Cho, S. O.

    2016-01-01

    If the temperature of the cladding materials increases above 1000 .deg. C, which can be caused by a loss of coolant accident (LOCA), Zr becomes an auto-oxidation catalyst and hence produces a huge amount of hydrogen gas from water. Therefore, many investigations are being carried out to prevent (or reduce) the hydrogen production from Zr-based cladding materials in the nuclear reactors. Our team has developed an anodization technique by which nanostructured oxide can be formed on various flat metallic elements such as Al, Ti, and Zr-based alloy. Anodization is a simple electrochemical technique and requires only a power supply and an electrolyte. In this study, Zr-based alloys with nanostructured oxide layers were oxidized by using Thermogravimetry analysis (TGA) and compared with the pristine one. It reveals that the nanostructured oxide layer can prevent oxidation of substrate metal in air. Oxidation behavior of the pristine Zr-Nb-Sn alloy and the Zr-Nb-Sn alloy with nanostructured oxide layer evaluated by measuring weight gain (TGA). In comparison with the pristine Zr-Nb-Sn alloy, weight gain of the Zr-Nb-Sn alloy with nanostructured oxide layer is lower than 10% even for 12 hours oxidation in air.

  4. Influence of preliminary radiation-oxidizing treatment on the corrosion resistance of zirconium in conditions of action of ionizing radiation

    International Nuclear Information System (INIS)

    Garibov, A. A.; Aliyev, A. G.; Agayev, T. N.; Velibekova, G. Z.

    2004-01-01

    Today mainly water-cooled nuclear reactors predominate in atomic energetics. For safe work of nuclear reactors detection of accumulation process of explosives, formed during radiation and temperature influence on heat-carriers in contact with materials of nuclear reactors in normal and emergency regimes of work is of great importance. The main sources of molecular hydrogen formation in normal and emergency regimes are the processes of liquid and vaporous water in vapo metallic reaction [1-5]. At the result of these processes molecular hydrogen concentration in heat-carrier composition always exceeds theoretically expected concentration. One of the main ways to solve the problem of water-cooled reactors safety is detection of possibilities to raise material resistance of fuel elements and heat carrier to joint action of ionizing radiation and temperature. The second way is inhibition of radiation-catalytic activity of construction materials' surface during the process of water decomposition. It's been established, that one of the ways to raise resistance of zirconium materials to the influence of ionizing radiation is formation of thin oxide film on the surface of metals. In the given work the influence of preliminary oxidizing treatment of zirconium surface on its radiation-catalytic activity during the process of water decomposition. With this aim zirconium is exposed to preliminary influence of gamma-quantum in contact with hydrogen peroxide at different meanings of absorbed radiation dose

  5. Zirconium oxide deposits (ZrO2) and titanium oxide (TiO2) on 304l stainless steel

    International Nuclear Information System (INIS)

    Davila N, M. L.

    2015-01-01

    This research project aims to carry out the surface and electrochemical characterization to obtain the optimum conditions of the hydrothermal deposits of zirconium oxide ZrO 2 (baddeleyite) and titanium oxide TiO 2 (anatase and rutile phases) on 304l stainless steel, simulating an inhibiting protective layer. 304l steel specimens were cut, pre-oxidized in water at a temperature of 288 degrees Celsius and 8 MPa, similar to those of a typical BWR conditions. From the titanium oxide anatase crystalline phase, the rutile phase was obtained by a heat treatment at 1000 degrees Celsius. The Sigma-Aldrich pre-oxidized powders and steel 304l were characterized using techniques of X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, chemical mapping and Raman spectrometry. The pre-oxidized steel has two oxide layers, an inner layer with nano metric crystals and another outer of larger crystals to 1μm, with the formation of hematite and magnetite, this predominating. The surface that contacted the sample holder has larger crystals. Hydrothermal deposits were carry out from suspensions of 10, 100 and 1000 ppm, of the crystal phases of anatase, rutile and baddeleyite, on the pre-oxidized steel at a temperature of 150 degrees Celsius for 2 and 7 days, samples were analyzed by X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, Raman spectrometry and Tafel polarization. The suspension to 1000 ppm for 7 days coated surface most; the baddeleyite deposit is noticed more homogeneous than anatase and rutile. The deposit is favored when hematite and magnetite crystals are larger. The chemical mapping on deposits show that even after being immersed in water to 288 degrees Celsius during 30 days, the deposits are still present although a loss is observed. A reference electrode was assembled to conduct electrochemical tests of Tafel able to withstand a temperature of 288 degrees Celsius and pressure of 8 MPa. The baddeleyite deposit presented

  6. Effects of Oxidation and fractal surface roughness on the wettability and critical heat flux of glass-peened zirconium alloy tubes

    International Nuclear Information System (INIS)

    Fong, R.W.L.; Nitheanandan, T.; Bullock, C.D.; Slater, L.F.; McRae, G.A.

    2003-05-01

    Glass-bead peening the outside surfaces of zirconium alloy tubes has been shown to increase the Critical Heat Flux (CHF) in pool boiling of water. The CHF is found to correlate with the fractal roughness of the metal tube surfaces. In this study on the effect of oxidation on glass-peened surfaces, test measurements for CHF, surface wettability and roughness have been evaluated using various glass-peened and oxidized zirconium alloy tubes. The results show that oxidation changes the solid-liquid contact angle (i.e., decreases wettability of the metal-oxide surface), but does not change the fractal surface roughness, appreciably. Thus, oxidation of the glass-peened surfaces of zirconium alloy tubes is not expected to degrade the CHF enhancement obtained by glass-bead peening. (author)

  7. Physicochemical and mechanical properties of zirconium oxide and niobium oxide modified Portland cement-based experimental endodontic sealers.

    Science.gov (United States)

    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) and lower solubility when compared with MTA Fillapex and Sealapex (P 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.

  8. Trap state passivation improved hot-carrier instability by zirconium-doping in hafnium oxide in a nanoscale n-metal-oxide semiconductor-field effect transistors with high-k/metal gate

    International Nuclear Information System (INIS)

    Liu, Hsi-Wen; Tsai, Jyun-Yu; Liu, Kuan-Ju; Lu, Ying-Hsin; Chang, Ting-Chang; Chen, Ching-En; Tseng, Tseung-Yuen; Lin, Chien-Yu; Cheng, Osbert; Huang, Cheng-Tung; Ye, Yi-Han

    2016-01-01

    This work investigates the effect on hot carrier degradation (HCD) of doping zirconium into the hafnium oxide high-k layer in the nanoscale high-k/metal gate n-channel metal-oxide-semiconductor field-effect-transistors. Previous n-metal-oxide semiconductor-field effect transistor studies demonstrated that zirconium-doped hafnium oxide reduces charge trapping and improves positive bias temperature instability. In this work, a clear reduction in HCD is observed with zirconium-doped hafnium oxide because channel hot electron (CHE) trapping in pre-existing high-k bulk defects is the main degradation mechanism. However, this reduced HCD became ineffective at ultra-low temperature, since CHE traps in the deeper bulk defects at ultra-low temperature, while zirconium-doping only passivates shallow bulk defects.

  9. Effect of DC Plasma Electrolytic Oxidation on Surface Characteristics and Corrosion Resistance of Zirconium

    Directory of Open Access Journals (Sweden)

    Maciej Sowa

    2018-05-01

    Full Text Available 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(H2PO22, Ca(HCOO2, and Mg(CH3COO2 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    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 R dq 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

  11. Zirconium metal-water oxidation kinetics. V. Oxidation of Zircaloy in high pressure steam

    International Nuclear Information System (INIS)

    Pawel, R.E.; Cathcart, J.V.; Campbell, J.J.; Jury, S.H.

    1977-12-01

    A series of scoping tests to determine the influence of steam pressure on the isothermal oxidation kinetics of Zircaloy-4 PWR tubing was undertaken. The oxidation experiments were conducted in flowing steam at 3.45, 6.90, and 10.34 MPa (500, 1000, and 1500 psi) at 905 0 C (1661 0 F), and at 3.45 and 6.90 MPa at 1101 0 C (2014 0 F). A comparison of the results of these experiments with those obtained for oxidation in steam at atmospheric pressure under similar conditions indicated that measurable enhancement of the oxidation rate occurred with increasing pressure at 905 0 C, but not at 1100 0 C

  12. Electroless deposition process for zirconium and zirconium alloys

    Science.gov (United States)

    Donaghy, Robert E.; Sherman, Anna H.

    1981-01-01

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

  13. Zirconium metal-water oxidation kinetics. III. Oxygen diffusion in oxide and alpha Zircaloy phases

    International Nuclear Information System (INIS)

    Pawel, R.E.

    1976-10-01

    The reaction of Zircaloy in steam at elevated temperature involves the growth of discrete layers of oxide and oxygen-rich alpha Zircaloy from the parent beta phase. The multiphase, moving boundary diffusion problem involved is encountered in a number of important reaction schemes in addition to that of Zircaloy-oxygen and can be completely (albeitly ideally) characterized through an appropriate model in terms of oxygen diffusion coefficients and equilibrium concentrations for the various phases. Conversely, kinetic data for phase growth and total oxygen consumption rates can be used to compute diffusion coefficients. Equations are developed that express the oxygen diffusion coefficients in the oxide and alpha phases in terms of the reaction rate constants and equilibrium solubility values. These equations were applied to recent experimental kinetic data on the steam oxidation of Zircaloy-4 to determine the effective oxygen diffusion coefficients in these phases over the temperature range 1000--1500 0 C

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

    Science.gov (United States)

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

    2017-02-01

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

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

    Science.gov (United States)

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

    2015-03-02

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

  16. Multifunctional zirconium oxide doped chitosan based hybrid nanocomposites as bone tissue engineering materials.

    Science.gov (United States)

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

    2016-10-20

    This paper reports the development of multifunctional zirconium oxide (ZrO2) doped nancomposites having chitosan (CTS), organically modified montmorillonite (OMMT) and nano-hydroxyapatite (HAP). Formation of these nanocomposites was confirmed by various characterization techniques such as Fourier transform infrared spectroscopy and powder X-ray diffraction. Scanning electron microscopy images revealed uniform distribution of OMMT and nano-HAP-ZrO2 into CTS matrix. Powder XRD study and TEM study revealed that OMMT has partially exfoliated into the polymer matrix. Enhanced mechanical properties in comparison to the reported literature were obtained after the addition of ZrO2 nanoparticle into the nanocomposites. In rheological measurements, CMZH I-III exhibited greater storage modulus (G') than loss modulus (G″). TGA results showed that these nanocomposites are thermally more stable compare to pure CTS film. Strong antibacterial zone of inhibition and the lowest minimum inhibition concentration (MIC) value of these nanocomposites against bacterial strains proved that these materials have the ability to prevent bacterial infection in orthopedic implants. Compatibility of these nanocomposites with pH and blood of human body was established. It was observed from the swelling study that the swelling percentage was increased with decreasing the hydrophobic OMMT content. Human osteoblastic MG-63 cell proliferations were observed on the nanocomposites and cytocompatibility of these nanocomposites was also established. Moreover, addition of 5wt% OMMT and 5wt% nano-HAP-ZrO2 into 90wt% CTS matrix provides maximum tensile strength, storage modulus, aqueous swelling and cytocompatibility along with strong antibacterial effect, pH and erythrocyte compatibility. Copyright © 2016 Elsevier Ltd. All rights reserved.

  17. Biocompatibility study of lithium disilicate and zirconium oxide ceramics for esthetic dental abutments

    Science.gov (United States)

    2016-01-01

    Purpose The increasing demand for esthetically pleasing results has contributed to the use of ceramics for dental implant abutments. The aim of this study was to compare the biological response of epithelial tissue cultivated on lithium disilicate (LS2) and zirconium oxide (ZrO2) ceramics. Understanding the relevant physicochemical and mechanical properties of these ceramics will help identify the optimal material for facilitating gingival wound closure. Methods Both biomaterials were prepared with 2 different surface treatments: raw and polished. Their physicochemical characteristics were analyzed by contact angle measurements, scanning white-light interferometry, and scanning electron microscopy. An organotypic culture was then performed using a chicken epithelium model to simulate peri-implant soft tissue. We measured the contact angle, hydrophobicity, and roughness of the materials as well as the tissue behavior at their surfaces (cell migration and cell adhesion). Results The best cell migration was observed on ZrO2 ceramic. Cell adhesion was also drastically lower on the polished ZrO2 ceramic than on both the raw and polished LS2. Evaluating various surface topographies of LS2 showed that increasing surface roughness improved cell adhesion, leading to an increase of up to 13%. Conclusions Our results demonstrate that a biomaterial, here LS2, can be modified using simple surface changes in order to finely modulate soft tissue adhesion. Strong adhesion at the abutment associated with weak migration assists in gingival wound healing. On the same material, polishing can reduce cell adhesion without drastically modifying cell migration. A comparison of LS2 and ZrO2 ceramic showed that LS2 was more conducive to creating varying tissue reactions. Our results can help dental surgeons to choose, especially for esthetic implant abutments, the most appropriate biomaterial as well as the most appropriate surface treatment to use in accordance with specific clinical

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

    International Nuclear Information System (INIS)

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

    2015-01-01

    Highlights: • The nanocomposite HZO-201 was stable under varying solution chemistry. • HZO-201 exhibited preferable phosphate removal over other ubiquitous anions. • Selective sorption mechanism was probed and discussed. • HZO-201 could be regenerated for cyclic use with constant efficiency. - Abstract: In this study, we employed a new nanocomposite adsorbent HZO-201, which featured high stability under varying solution chemistry, for preferable removal of phosphate from synthetic solution and a real effluent. An anion exchange resin (D-201) was employed as the host of HZO-201, where nano-hydrous zirconium oxide (HZO) was encapsulated as the active species. D-201 binds phosphate through nonspecific electrostatic affinity, whereas the loaded HZO nanoparticles capture phosphate through formation of the inner-sphere complexes. Quantitative contribution of both species to phosphate adsorption was predicted based on the double-Langmuir model. Preferable removal of phosphate by HZO-201 was observed in the presence of the competing anions at higher levels (Cl − , NO 3 − , SO 4 2− , HCO 3 − ). Fixed-bed adsorption indicated that the effective volume capacity of a synthetic water (2.0 mg P-PO 4 3− /L) by using HZO-201 was ∼1600 BV in the first run (<0.5 mg P-PO 4 3− /L), comparable to Fe(III)-based nanocomposite HFO-201 (∼1500 BV) and much larger than D-201 (<250 BV). The exhausted HZO-201 can be in situ regenerated by using a binary NaOH–NaCl solution for cyclic runs, whether fed with the synthetic solution or real effluent. In general, HZO-201 is a promising alternative to Fe(III)-based adsorbents for trace phosphate removal from effluent particularly at acidic pH

  19. Zirconium and cast zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Krone, K

    1977-04-01

    A survey is given on the occurence of zirconium, production of Zr sponge and semi-finished products, on physical and mechanical properties, production of Zr cast, composition of the commercial grades and reactor grades qualities, metal cutting, welding, corrosion behavior and use.

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

    Science.gov (United States)

    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 (pzirconium-oxide ceramics. Copyright © 2015 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

  1. Oxidation protection and behavior of in-situ zirconium diboride–silicon carbide coating for carbon/carbon composites

    International Nuclear Information System (INIS)

    Li, Lu; Li, Hejun; Yin, Xuemin; Chu, Yanhui; Chen, Xi; Fu, Qiangang

    2015-01-01

    Highlights: • ZrB 2 –SiC coating was prepared on C/C composite by in-situ reaction. • A two-layered structure was obtained when the coating was oxidized at 1500 °C. • The formation and collapse of bubbles influenced the coating oxidation greatly. • The morphology evolution of oxide scale during oxidation was illuminated. - Abstract: To protect carbon/carbon (C/C) composites against oxidation, zirconium diboride–silicon carbide (ZrB 2 –SiC) coating was prepared by in-situ reaction using ZrC, B 4 C and Si as raw materials. The in-situ ZrB 2 –SiC coated C/C presented good oxidation resistance, whose weight loss was only 0.15% after isothermal oxidation at 1500 °C for 216 h. Microstructure evolution of coating at 1500 °C was studied, revealing a two-layered structure: (1) ZrO 2 (ZrSiO 4 ) embedded in SiO 2 -rich glass, and (2) unaffected ZrB 2 –SiC. The formation and collapse of bubbles influenced the coating oxidation greatly. A model based on the evolution of oxide scale was proposed to explain the failure mechanism of coating

  2. Fundamental aspects of actinide-zirconium pyrochlore oxides: Systematic comparison of the Pu, Am, Cm, Bk and Cf systems

    International Nuclear Information System (INIS)

    Haire, R.G.; Raison, P.E.

    2000-01-01

    Zirconium- and hafnium-based oxide materials have gained attraction for various nuclear applications. These materials have features in common with one of the early, well-publicized inorganic ceramics for immobilizing nuclear waste. Our interests have addressed the fundamental structural and chemical properties of these oxide systems. We pursued both the crystal chemical constraints of the oxide matrices, as well as the importance of the chemistry of the f-elements. By incorporating five actinide elements in our studies, we were able to compare systematically the materials science of these materials with the fundamental chemistry and electronic configurations of these actinides employed. It is expected that this basic information will be useful technologically in the realm of tailor-made materials for different applications

  3. Contribution to the identification of the processes kinetically limiting of the zirconium alloys oxidation; characterization of the oxide films formed at high temperature by solids electrochemistry

    International Nuclear Information System (INIS)

    Vermoyal, J.J.

    2000-06-01

    The corrosion behavior of zirconium alloys used for cladding tubes has been extensively studied under several oxidation conditions (temperature, steam, dry air, oxygen...) in order to clarify the mechanism(s) of oxide growth and breakdown. Oxidation rate is generally assumed to be controlled by oxygen diffusion inwards the oxide layer. Nevertheless, several experimental facts, such as acceleration or inhibition of corrosion rate in coupling conditions, suggest that electrochemical processes are involved as a rate determining step. This work is an attempt to shed light about the rate-limiting-mechanism of two zirconium alloys oxidation: Zircaloy-4 (Zy-4) and Zr-Nb(1%)O(0,13%). Impedance spectroscopy characterizations of oxide films formed in high temperature water and studied in gaseous atmosphere clearly show the difference of electrical properties between the two alloys. The in situ electrochemical and thermogravimetric investigations in gaseous medium, and the polarization effects on oxidation and hydridation of Zr alloys in PWRs conditions indicate that oxygen diffusion can be considered as the limiting kinetic step for Zy-4 oxidation. On the contrary, the acceleration of oxide growth on Zr-Nb(1%)O(0,13%) under anodic polarization in PWRs conditions (360 deg C) suggests that either the electronic conductivity in the oxide or an interfacial process at least partially control the oxidation rate. Catalytic effects observed in gaseous medium when noble metals increase the oxygen reduction rate would tend to corroborate the oxidation control of this alloy by an interfacial mechanism. An electrochemical description and a heterogeneous kinetics approach based on a diffusion-interfacial process as rate determining step are then proposed. (author)

  4. Influence of hydratation on the characteristics of zirconium alloys oxide layers

    Czech Academy of Sciences Publication Activity Database

    Gosmanová, G.; Kraus, I.; Kolega, M.; Vrtílková, V.; Weishauptová, Zuzana

    2008-01-01

    Roč. 54, č. 1 (2008), s. 1576-1580 ISSN 1210-0471 R&D Projects: GA ČR GA106/04/0043 Institutional research plan: CEZ:AV0Z30460519 Keywords : zirconium alloys * corrosion layer * hydrated ZrO2 Subject RIV: JF - Nuclear Energetics

  5. Diagnostic study of the roughness surface effect of zirconium on the third-order nonlinear-optical properties of thin films based on zinc oxide nanomaterials

    Energy Technology Data Exchange (ETDEWEB)

    Bahedi, K., E-mail: bahedikhadija@yahoo.com [Laboratoire Optoelectronique et Physico-chimie des Materiaux Universite Ibn Tofail, Faculte des Sciences BP 133 Kenitra 14000, Maroc (Morocco); Addou, M.; El Jouad, M.; Sofiani, Z.; Alaoui Lamrani, M.; El Habbani, T.; Fellahi, N.; Bayoud, S.; Dghoughi, L. [Laboratoire Optoelectronique et Physico-chimie des Materiaux Universite Ibn Tofail, Faculte des Sciences BP 133 Kenitra 14000, Maroc (Morocco); Sahraoui, B.; Essaidi, Z. [Laboratoire POMA, UMR CNRS 6136, Universite d' Angers 2, Bd Lavoisier, 49045 France (France)

    2009-02-01

    Zinc oxide (ZnO) and zirconium doped zinc oxide (ZnO:Zr) thin films were deposited by reactive chemical pulverization spray pyrolysis technique on heated glass substrates at 500 deg. C using zinc and zirconium chlorides as precursors. Effects of zirconium doping agent and surface roughness on the nonlinear optical properties were investigated in detail using atomic force microscopy (AFM) and third harmonic generation (THG) technique. The best value of nonlinear optical susceptibility {chi}{sup (3)} was obtained from the doped films with less roughness. A strong third order nonlinear optical susceptibility {chi}{sup (3)} = 20.12 x 10{sup -12} (esu) of the studied films was found for the 3% doped sample.

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

    Science.gov (United States)

    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

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

    Directory of Open Access Journals (Sweden)

    Siti Mariah Mohd Yasin

    2014-01-01

    Full Text Available 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.

  8. Titanium and zirconium alloys

    International Nuclear Information System (INIS)

    Pinard Legry, G.

    1994-01-01

    Titanium and zirconium pure and base alloys are protected by an oxide film with anionic vacancies which gives a very good resistance to corrosion in oxidizing medium, in some ph ranges. Results of pitting and crevice corrosion are given for Cl - , Br - , I - ions concentration with temperature and ph dependence, also with oxygenated ions effect. (A.B.). 32 refs., 6 figs., 3 tabs

  9. Corrosion behavior of stainless steel and zirconium in nitric acid containing highly oxidizing species

    International Nuclear Information System (INIS)

    Mayuzumi, Masami; Fujita, Tomonari

    1994-01-01

    Corrosion behavior of 304ELC, 310Nb stainless steels and Zirconium was investigated in the simulated dissolver solution of a reprocessing plant to obtain fundamental data for life prediction. Corrosion of heat transfer surface was also investigated in nitric acid solutions containing Ce ion. The results obtained are as follows: (1) Stainless steels showed intergranular corrosion in the simulated dissolver solution. The corrosion rate increased with time and reached to a constant value after several hundred hours of immersing time. The constant corrosion rate changed depending on potential suggesting that corrosion potential dominates the corrosion process. 310Nb showed superior corrosion resistance to 304ELC. (2) Corrosion rate of stainless steels increased in the heat transfer condition. The causes of corrosion enhancement are estimated to be higher corrosion potential and higher temperature of heat transfer surface. (3) Zirconium showed perfect passivity in all the test conditions employed. (author)

  10. Experimental study of the zirconium alloy oxidation under high pressure of steam and modelling of the mechanisms

    International Nuclear Information System (INIS)

    Dali, Yacoub

    2007-01-01

    The corrosion of the cladding materials used for the fuel rods is one of the limiting factor of their lifetime in light water reactors. In this field, the aim of the nuclear industry is today to increase the time and the number of cycles and to submit the claddings in zirconium alloys to higher corrosive conditions. In this way, new alloys devoted to replace the standard Zircaloy-4, for instance Nb containing alloys, have been recently developed and licensed and show better corrosion resistance. A better understanding of the corrosion mechanisms of the zirconium alloys is necessary to predict the corrosion behaviour of these materials. In this work, the oxidation rate of model alloys of two metallurgic families has been studied in steam in a pressure range between 100 milli-bars and 100 bars. The Zircaloy type alloys contain as alloying elements oxygen and/or tin and/or iron and chromium. For the Zr-Nb family, three niobium contents have been studied, respectively 0.2, 0.4 and 1 weight percent of niobium. Our objectives were to understand the variations of the reactivity between the low pressure and the high pressure range, in quantifying the dependency of the corrosion rate with the steam pressure and the alloying element concentrations. The segregation process of the niobium at the surface has also been studied on the Zr-Nb alloys. During this work, a magnetic suspension thermo-balance has been developed and used to follow in-situ the corrosion rate at high pressure of water vapour. The oxide layers have been characterized by many techniques, macro and micro-photo-electrochemistry, XRD, FEG-SEM, XPS, HR-TEM and SIMS. For the Zircaloy type alloys, we have confirmed the major role of the intermetallic precipitates Zr(Fe,Cr) 2 on the corrosion resistance. Unlike the standard Zircaloy-4, for which the oxidation rate does not depend on the pressure of the water vapour and is thus limited by the vacancy diffusion in the oxide layer, we have shown that the rate of the

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

    Science.gov (United States)

    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 zirconium-oxide-based ceramic CAD/CAM crowns with vertical and horizontal finish line preparations were not different. © 2015 by the American College of Prosthodontists.

  12. Synthesis of amorphous zirconium oxide with luminescent characteristics; Sintesis de oxido de circonio amorfo con caracteristicas luminiscentes

    Energy Technology Data Exchange (ETDEWEB)

    Barrera S, M; Chavez G, M; Soto E, A M; Velasquez O, C; Garcia S, M A; Olvera T, L; Rivera M, T [UAM-I, 09340 Mexico D.F. (Mexico)

    2004-07-01

    It was prepared zirconium oxide, ZrO{sub 2}, by means of hydrolysis-condensation reactions (sol-gel method), using zirconium propoxide, Zr(C{sub 3}H{sub 7}O){sub 4}, as precursor and nitric acid, HNO{sub 3}, as catalyst of the hydrolysis reaction. In this synthesis it was used a molar ratio water-alkoxide, r=n{sub H2O}/n{sub Zr}(C{sub 3}H{sub 7}0){sub 4}, high, similar to 200, so that the hydrolysis happens quickly and the nucleation and growth are completed in very little time. The solid was characterized with Ftir spectrophotometry, Differential thermal analysis (Dta), Thermal gravimetric analysis (T G), X-ray diffraction of powders, Scanning electron microscopy (Sem) and X-ray Dispersion energy (EDX). The ZrO{sub 2} obtained by this way is amorphous even to 300 C and it consists of big aggregates. The amorphous ZrO{sub 2}, presents thermoluminescent behavior, after it was irradiated with UV radiation and beta particles of {sup 90}Sr/{sup 90}Y and it was thermally stimulated. (Author)

  13. Oxygen control in solid fuel fired heating systems with zirconium oxide cells. Iltstyring af fastbraendselsfyrede anlaeg med zirkoniumoxidcelle

    Energy Technology Data Exchange (ETDEWEB)

    Zielke, U.

    1988-10-15

    During the heating season 87-88 the Jutland Technological Institute has carried out investigations of the zirconium oxygen meters of solid fuel heating units. The aim was to investigate whether the combustion of inflammable flue gas components on the surface of the oxygen meter cell is of any importance to the running and emissions of the units. The used zirconium oxide oxygen meters normally measure lower concentrations of oxygen as the paramagnetic comparator of the laboratory. The relative deviation is lowest at coal fired units (5.5% and highest at straw fired units (20%)). At several units there is a clear tendency towards increasing development of CO at an increasing surplus of air. Because of too large a surplus of air, and in consequence of this the formation of CO, the chimney waste of the units is increased by up to 6%. Both the surplus of air and the concentration of CO have been included as long term average values. Especially at the straw fired units, periodically very high concentrations of non-inflammable flue gas components can be found, resulting in an undesirable influence on the environment. The development of improved control systems and regulation equipment is recommended.

  14. Electron effective mass in Sn-doped monoclinic single crystal β-gallium oxide determined by mid-infrared optical Hall effect

    Science.gov (United States)

    Knight, Sean; Mock, Alyssa; Korlacki, Rafał; Darakchieva, Vanya; Monemar, Bo; Kumagai, Yoshinao; Goto, Ken; Higashiwaki, Masataka; Schubert, Mathias

    2018-01-01

    The isotropic average conduction band minimum electron effective mass in Sn-doped monoclinic single crystal β-Ga2O3 is experimentally determined by the mid-infrared optical Hall effect to be (0.284 ± 0.013)m0 combining investigations on (010) and ( 2 ¯01 ) surface cuts. This result falls within the broad range of values predicted by theoretical calculations for undoped β-Ga2O3. The result is also comparable to recent density functional calculations using the Gaussian-attenuation-Perdew-Burke-Ernzerhof hybrid density functional, which predict an average effective mass of 0.267m0. Within our uncertainty limits, we detect no anisotropy for the electron effective mass, which is consistent with most previous theoretical calculations. We discuss upper limits for possible anisotropy of the electron effective mass parameter from our experimental uncertainty limits, and we compare our findings with recent theoretical results.

  15. MOCVD of zirconium oxide from the zirconium guanidinate complex |ZrCp′{2-(iPrN)2CNMe2}2Cl

    NARCIS (Netherlands)

    Blackman, C.S.; Carmalt, C.J.; Moniz, S.J.A.; Potts, S.E.; Davies, H.O.; Pugh, D.C.

    2009-01-01

    Parallel to successful studies into use of [ZrCp'{¿ 2-(iPrN)2CNMe2} 2Cl] as a precursor to the deposition of zirconium carbonitride via CVD the same precursor was utilised for the MOCVD of thin films of ZrO 2 using borosilicate glass substrates. The deposited films were of mixed phase; films

  16. Effect of additions of cerium, lanthanum, and zirconium on the state of plantinum and the activity of aluminoplatinum catalysts for the complete oxidation of hydrocarbons

    International Nuclear Information System (INIS)

    Drozdov, V.A.; Davydov, A.A.; Popovskii, V.V.; Tsyrul'nikov, P.G.

    1986-01-01

    It is shown from an analysis of the diffuse reflectance spectra that additions of cerium, lanthanum or zirconium to aluminoplatinum catalyst stabilize the platinum in an oxidized state. This leads to a change in the specific catalytic activity (SCA) towards the total oxidation of methane and butane. The SCA of modified, reduced samples is greater than the SCA of samples that were calcined in air. This is because of the greater activity of metallic platinum compared to the ionic form

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

    Science.gov (United States)

    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

  18. Quantification of chlorine in zirconium oxide and biological samples by instrumental NAA utilizing PCF of Dhruva reactor

    International Nuclear Information System (INIS)

    Shinde, Amol D.; Reddy, A.V.R.; Acharya, R.; Balaji Rao, Y.

    2012-01-01

    Recently studies on chlorine contents in various samples are being pursued due to its corrosive nature. Chlorine present at trace level in various finished products as well as powder is used as a raw material for production of different types of zircaloys used as structural materials in nuclear technology. As a part of quality assurance program, it is necessary to quantify chlorine accurately with suitable and simple technique. In the present work we have applied instrumental neutron activation analysis (INAA) utilizing its short-lived activation product ( 38 Cl, 37 min, 1642 and 2168 keV) for its estimation. Pneumatic Carrier Facility (PCF) of Dhruva reactor, BARC was used sample irradiation of zirconium oxide dry powder, synthetic wax and IAEA RMs 1515 (Apple leaves) and Lichen 336. (author)

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

    Science.gov (United States)

    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 zirconium on XLPE groups also showed lower (p zirconium groups were compared, no differences were

  20. Modeling of mechanical behavior of quenched zirconium-based nuclear fuel claddings after a high temperature oxidation

    International Nuclear Information System (INIS)

    Cabrera-Salcedo, A.

    2012-01-01

    During the second stage of Loss Of Coolant Accident (LOCA) in Pressurized Water Reactors (PWR) zirconium-based fuel claddings undergo a high temperature oxidation (up to 1200 C), then a water quench. After a single-side steam oxidation followed by a direct quench, the cladding is composed of three layers: an oxide (Zirconia) outer layer (formed at HT), always brittle at Room Temperature (RT), an intermediate oxygen stabilized alpha layer, always brittle at RT, called alpha(O), and an inner 'prior-beta' layer, which is the only layer able to keep some significant Post Quench (PQ) ductility at RT. However, hydrogen absorbed because of service exposure or during the LOCA transient, concentrates in this layer and may leads to its embrittlement. To estimate the PQ mechanical properties of these materials, Ring Compression Tests (RCT) are widely used because of their simplicity. Small sample size makes RCTs advantageous when a comparison with irradiated samples is required. Despite their good reproducibility, these tests are difficult to interpret as they often present two or more load drops on the engineering load-displacement curve. Laboratories disagree about their interpretation. This study proposes an original fracture scenario for a stratified PQ cladding tested by RCT, and its associated FE model. Strong oxygen content gradient effect on layers mechanical properties is taken into account in the model. PQ thermal stresses resulting from water quench of HT oxidized cladding are investigated, as well as progressive damage of three layers during an RCT. The proposed scenario is based on interrupted RCT analysis, post- RCT sample's outer layers observation for damage evaluation, RCTs of prior-beta single-layer rings, and mechanical behavior of especially chemically adjusted samples. The force displacement curves appearance is correctly reproduced using the obtained FE model. The proposed fracture scenario elucidates RCTs of quenched zirconium-based nuclear fuel

  1. Quantum chemical study of the elementary reactions in zirconium oxide atomic layer deposition

    International Nuclear Information System (INIS)

    Widjaja, Yuniarto; Musgrave, Charles B.

    2002-01-01

    Elementary reactions in atomic layer deposition of zirconia using zirconium tetrachloride and water are investigated using the density functional theory. The atomistic mechanisms of the two deposition half cycles on the Zr-OH and Zr-Cl surface sites are investigated. Both half reactions proceed through the formation of stable intermediates, resulting in high barriers for HCl formation. We find that the intermediate stability is lowered as the surface temperature is raised. However, increasing temperature also increases the dissociation free-energy barrier, which in turn results in increased desorption of adsorbed precursors

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

    Science.gov (United States)

    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.

  3. Zirconium oxide-coated sand based batch and column adsorptive removal of arsenic from water: Isotherm, kinetic and thermodynamic studies

    Directory of Open Access Journals (Sweden)

    Saif Ali Chaudhry

    2017-06-01

    Full Text Available This paper reports zirconium oxide-coated sand preparation, characterization by SEM, EDX, XRD, FT-IR and thermoanalytical techniques, and use as an adsorbent for the removal of most toxic form of arsenic, As(III, from aqueous solution in both batch and column methods. Batch experimental parameters such as contact time, concentration, dose of adsorbent, pH of As(III solution and temperature were optimized. The adsorption data was fitted to Langmuir, Freundlich, Temkin and Dubinin-Radushkevich isotherms at 303, 308 and 313 K. The maximum Langmuir monolayer adsorption capacity was found to be 136.98 μg/g at 313 K. Values of ΔH°, ΔG° and ΔS° were found to be −12.90, −8.74 to –8.28 and 0.014 kJ/mol, suggesting exothermic and spontaneous adsorption process with slight increase in entropy. The adsorption process followed pseudo-second order kinetics and was controlled by film diffusion step. The column studies showed that when flow rate was increased from 3.0 to 5.0 mL/min, the arsenic adsorption capacity of ZrOCS increased from 33.104 to 42.231 μg/g and breakthrough, and exhaustion times got reduced reduced. The results indicated that zirconium oxide-coated sand (ZrOCS is an excellent adsorbent for the removal of As(III from water.

  4. On the mechanical effects of a nanocrystallisation treatment for ZrO2 oxide films growing on a zirconium alloy

    International Nuclear Information System (INIS)

    Panicaud, B.; Grosseau-Poussard, J.-L.; Retraint, D.; Guérain, M.; Li, L.

    2013-01-01

    Highlights: ► Raman spectroscopy is performed to determine the stress evolution in a Zr/ZrO 2 system. ► Analytical relations are used to determine material characteristics. ► A specific modelling of the mechanical fields within the oxide is done. ► Relaxation and growth parameters are identified from an inverse method. - Abstract: In the present work, mechanical features are investigated in the case of ZrO 2 thermal oxide films growing on a Zr alloy at the temperature of 550 °C. The effects of a nanocrystallisation treatment on high temperature oxidation of a zirconium alloy are specifically studied. High temperature oxidation is performed in order to show benefits of such a nanocrystallisation on corrosion resistance and its influence on the mechanical fields. Experimental results obtained by Raman spectroscopy give the growth stress evolution in ZrO 2 films. Using a modelling of the system, both asymptotic forms and an optimization procedure are developed to determine the mechanical characteristic parameters of the system.

  5. Experimental study and modeling of high-temperature oxidation and phase transformation of cladding-tubes made in zirconium alloy

    International Nuclear Information System (INIS)

    Mazeres, Benoit

    2013-01-01

    One of the hypothetical accident studied in the field of the safety studies of Pressurized light Water Reactor (PWR) is the Loss-Of-Coolant-Accident (LOCA). In this scenario, zirconium alloy fuel claddings could undergo an important oxidation at high temperature (T≅ 1200 C) in a steam environment. Cladding tubes constitute the first confinement barrier of radioelements and then it is essential that they keep a certain level of ductility after quenching to ensure their integrity. These properties are directly related to the growth kinetics of both the oxide and the αZr(O) phase and also to the oxygen diffusion profile in the cladding tube after the transient. In this context, this work was dedicated to the understanding and the modeling of the both oxidation phenomenon and oxygen diffusion in zirconium based alloys at high temperature. The numerical tool (EKINOX-Zr) used in this thesis is based on a numerical resolution of a diffusion/reaction problem with equilibrium-conditions on three moving boundaries: gas/oxide, oxide/αZr(O), αZr(O)/βZr. EKINOX-Zr kinetics model is coupled with ThermoCalc software and the Zircobase database to take into account the influence of the alloying elements (Sn, Fe, Cr, Nb) but also the influence of hydrogen on the solubility of oxygen. This study focused on two parts of the LOCA scenario: the influence of a pre-oxide layer (formed in-service) and the effects of hydrogen. Thanks to the link between EKINOX-Zr and the thermodynamic database Zircobase, the hydrogen effects on oxygen solubility limit could be considered in the numerical simulations. Thus, simulations could reproduce the oxygen diffusion profiles measured in pre-hydrided samples. The existence of a thick pre-oxide layer on cladding tubes can induce a reduction of this pre-oxide layer before the growth of a high-temperature one during the high temperature dwell under steam. The first simulations performed using the numerical tool EKINOX-Zr showed that this particular

  6. Effect of oxide additives on radiolytic decomposition of zirconium and thorium nitrates

    International Nuclear Information System (INIS)

    Joshi, N.G.; Garg, A.N.; Natarajan, V.; Sastry, M.D.

    1996-01-01

    Gamma ray-induced decomposition of the binary mixtures of zirconium and thorium nitrates with 2.5, 5 and 10 mol% of V 2 O 5 , PbO, ThO 2 , ZrO 2 , and MnO 2 has been studied at different doses up to 260 kGy. Radiation chemical yield G(NO 2 - )-values are enhanced by V 2 O 5 , PbO, and ThO 2 but are decreased by ZrO 2 and MnO 2 . The effect of radiation dose on the G(NO 2 - ) values of the binary mixtures of zirconium nitrate with 10 mol% of As 2 O 3 , CuO, MgO, MoO 3 , PbO, ZnO, V 2 O 5 , ThO 2 , MnO 2 and ZrO 2 has been studied. ESR and TL measurements suggest the formation of radical species which interact with the damage entities to enhance or retard the decomposition of the nitrates. A possible mechanism based on the interaction of radical species has been suggested. (Author)

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

    Science.gov (United States)

    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.

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

    Directory of Open Access Journals (Sweden)

    Qifeng Lu

    2015-07-01

    Full Text Available 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 LaZrOx; (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 × 1012 cm−2 for as-deposited sample to 4.55 × 1012 cm−2 for the 800 °C annealed one. In addition, the leakage current density increase from about 10−6 A/cm2 at Vg = +0.5 V for the as-deposited sample to 10−3 A/cm2 at Vg = +0.5 V for the 900 °C annealed one.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    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 (ZrO_2NPs). 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 770 mV on a GCE. However, MWCNTs/GCE presented an electrocatalytic effect toward the oxidation of terbutaline with a better anodic peak at 660 mV. Furthermore, the electrochemical behavior of terbutaline has greatly been improved at a GCE modified with a composite of MWCNTs and nanoparticles of ZrO_2. The ZrO_2NPs/MWCNTs/GCE exhibited a sharp anodic wave at 645 mV with a large enhancement of the current response for terbutaline. Square wave voltammetry (SWV) was performed for the determination of terbutaline at ZrO_2NPs/MWCNTs/GCE. A linear plot was obtained for the current responses of terbutaline against concentrations in the range of 10–160 nM yielding a detection limit of 2.25 nM (based on 3S_b/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 ZrO_2NPs/MWCNTs/GCE system of great interest for monitoring its therapeutic use. - Graphical abstract: A sensitive determination of terbutaline in pharmaceuticals and urine samples using a composite electrode based on zirconium oxide nanoparticles. Display Omitted - Highlights: • A composite electrode was prepared using nanoparticles of ZrO_2 and MWCNTs. • The ZrO_2NPs/MWCNTs/GCE has greatly improved the voltammetry of terbutaline • The proposed electrode enabled a detection limit of 2.25 nM. • The proposed electrode exhibited good reproducibility and long

  10. Improved Oxidation Resistance of Zirconium Resulting from Addition of Small Amounts of Copper; Amelioration de la Resistance a l'Oxydation du Zirconium par de Faibles Additions de Cuivre; Povyshenie soprotivlyaemosti k okisleniyu tsirkoniya posle dobavlenij nebol'shikh kolichestv medi; Aumento de la Resistencia del Circonio a la Oxidacion por Agregado de Pequenas Cantidades de Cobre

    Energy Technology Data Exchange (ETDEWEB)

    Loriers, H.; Darras, R.; Baque, P. [Centre d' Etudes Nucleaires de Saclay (France)

    1966-02-15

    The authors have tried to explain the process by which the addition of small amounts of copper improves the resistance of zirconium to oxidation by pressurized carbon dioxide between 600 and 700 Degree-Sign C. The resulting alloys, particularly that with 2.5% copper, seem to offer interesting possibilities as cladding or structural materials for the fuel elements of reactors of the heavy water-carbon dioxide type. The corrosion of zirconium by carbon dioxide amounts essentially to oxidation, in which two processes are involved: (1) the building up of a layer of monoclinic zirconia, through which oxygen diffuses by migration of the anionic vacancies: (2) the dissolution and diffusion of oxygen, which penetrates into the metal. The combination of gravimetric data and measurements of the thickness of the oxide layers permits evaluation of the two corresponding diffusion coefficients. This calculation has been extended, by analogy, to the case of binary zirconium-copper alloys with a concentration of copper less than or equal to 4% by weight. Comparison of the results obtained shows that the apparent diffusion coefficient of oxygen in the oxide layer that is formed decreases as the copper content of the alloy in question increases; as regards the apparent diffusion coefficient of the oxygen in the alloy, though this is only slightly modified at 600 Degree-Sign C, at 700 Degree-Sign C it too decreases when the copper content is increased to 2.5%. The improved oxidation resistance associated with slowing down of the diffusion processes results, in particular, in prolongation of parabolic-type kinetics whereas, in the case of non-alloyed zirconium or other alloys, cracking in the oxide layer rapidly leads to linear oxidation kinetics as a result of the phenomenon of peeling. (author) [French] Les auteurs ont cherche a interpreter l'amelioration apportee par de faibles additions de cuivre a la resistance a l'oxydation du zirconium par le gaz carbonique sous pression entre

  11. Corrosion mechanisms of zirconium alloys - study of the initial oxidation kinetics and of the mechanical behaviour of the metal/oxide system

    International Nuclear Information System (INIS)

    Parise, M.

    1996-12-01

    Nuclear fuel claddings are made of zirconium alloys. The conditions of use lead the cladding oxidize outside. The so-formed layers behaves like a thermal barrier and prevents from using oxidized claddings with an oxide thickness larger than 100 μm. The oxidation kinetic is approximately cubic for oxide thicknesses smaller than about 2μm, linear beyond. A kinetic model has been proposed which estimates the post-transition growth rate from the kinetic parameters of the pre-transition state and morphological features of post-transition layers. This work aims at providing the necessary elements to validate this model and studying the layers around the kinetic transition, in order to determine whether the oxidation mechanisms before and after the transition are similar. Thicknesses of the 50 - 500 nm range of the oxide layers are measured by an optical method; pre-transition kinetics are thus precisely determined. The effect of the composition, the thermal treatment and the presence of oxygen in solid solution is studied. The morphological and crystallographic study of the layers show that they exhibit a lot of similarities before and after the kinetic transition. The results concerning the kinetic aspects and the morphology of the post-transition layers point out that the proposed model leads to realistic post-transition growth rates. Furthermore, the kinetic transition corresponds to the appearance of cracks in the oxide layer. The mechanical behaviour of the metal/oxide system has been modelled at different scales. When the specific behaviours of the metal and the oxide are taken into account together with the interface geometry, radial stresses appear, which are high enough to locally open cracks. The appearance and localization of cracks depend on both the interface geometry and the stress distribution in the metal/oxide system. (author)

  12. Porous Silicates Modified with Zirconium Oxide and Sulfate Ions for Alcohol Dehydration Reactions

    Directory of Open Access Journals (Sweden)

    Heriberto Esteban Benito

    2015-01-01

    Full Text Available Porous silicates were synthesized by a nonhydrothermal method, using sodium silicate as a source of silica and cetyltrimethylammonium bromide as a template agent. Catalysts were characterized using thermogravimetric analysis, N2 physisorption, X-ray diffraction, FTIR spectroscopy, pyridine adsorption, potentiometric titration with n-butylamine, scanning electronic microscopy, and transmission electronic microscopy. The surface area of the materials synthesized was greater than 800 m2/g. The introduction of zirconium atoms within the porous silicates increased their acid strength from −42 to 115 mV, while the addition of sulfate ions raised this value to 470 mV. The catalytic activity for the dehydration of alcohols yields conversions of up to 70% for ethanol and 30% for methanol.

  13. Evaluation of a Ductility after High Temperature Oxidation with the Three-Point Bend Test in Zirconium Alloys

    International Nuclear Information System (INIS)

    Jung, Yang Il; Park, Sang Yoon; Park, Jeong Yong; Jeong, Yong Hwan

    2010-01-01

    In a light water reactor, the fuel cladding play an important role of preventing leakage of radioactive materials into the coolant, and thus the mechanical integrity of the cladding should be guaranteed under the conditions of normal and transient operation. In the case of a loss of coolant accident (LOCA), the cladding is subjected to a high temperature oxidation which is finally quenched because of an emergency coolant reflooding into the core. In this situation, the current LOCA criteria consist of five separate requirements: i) peak cladding temperature, ii) maximum cladding oxidation, iii) maximum hydrogen generation, iv) coolable geometry, and v) long-term cooling. The claddings lose their ductility due to the microstructural phase transformation from beta to martensite alpha-prime. and hydrogen up-take after LOCA. Since the reduction in ductility can induce embrittlement of claddings, post-quench ductility is one of the major concerns in transient operation circumstances. For the analysis, usually ring compression test are performed on ring samples cut from the tube to examine the oxidized cladding ductility. However, the test would not be applicable to the platelet samples which are general form of a specimen for developing alloys. As a high burn-up fuel cladding materials, Zircaloys are being replaced by modern zirconium alloys such as ZIRLO, and M5. Korea has also developed a new fuel cladding material HANA (high performance alloy for nuclear application) by the Korea Atomic Energy Research Institute. Because of the different composition of the newer claddings in comparison with the conventional Zircaloy-4, the high temperature oxidation behavior and the ductility after the oxidation would be different, and the properties should be evaluated how much the newer claddings were improved

  14. An X-ray absorption near-edge structure (XANES) study of the Sn L_3 edge in zirconium alloy oxide films formed during autoclave corrosion

    International Nuclear Information System (INIS)

    Hulme, Helen; Baxter, Felicity; Babu, R. Prasath; Denecke, Melissa A.; Gass, Mhairi; Steuwer, Axel; Norén, Katarina; Carlson, Stefan; Preuss, Michael

    2016-01-01

    Highlights: • Characterisation of tin speciation in zirconium alloy metal and oxide films using Sn L_3-XANES. • Chemical environment of tin in Zircaloy-4 and ZIRLO™ oxide films shown to be similar. • Tin in the oxide films is present in both the di- and tetravalent states and oxidises progressively with oxide-layer growth. - Abstract: Application of Sn L_3-XANES to study the oxidation state of alloying additions of tin (1–1.2 wt%) in <2 μm oxide layers formed on nuclear grade zirconium alloy has been demonstrated. Data obtained for metallic and corroded ZIRLO™ (1 wt% Sn) and Zircaloy-4 (1.2 wt% Sn) indicate tin has a similar chemical speciation in both metal alloys but this differs in the oxidised surface layers. By recording XANES at various incident angles to vary the photon penetration depth and amount of the oxide layer probed in the measurement, the authors found evidence that the oxidation of tin progresses with increasing oxide thickness.

  15. Formation of inorganic nanofibers by heat-treatment of poly(vinyl alcohol-zirconium compound hybrid nanofibers

    Directory of Open Access Journals (Sweden)

    Nakane K.

    2013-01-01

    Full Text Available Poly(vinyl alcohol-zirconium compound hybrid nanofibers (precursors were formed by electrospinning employing water as a solvent for the spinning solution. The precursors were converted into oxide (ZrO2, carbide (ZrC or nitride (ZrN nanofibers by heating them in air, Ar or N2 atmospheres. Monoclinic ZrO2 nanofibers with high-specific surface area were obtained by heat-treatment of the precursors in air. ZrC and ZrN nanofibers could be obtained below theoretical temperatures calculated from thermodynamics data.

  16. A monoclinic polymorph of theophylline

    Directory of Open Access Journals (Sweden)

    Shuo Zhang

    2011-12-01

    Full Text Available A monoclinic polymorph of theophylline, C7H8N4O2, has been obtained from a chloroform/methanol mixture by evaporation under ambient conditions. The new polymorph crystallizes with two molecules in the asymmetric unit. The structure features intermolecular N—H...O hydrogen bonds, resulting in the formation of dimers between two crystallographically different molecules; each molecule acts as both donor and acceptor.

  17. Investigation of nano-structured Zirconium oxide film on Ti6Al4V substrate to improve tribological properties prepared by PIII&D

    Energy Technology Data Exchange (ETDEWEB)

    Saleem, Sehrish [Department of Physics, Government College University, Lahore 54000 (Pakistan); Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon (Hong Kong); Ahmad, R., E-mail: ahriaz@gcu.edu.pk [Department of Physics, Government College University, Lahore 54000 (Pakistan); Centre for Advanced Studies in Physics (CASP), Government College University, Lahore 54000 (Pakistan); Ayub, R. [Centre for Advanced Studies in Physics (CASP), Government College University, Lahore 54000 (Pakistan); Ikhlaq, Uzma [Department of Physics, Government College University, Lahore 54000 (Pakistan); Jin, Weihong; Chu, Paul K. [Department of Physics and Materials Science, City University of Hong Kong, Tat Chee Avenue, Kowloon (Hong Kong)

    2017-02-01

    Highlights: • ZrO{sub 2} film was deposited on Ti6Al4V alloy using the plasma immersion ion implantation and deposition at various bias voltage. • The deposited film was characterized by XPS, AFM, Ellipometry, Nano-indentation and Pin-on disk machine. • A dense zirconium oxide film with the maximum thickness 108 nm was formed at maximum applied voltage. • The hardness and wear resistance of film is much higher as compared to the substrate. - Abstract: Plasma immersion ion implantation and deposition (PIII&D) is the most attractive and efficient technique used in the medical field to tailor materials for biomedical applications. In the present study zirconium oxide nano-structured thin films were deposited on surface of Ti6Al4V alloy for bias voltages of 15, 20 and 25 kV. The chemical composition, surface roughness and thickness of deposited films were characterized by the x-ray photoelectron spectroscopy (XPS), atomic force microscope (AFM) and ellipsometry respectively. The XPS results confirm the formation of a dense zirconium oxide film of the treated specimens. AFM results exhibit a smooth film with maximum roughness of about 8.4 nm is formed. The thickness of the film is increased with the increase in bias voltages and is maximum at 25 kV. The effect of bias voltages on wear characteristics was further investigated by pin-on-disk test. It is observed that the friction coefficient is reduced, whereas wear resistance is enhanced and it is found to be maximum at 25 kV compared to the other bias voltages. Nanohardness is improved up to twice compared to untreated specimen at the maximum bias voltage. Therefore, it is concluded that deposition of zirconium oxide using the PIII&D is produced a dense layer on the substrate surface, which can be used as a promising candidate for the improved tribological properties of Ti6Al4V.

  18. Corrosion of zirconium alloys in nuclear reactors: A model for irradiation induced enhancement by local radiolysis in the porous oxide

    Energy Technology Data Exchange (ETDEWEB)

    Lemaignan, C; Salot, R [CEA/DRN/DTP, CENG-SECC, Grenoble (France)

    1997-02-01

    An analysis has been undertaken of the various cases of local enhancement of corrosion rate of zirconium alloys under irradiation. It is observed that in most cases a strong emission of energetic {beta}{sup -} is present leading to a local energy deposition rate higher than the core average. This suggests that the local transient radiolytic oxidizing species produced in the coolant by the {beta}{sup -} particles could contribute to corrosion enhancement, by increasing the local corrosion potential. This process is applicable to the local enhanced corrosion found in front of stainless steels structural parts, due to the contribution of Mn, and in front of Pt inserts or Cu-rich cruds. It explains also the irradiation corrosion enhancement of Cu-Zr alloys. Enhanced corrosion around neutron absorbing material is explained similarly by pair production from conversion of high energy capture photons in the cladding, leading to energetic electrons. The same process was found to be active with other highly ionizing species like {alpha} from Ni-rich alloys and fission products in homogeneous reactors. Due to the changes induced by the irradiation intensity on the concentration of the radiolytic species, the coolant chemistry, that controls the boundary conditions for oxide growth, has to be analyzed with respect to the local value of the energy deposition rate. An analysis has been undertaken which shows that, in a porous media, the water is exposed to a higher intensity than bulk water. This leads to a higher concentration of oxidizing radiolytic species at the root of the cracks of the porous oxide, and increases the corrosion rate under irradiation. This mechanism, deduced from the explanation proposed for localized irradiation enhanced corrosion, can be extended to the whole reactor core, where the general enhancement of Zr alloys corrosion under irradiation could be attributed to the general radiolysis in the porous zirconia. (author). 18 refs, 3 figs, 3 tabs.

  19. Nucleation and growth of oxides on metals with special reference to mild steel and zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Gadiyar, H S [Bhabha Atomic Research Centre, Bombay (India). Metallurgy Div.

    1977-01-01

    The oxidation of metals is a complex phenomenon of metal-gas interface for the understanding of which a multidisciplinary approach is necessary. Some aspects of this phenomena are discussed with reference to oxygen or steam as the oxidant. As a case study, the nucleation of oxide through microstructural characterisation, the kinetics and mechanism involved in the case of oxidation of Zr and its alloys have been examined.

  20. Thick-film effects in the oxidation and hydriding of zirconium alloys

    International Nuclear Information System (INIS)

    Johnson, A.B. Jr.

    1989-08-01

    One of the fundamental discoveries involving radiation effects on the oxidation of Zircaloy in low-oxygen aqueous environments is the influence of thick oxide films. Zircaloy oxidation rates in low-oxygen (hydrogen-rich) coolants initially proceed at relatively low rates, often almost uninfluenced by radiation. Marked upturns in oxidation rate have signaled the onset of radiation effects. The radiation effects appear to correlate with a threshold oxide thickness. Results of the test reactor experiments lead to formulation of the Thick-Film Hypothesis: beyond a threshold oxide thickness, radiolysis of water that infiltrates oxide cracks and pores controls the oxidation rate; radiation creates microenvironments inside the oxide film, producing highly oxidizing conditions, that are no longer suppressed by the coolant-borne hydrogen. Upturns in oxidation rate on high-exposure Zircaloy pressure tubes add confirmatory evidence for the thick-film effect. This paper summarizes the early evidence for thick-film behavior, including oxidation and hydriding trends, updates confirmatory evidence from Zircaloy reactor and fuel assembly components, and highlights other observations from the test reactor series that have potential fundamental significance to explanations of radiation effects on Zircaloy. 23 refs., 10 figs

  1. The surface oxidation kinetics of zirconium-niobium alloys and aα-Fe with prevailing cubical texture

    International Nuclear Information System (INIS)

    Mukhambetov, D.G.; Kargin, D.B.; Chalaya, O. V.; Berber, N.N.

    2002-01-01

    It is known, that the kinetics of oxidation of zirconium at formed heating is characterized by two consecutive stages. At the initial stage the thin protecting film will be derived. The relation of its depth from time h (t) is described predominantly by parabolic law. Some time later there can be a transition to the linear law of oxidation. The time moment divided these areas on the kinetic relation is called as a point of break. The film is formed at the second stage, has a developed grid of pores or cracks, can be flake away and be crumbled by losing its protective properties. At the oxidation of the surface shells of the heat generating elements and the technological channels of atomic boilers both stages are proceeded simultaneously. This phenomenon is called modular corrosion. Its consequences can be dangerous for the equipment. Its mechanism is not clear till now. Similar dependencies h(t), with the break point, beginning from which the thin film is transformed into the thick one were found by us at the oxidation α-Fe with prevailing cubical texture. The task of the work was to study the oxide film growth laws in order to clarify the mechanisms of transition of the thin film into the oxide layer on the α-Fe surface and Zr-Nb alloy modular corrosion emergence. Low-carbonate steel with contents 99.43 % of α-Fe was used as a model object of our research. In the texture of the steel surface planar direction [100] was prevalent. Its part accounted for about 40 %. The isothermal air oxidation was carried out in the interval of 450-500 deg. C . Phase composition of the film was determined with X-ray diffraction. The mathematical treatment of the dependencies h(t) obtained by experiment showed that the kinetics of the film growth can be conditionally divided into 4-stages. The initial stage is described by function logarithmic function, the other stages - by the power mode h n =A n ·t, namely, the second stage - is described by function close to cubical (n≅3

  2. The solubilities and solubility products of zirconium hydroxide and oxide after aging at 278, 313, and 333 K

    Energy Technology Data Exchange (ETDEWEB)

    Kobayashi, Taishi; Uemura, Takuya; Sasaki, Takayuki; Takagi, Ikuji [Kyoto Univ. (Japan). Dept. of Nuclear Engineering; Moriyama, Hirotake [Kyoto Univ. (Japan). Research Reactor Inst.

    2016-07-01

    The solubilities of zirconium hydroxide and oxide after aging at 278, 313, and 333 K were measured at 278, 298, 313, and 333 K in the pH{sub c} range of 0.3-7 in a 0.5 M ionic strength solution of NaClO{sub 4} and HClO{sub 4}. Size distributions of the colloidal species were investigated by ultrafiltration using membranes with different pore sizes, and the solid phases were examined by X-ray diffraction. The apparent solubility of zirconium amorphous hydroxide (Zr(OH){sub 4}(am)), prepared by the oversaturation method, decreased with increasing aging temperature (T{sub a}), and the size distributions obtained after aging at elevated temperatures indicated the growth of the colloidal species. We, therefore, suggested that agglomeration of the colloidal species and dehydration and crystallization of Zr(OH){sub 4}(am) as the solubility-limiting solid phase occurred over the course of aging at elevated temperatures. For sample solutions of the crystalline oxide (ZrO{sub 2}(cr)), the aging temperature had no significant effect on the solubility, but the solubility data at lower temperatures were found to be slightly higher than those at higher temperatures, implying a small fraction of the amorphous components. In the analysis of different solid phases (Zr(OH){sub 4}(s,T{sub a}), T{sub a} = 278, 313, and 333 K) depending on the aging temperatures, the solubility products (K{sub sp}, T{sub a}) were determined at different measurement temperatures, and the enthalpy change (Δ{sub r}H {sup circle}) for Zr{sup 4+} 4OH{sup -} <=> Zr(OH){sub 4}(s,T{sub a}) was calculated using the van't Hoff equation. The solid-phase-transformation process at elevated temperatures was also analyzed based on the obtained K{sub sp}, T{sub a} and Δ{sub r}H {sup circle} values.

  3. Zirconium alloy barrier having improved corrosion resistance

    International Nuclear Information System (INIS)

    Adamson, R.B.; Rosenbaum, H.S.

    1983-01-01

    A nuclear fuel element for use in the core of a nuclear reactor has a composite cladding container having a substrate and a dilute zirconium alloy liner bonded to the inside surface of the substrate. The dilute zirconium alloy liner forms about 1 to about 20 percent of the thickness of the cladding and is comprised of zirconium and a metal selected from the group consisting of iron, chromium, iron plus chromium, and copper. The dilute zirconium alloy liner shields the substrate from impurities or fission products from the nuclear fuel material and protects the substrate from stress corrosion and stress cracking. The dilute zirconium alloy liner displays greater corrosion resistance, especially to oxidation by hot water or steam than unalloyed zirconium. The substrate material is selected from conventional cladding materials, and preferably is a zirconium alloy. (author)

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

    Science.gov (United States)

    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.

  5. Articulation of Native Cartilage Against Different Femoral Component Materials. Oxidized Zirconium Damages Cartilage Less Than Cobalt-Chrome.

    Science.gov (United States)

    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.

  6. Zirconium-barrier cladding attributes

    International Nuclear Information System (INIS)

    Rosenbaum, H.S.; Rand, R.A.; Tucker, R.P.; Cheng, B.; Adamson, R.B.; Davies, J.H.; Armijo, J.S.; Wisner, S.B.

    1987-01-01

    This metallurgical study of Zr-barrier fuel cladding evaluates the importance of three salient attributes: (1) metallurgical bond between the zirconium liner and the Zircaloy substrate, (2) liner thickness (roughly 10% of the total cladding wall), and (3) softness (purity). The effect that each of these attributes has on the pellet-cladding interaction (PCI) resistance of the Zr-barrier fuel was studied by a combination of analytical model calculations and laboratory experiments using an expanding mandrel technique. Each of the attributes is shown to contribute to PCI resistance. The effect of the zirconium liner on fuel behavior during off-normal events in which steam comes in contact with the zirconium surface was studied experimentally. Simulations of loss-of-coolant accident (LOCA) showed that the behavior of Zr-barrier cladding is virtually indistinguishable from that of conventional Zircaloy cladding. If steam contacts the zirconium liner surface through a cladding perforation and the fuel rod is operated under normal power conditions, the zirconium liner is oxidized more rapidly than is Zircaloy, but the oxidation rate returns to the rate of Zircaloy oxidation when the oxide phase reaches the zirconium-Zircaloy metallurgical bond

  7. Investigation of strontium and uranium sorption onto zirconium-antimony oxide/polyacrylonitrile (Zr-Sb oxide/PAN) composite using experimental design

    Energy Technology Data Exchange (ETDEWEB)

    Cakir, Pelin; Inan, Suleyman, E-mail: suleyman.inan@ege.edu.tr; Altas, Yuksel

    2014-04-01

    Highlights: • We model Sr{sup 2+} and UO{sub 2}{sup 2+} sorption onto Zr-Sb oxide/PAN composite. • Central composite design was separately employed for Sr{sup 2+} and UO{sub 2}{sup 2+} sorption. • The model F values indicate that both models are statistically significant. • All of the single factors were determined as significant for the sorption of Sr{sup 2+} and UO{sub 2}{sup 2+}. • Zr-Sb oxide/PAN can be used effectively for Sr{sup 2+} and UO{sub 2}{sup 2+} removal from acidic solutions. - Abstract: A study on the sorption of strontium (Sr{sup 2+}) and uranium (UO{sub 2}{sup 2+}) onto zirconium-antimony oxide/PAN (Zr-Sb oxide/PAN) composite was conducted. The zirconium-antimony oxide was synthesized and was then turned into composite spheres by mixing it with polyacrylonitrile (PAN). The single and combined effects of independent variables such as initial pH, temperature, initial ion concentration and contact time on the sorption of Sr{sup 2+} and UO{sub 2}{sup 2+} were separately analyzed using response surface methodology (RSM). Central composite design (CCD) was separately employed for Sr{sup 2+} and UO{sub 2}{sup 2+} sorption. Analysis of variance (ANOVA) revealed that all of the single effects found statistically significant on the sorption of Sr{sup 2+} and UO{sub 2}{sup 2+}. Probability F-values (F = 2.45 × 10{sup −08} and F = 9.63 × 10{sup −12} for Sr{sup 2+} and UO{sub 2}{sup 2+}, respectively) and correlation coefficients (R{sup 2} = 0.96 for Sr{sup 2+} and R{sup 2} = 0.98 for UO{sub 2}{sup 2+}) indicate that both models fit the experimental data well. At optimum sorption conditions Sr{sup 2+} and UO{sub 2}{sup 2+} sorption capacities of the composite were found as 39.78 and 60.66 mg/g, respectively. Sorption isotherm data pointed out that Langmuir model is more suitable for the Sr{sup 2+} sorption, whereas the sorption of UO{sub 2}{sup 2+} was correlated well with the Langmuir and Freundlich models. Thermodynamic parameters such as

  8. The Retentive Strength of Cemented Zirconium Oxide Crowns after Dentin Pretreatment with Desensitizing Paste Containing 8% Arginine and Calcium Carbonate

    Science.gov (United States)

    Pilo, Raphael; Harel, Noga; Nissan, Joseph; Levartovsky, Shifra

    2016-01-01

    The effect of dentin pretreatment with Desensitizing Paste containing 8% arginine and calcium carbonate on the retention of zirconium oxide (Y-TZP) crowns was tested. Forty molar teeth were mounted and prepared using a standardized protocol. Y-TZP crowns were produced using computer-aided design and computer-aided manufacturing (CAD-CAM) technology. The 40 prepared teeth were either pretreated with Desensitizing Paste or not pretreated. After two weeks, each group was subdivided into two groups, cemented with either Resin Modified Glass Ionomer Cement (RMGIC) or Self Adhesive Resin Cement (SARC)). Prior to cementation, the surface areas of the prepared teeth were measured. After aging, the cemented crown-tooth assemblies were tested for retentive strength using a universal testing machine. The debonded surfaces of the teeth and crowns were examined microscopically at 10× magnification. Pretreating the dentin surfaces with Desensitizing Paste prior to cementation did not affect the retention of the Y-TZP crowns. The retentive values for RMGIC (3.04 ± 0.77 MPa) were significantly higher than those for SARC (2.28 ± 0.58 MPa). The predominant failure modes for the RMGIC and SARC were adhesive cement-dentin and adhesive cement-crown, respectively. An 8.0% arginine and calcium carbonate in-office desensitizing paste can be safely used to reduce post-cementation sensitivity without reducing the retentive strength of Y-TZP crowns. PMID:27023532

  9. The Retentive Strength of Cemented Zirconium Oxide Crowns after Dentin Pretreatment with Desensitizing Paste Containing 8% Arginine and Calcium Carbonate

    Directory of Open Access Journals (Sweden)

    Raphael Pilo

    2016-03-01

    Full Text Available The effect of dentin pretreatment with Desensitizing Paste containing 8% arginine and calcium carbonate on the retention of zirconium oxide (Y-TZP crowns was tested. Forty molar teeth were mounted and prepared using a standardized protocol. Y-TZP crowns were produced using computer-aided design and computer-aided manufacturing (CAD-CAM technology. The 40 prepared teeth were either pretreated with Desensitizing Paste or not pretreated. After two weeks, each group was subdivided into two groups, cemented with either Resin Modified Glass Ionomer Cement (RMGIC or Self Adhesive Resin Cement (SARC. Prior to cementation, the surface areas of the prepared teeth were measured. After aging, the cemented crown-tooth assemblies were tested for retentive strength using a universal testing machine. The debonded surfaces of the teeth and crowns were examined microscopically at 10× magnification. Pretreating the dentin surfaces with Desensitizing Paste prior to cementation did not affect the retention of the Y-TZP crowns. The retentive values for RMGIC (3.04 ± 0.77 MPa were significantly higher than those for SARC (2.28 ± 0.58 MPa. The predominant failure modes for the RMGIC and SARC were adhesive cement-dentin and adhesive cement-crown, respectively. An 8.0% arginine and calcium carbonate in-office desensitizing paste can be safely used to reduce post-cementation sensitivity without reducing the retentive strength of Y-TZP crowns.

  10. Synthesis of hydrous zirconium oxide-impregnated chitosan beads and their application for removal of fluoride and lead

    Energy Technology Data Exchange (ETDEWEB)

    Cho, Dong-Wan [Department of Environment and Energy, Sejong University, Seoul 143-747 (Korea, Republic of); Jeon, Byong-Hun, E-mail: bhjeon@hanyang.ac.kr [Department of Natural Resources and Environmental Engineering, Hanyang University, 222 6 Wangsimni-ro, Seongdong-gu, Seoul, 133-791 (Korea, Republic of); Jeong, Yoojin [Department of Environment and Energy, Sejong University, Seoul 143-747 (Korea, Republic of); Nam, In-Hyun [Geologic Environment Division, Korea Institute of Geoscience and Mineral Resources (KIGAM), Daejeon (Korea, Republic of); Choi, Ui-Kyu [Mine reclamation corporation, Coal Center, 2 Segye-ro, Wonju, Gangwon-do, 16464 (Korea, Republic of); Kumar, Rahul [Department of Natural Resources and Environmental Engineering, Hanyang University, 222 6 Wangsimni-ro, Seongdong-gu, Seoul, 133-791 (Korea, Republic of); Song, Hocheol, E-mail: hcsong@sejong.ac.kr [Department of Environment and Energy, Sejong University, Seoul 143-747 (Korea, Republic of)

    2016-05-30

    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 m{sup 2} g{sup −1}) with irregular cracks caused by HZO inclusion and amine functional groups. The rate of Pb{sup 2+} adsorption by HZOCB was relatively rapid. Most of Pb{sup 2+} (89%) was adsorbed within 2.5 h. A binary sorbate system was noticeably favorable for F{sup −} adsorption as compared to single sorbate system. Adsorption of F{sup −} and Pb{sup 2+} followed pseudo-second order kinetics. The maximum sorption capacities obtained from Langmuir isotherm model were 22.1 and 222.2 mg g{sup −1}, respectively. The study demonstrates that the developed composite could be a potential adsorbent for the simultaneous remediation of F{sup −} and Pb{sup 2+} contamination in water.

  11. Continuous precipitation of mineral products: influence of mixing conditions on the co-precipitation of cerium-zirconium mixed oxides

    International Nuclear Information System (INIS)

    Di Patrizio, Nicolas

    2015-01-01

    An automated experimental set-up with rapid mixers is used to study the influence of mixing conditions on the co-precipitation of cerium-zirconium mixed oxides. The intensity of mixing is controlled by the inlet flow rates of the reacting solutions. An engulfment model is used to estimate a mixing time from the measurement of a segregation index by the Villermaux-Dushman reaction system. Three geometries of Hartridge Roughton mixers are compared. Mixing performance is better when a separate mixing chamber upstream of a narrower outlet pipe is present. A better mixing decreases the maximal reducibility temperature of the material and increases the crystal strains of the particles calcined at 1100 C. This is probably due to a better homogenization of the particles content. The important incorporation of nitrates in the particle at the outlet of the mixers shows precipitation occurs while the mixing process is not finished. This experimental result was confirmed by numerical simulation and an estimation of sur-saturations during the mixing process. (author)

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

    Science.gov (United States)

    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.

  13. Zirconium(IV) oxide: New coating material for nanoresonators for shell-isolated nanoparticle-enhanced Raman spectroscopy

    Science.gov (United States)

    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.

  14. Conversion of actual flue gas CO 2 via cycloaddition to propylene oxide catalyzed by a single-site, recyclable zirconium catalyst

    KAUST Repository

    Kelly, Michael J.

    2017-06-12

    A reusable zirconium-based catalyst for the cycloaddition of CO2 to propylene oxide (PO) was prepared by the surface organometallic chemistry (SOMC) methodology. Accordingly, well-defined amounts of the ZrCl4·(OEt2)2 precursor were grafted on the surface of silica dehydroxylated at 700°C (SiO2-700) and at 200°C (SiO2-200) in order to afford surface coordination compounds with different podality and chemical environment. The identity of the surface complexes was thoroughly investigated by FT-IR, elemental microanalysis and solid state NMR and applied as a recoverable and reusable heterogeneous catalyst for the title reaction using pure CO2 and flue gas samples from a cement factory. The observed catalytic activity for the isolated zirconium complexes is rationalized by means of systematic DFT calculations.

  15. Conversion of actual flue gas CO 2 via cycloaddition to propylene oxide catalyzed by a single-site, recyclable zirconium catalyst

    KAUST Repository

    Kelly, Michael J.; Barthel, Alexander; Maheu, Clement; Sodpiban, Ounjit; Dega, Frank-Blondel; Vummaleti, Sai V.C.; Abou-Hamad, Edy; Pelletier, Jeremie; Cavallo, Luigi; D'Elia, Valerio; Basset, Jean-Marie

    2017-01-01

    A reusable zirconium-based catalyst for the cycloaddition of CO2 to propylene oxide (PO) was prepared by the surface organometallic chemistry (SOMC) methodology. Accordingly, well-defined amounts of the ZrCl4·(OEt2)2 precursor were grafted on the surface of silica dehydroxylated at 700°C (SiO2-700) and at 200°C (SiO2-200) in order to afford surface coordination compounds with different podality and chemical environment. The identity of the surface complexes was thoroughly investigated by FT-IR, elemental microanalysis and solid state NMR and applied as a recoverable and reusable heterogeneous catalyst for the title reaction using pure CO2 and flue gas samples from a cement factory. The observed catalytic activity for the isolated zirconium complexes is rationalized by means of systematic DFT calculations.

  16. A Review of Nanoscale Channel and Gate Engineered FINFETs for VLSI Mixed Signal Applications Using Zirconium-di-Oxide Dielectrics

    Directory of Open Access Journals (Sweden)

    D.Nirmal

    2014-07-01

    Full Text Available In the past, most of the research and development efforts in the area of CMOS and IC’s are oriented towards reducing the power and increasing the gain of the circuits. While focusing the attention on low power and high gain in the device, the materials of the device also been taken into consideration. In the present technology, Computationally intensive devices with low power dissipation and high gain are becoming a critical application domain. Several factors have contributed to this paradigm shift. The primary driving factor being the increase in scale of integration, the chip has to accommodate smaller and faster transistors than their predecessors. During the last decade semiconductor technology has been led by conventional scaling. Scaling, has been aimed towards higher speed, lower power and higher density of the semiconductor devices. However, as scaling approached its physical limits, it has become more difficult and challenging for fabrication industry. Therefore, tremendous research has been carried out to investigate the alternatives, and this led to the introduction of new Nano materials and concepts to overcome the difficulties in the device fabrications. In order to reduce the leakage current and parasitic capacitance in devices, gate oxide high-k dielectric materials are explored. Among the different high-k materials available the nano size Zirconium dioxide material is suggested as an alternate gate oxide material for devices due to its thermal stability and small grain size of material. To meet the requirements of ITRS roadmap 2012, the Multi gate devices are considered to be one of the most promising technologies for the future microelectronics industry due to its excellent immunity to short channel effects and high value of On current. The double gate or multi gate devices provide a better scalability option due to its excellent immunity to short-channel effects. Here the different high-k materials are replaced in different

  17. Influence of cobalt oxide on structure and phase composition of zirconium-containing materials

    International Nuclear Information System (INIS)

    Vladimirova, O.S.; Gruzdev, A.I.; Koposova, Z.L.; Lyutsareva, L.A.

    1986-01-01

    Effect of Co 3 O 4 addition in a quantity from 10 to 90% on microstructure, phase content, lattice parameter and structure of ZrO 2 ceramics spallings stabilized with yttrium oxide, is studied. It is found out that in the process of ceramics synthesis the formation of three-phased heterogeneous system of matrix type occurs. At cobalt oxide content within the range of 10-30% a matrix consist of ZrO 2 base solid solution, at cobalt oxide content from 50 to 90% it is a matrix base, at 40% Co 3 O 4 the regions with both type matrixes exist. Cobalt oxide introduction decreases the sintering temperature without loss in operation indices of heat sensitive ceramics for resistance transducers

  18. Influence of surface treatment on the oxidation behavior of zirconium and zircaloy-4

    International Nuclear Information System (INIS)

    Costa, I.; Ramanathan, L.V.

    1986-01-01

    The influence of fluoride concentration in surface treatment solutions on the oxidation behavior of Zr and Zircaloy-4 in the temperature range 350-760 0 C have been studied by means of thermogravimetric analysis. Two solutions containing different concentrations of hydrofluoric acid have been used for surface treatments, following which surface roughness measurements were also carried out. The influence of fluoride ion concentration on oxidation behavior has been found to be significant at higher temperatures. (Author) [pt

  19. Cathodic cycling effects in the oxide films formed on zirconium alloys type AB2

    International Nuclear Information System (INIS)

    Zerbino, J.O; Visintin, A; Triaca, W

    2003-01-01

    The passive behavior of ZrNi alloys near the rest potential is studied through in situ voltammetry, ellipsometry, and microscopic observation.A significant oxide layer growth is observed in aqueous 1 M KOH during the application of different potential programs currently used in the activation processes of the alloy.The understanding of both the alloy activation process and the hydrogen absorption process is important in the strategies employed for the design of electrodes for nickel metal hydride batteries.The kinetics of the oxide layer formation, under potential cycling in the cathodic region related to the rest potential, plays a significant role in the activation process of metal alloy.Cathodic potential cycling increases the thickness and decreases the compactness of the passive oxide layer.The protonation of the oxide decreases the barrier effect and makes the anodic polarization more effective.Potential cycling gives rise to increasing surface oxidation, hydrogen absorption and hydride formation, and produces the consequent fragmentation of the material mainly through grain limits (J.Solid State Eletrochem. in press)

  20. Glow discharge mass spectrometry study of chemical impurities diffusion in zirconium oxide layers

    International Nuclear Information System (INIS)

    Actis-Dato, L.O.

    2000-02-01

    In the Pressurised Water Reactors (PWR) the primary cooling system is water at 350 deg C and 16 Mpa. In these extreme conditions the corrosion of the out-of-pile components of the reactor and in particular of the Zircaloy cladding containing the nuclear fuel pellets is accelerated. The formation of a growing oxide layer is observed on the elements of the nuclear reactor core. When the thickness of the oxide layer reaches a critical value, problems like structural malfunction and material failure can occur. At this stage the danger of the release of radioactivity in the coolant becomes effective. In this work a glow discharge mass spectrometer is used to study the diffusion of impurities like lithium, zinc and boron in oxide layers growing on Zircaloy samples. After a brief description of the different technique used the preparation and analysis of Zircaloy samples on which oxide layers of different thickness have been produced will be described. The analysis of these samples will allow the determination and evaluation the depth profiles of the impurities absorbed by the oxide. The analysis of the shape of the crater produced during the mass spectrometric analysis will give additional informations on the quality of the results obtained. The technique developed will finally be applied to the study of samples produced during reactor operation under real irradiation conditions. The results obtained show a lithium intake in the oxide layer and confirm the beneficial effect on the corrosion produced by boron. The influence of zinc on the corrosion behaviour of Zircaloy has not been established. The technique developed has also shown interesting capabilities concerning the analysis of irradiated samples. (author)

  1. Oxygen self-diffusion mechanisms in monoclinic Zr O2 revealed and quantified by density functional theory, random walk analysis, and kinetic Monte Carlo calculations

    Science.gov (United States)

    Yang, Jing; Youssef, Mostafa; Yildiz, Bilge

    2018-01-01

    In this work, we quantify oxygen self-diffusion in monoclinic-phase zirconium oxide as a function of temperature and oxygen partial pressure. A migration barrier of each type of oxygen defect was obtained by first-principles calculations. Random walk theory was used to quantify the diffusivities of oxygen interstitials by using the calculated migration barriers. Kinetic Monte Carlo simulations were used to calculate diffusivities of oxygen vacancies by distinguishing the threefold- and fourfold-coordinated lattice oxygen. By combining the equilibrium defect concentrations obtained in our previous work together with the herein calculated diffusivity of each defect species, we present the resulting oxygen self-diffusion coefficients and the corresponding atomistically resolved transport mechanisms. The predicted effective migration barriers and diffusion prefactors are in reasonable agreement with the experimentally reported values. This work provides insights into oxygen diffusion engineering in Zr O2 -related devices and parametrization for continuum transport modeling.

  2. Effect of Zirconium Oxide and Zinc Oxide Nanoparticles on Physicochemical Properties and Antibiofilm Activity of a Calcium Silicate-Based Material

    Science.gov (United States)

    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

  3. Correlation between zirconium oxide impedance and corrosion behavior of Zr-Nb-Sn-Fe-Cu alloys

    International Nuclear Information System (INIS)

    Park, Sang Yoon; Lee, Myung Ho; Choi, Byoung Kwon; Jeong, Yong Hwan; Jung, Youn Ho

    2001-01-01

    To evaluate the correlation of Zr oxide impedance and corrosion behavior of Zr-Nb-Sn-Fe-Cu alloys, the corrosion behavior of the alloys was tested in the autoclave containing 70 ppm LiOH solution at 360 .deg. C. The characteristics of the oxide on the alloys were investigated by using the electrochemical impedance spectrosocpy (EIS) method. The corrosion resistance of the alloys was evaluated from the corrosion rate determined as a function of the concentration of Nb. The equivalent circuit of the oxide was composed on the base of the spectrum from EIS measurements on the oxide layers that had formed at pre-and post-transition regions on the curve of corrosion rate. By using the capacitance characteristics of the equivalent circuit, the thickness of impervious layer, it's electrical resistance and characteristics of space charge layer were evaluated. The corrosion characteristics of the Zr-Nb-Sn-Fe-Cu alloys were successfully explained by applying the EIS test results

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

    Czech Academy of Sciences Publication Activity Database

    Štengl, Václav; Houšková, Vendula; Bakardjieva, Snejana; Murafa, Nataliya; Maříková, Monika; Opluštil, F.; Němec, T.

    2010-01-01

    Roč. 61, č. 11 (2010), s. 1080-1088 ISSN 1044-5803 Institutional research plan: CEZ:AV0Z40320502 Keywords : warfare agents * nano-dispersed oxides * homogeneous hydrolysis Subject RIV: CA - Inorganic Chemistry Impact factor: 1.496, year: 2010

  5. Zirconium and hafnium

    Science.gov (United States)

    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

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

    Science.gov (United States)

    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.

  7. Storage and characterization of the hydrogen in mixed oxides on base of cerium-nickel and zirconium or the aluminium

    International Nuclear Information System (INIS)

    Debeusscher, S.

    2008-12-01

    The mixed oxides based on cerium-nickel and zirconium or aluminium are able to store large quantities of hydrogen, To determine nature, reactivity and properties of hydrogen species (spill-over, direct desorption), the solid were studied by different physicochemical techniques in the dried, calcined and partially reduced states: XRD, porosity, TGA, TPR, TPA, TPD, chemical titration and inelastic neutron scattering (INS). Solids are mainly meso-porous with a common pore size at 4 nm, They are constituted of CeO 2 phase, Ce-Ni or Ce-Ni-Zr solid solution and of Ni(OH) 2 in the dried state and NiO in the calcined state. The Ni species are in various environments and the strong interactions between the cations in solid solution and at different particles interface influence their reducibility and the creation of anionic vacancies. Activation in H 2 in temperature is determining for hydrogen storage in the solid while calcination step is not necessary. INS Analyses evidence that the hydrogen species inserted during treatment in H 2 are H + (OH - ), hydride H - and H * (metallic nickel) species, present in various chemical environments, in particular for hydride species. All kinds of hydrogen species participate to the reaction during the chemical titration in agreement with the proposed hydrogenation mechanism. The study of the adsorption of hydrogen shows that this step is fast and in quantity of the same order as that measured by chemical titration. The direct desorption of H 2 is very low, linked to the presence of hydrogen in interaction with metallic nickel (H *- .). Desorption of water is also observed, in parallel, corresponding to the elimination of groups. The hydride species are not desorbed. These various observations allow connecting hydrogen species properties with their localization in the structure and to model active sites. (author)

  8. Oxidation Behavior of FeCrAl -coated Zirconium Cladding prepared by Laser Coating

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Il-Hyun; Kim, Hyun-Gil; Choi, Byung-Kwan; Park, Jeong-Yong; Koo, Yang-Hyun; Kim, Jin-Seon [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2015-05-15

    From the recent research trends, the ATF cladding concepts for enhanced accident tolerance are divided as follows: Mo-Zr cladding to increase the high temperature strength, cladding coating to increase the high temperature oxidation resistance, FeCrAl alloy and SiC/SiCf material to increase the oxidation resistance and strength at high temperature. To commercialize the ATF cladding concepts, various factors are considered, such as safety under normal and accident conditions, economy for the fuel cycle, and developing development challenges, and schedule. From the proposed concepts, it is known that the cladding coating, FeCrAl alloy, and Zr-Mo claddings are considered as a near/mid-term application, whereas the SiC material is considered as a long-term application. Among them, the benefit of cladding coating on Zr-based alloys is the fuel cycle economy regarding the manufacturing, neutron cross section, and high tritium permeation characteristics. However, the challenge of cladding coating on Zr-based alloys is the lower oxidation resistance and mechanical strength at high-temperature than other concepts. Another important point is the adhesion property between the Zr-based alloy and coating materials. A laser coating method supplied with FeCrAl powders was developed to decrease the high-temperature oxidation rate in a steam environment through a systematic study for various coating parameters, and a FeCrAl-coated Zircaloy-4 cladding tube of 100 mm in length to the axial direction can be successfully manufactured.

  9. Raman and luminescence spectroscopy of zirconium oxide with the use of the MOLE microprobe

    International Nuclear Information System (INIS)

    Doyle, T.E.; Alvarez, J.L.

    1984-01-01

    Raman and luminescence spectroscopy with the use of the MOLE microprobe has been used to characterize ZrO 2 originating from oxidized fuel-rod cladding in nuclear accidents. Micro-Raman analysis of samples from Three Mile Island Unit 2 and the Power Burst Facility identified tetragonal and cubic ZrO 2 . The tetragonal and cubic phases are high-temperature polymorphs of ZrO 2 and provide information about temperatures and hydrogen formation in the TMI-2 core. The data suggest that the tetragonal ZrO 2 in TMI-2 samples was stabilized by a crystallite size effect, whereas cubic ZrO 2 in PBF debris samples was stabilized by impurities. Luminescence was used to differentiate yttria-stabilized ZrO 2 ceramics and oxidized fuel-rod cladding in PBF debris samples. The ZrO 2 ceramics produced strong, sharp luminescence peaks which indicated the presence of titanium and yttria in the ZrO 2 . Oxidized fuel-rod cladding displayed no luminescence

  10. Study of the thermal oxidation of titanium and zirconium under argon ion irradiation in the low MeV range (E = 15 MeV)

    International Nuclear Information System (INIS)

    Do, N.-L.

    2012-01-01

    We have shown that argon ion irradiation between 1 and 15 MeV produces damage on both titanium and zirconium surfaces, taking the form of accelerated oxidation and/or craterization effects, varying as a function of the projectile energy and the annealing atmosphere (temperature and pressure) simulating the environmental conditions of the fuel/cladding interface of PWR fuel rods. Using AFM, we have shown that the titanium and zirconium surface is attacked under light argon ion bombardment at high temperature (up to 500 C) in weakly oxidizing medium (under rarefied dry air pressure ranging from 5,7 10 -5 Pa to 5 10 -3 Pa) for a fixed fluence of about 5 10 14 ions.cm -2 . We observed the formation of nano-metric craters over the whole titanium surface irradiated between 2 and 9 MeV and the whole zirconium surface irradiated at 4 MeV, the characteristics of which vary depending on the temperature and the pressure. In the case of the Ar/Ti couple, the superficial damage efficiency increases when the projectile energy decreases from 9 to 2 MeV. Moreover, whereas the titanium surface seems to be transparent under the 15-MeV ion beam, the zirconium surface exhibits numerous micrometric craters surrounded by a wide halo. The crater characteristics (size and superficial density) differ significantly from that observed both in the low energy range (keV) where the energy losses are controlled by ballistic collisions (Sn) and in the high energy range (MeV - GeV) where the energy losses are controlled by electronic excitations (Se), which was not completely unexpected in this intermediate energy range for which combined Sn - Se stopping power effects are possibly foreseen. Using XPS associated to ionic sputtering, we have shown that there is an irradiation effect on thermal oxidation of titanium, enhanced under the argon ion beam between 2 and 9 MeV, and that there is also an energy effect on the oxide thickness and stoichiometry. The study conducted using Spectroscopic

  11. Dynamically formed hydrous zirconium (IV) oxide-polyelectrolyte membranes. III: Poly(acrylic acid) and substituted poly(acrylic acid) homo, co and terpolymer membranes

    International Nuclear Information System (INIS)

    Van Reenen, A.J.; Sanderson, R.D.

    1989-01-01

    A series of acrylic acid and substituted acrylic acid homo, co and terpolymers was synthesised. These polymers were used as polyelectrolytes in dynamically formed hydrous zirconium (iv) oxide-polyelectrolyte membranes. Substitution of the acrylic acid α-hydrogen was done to increase the number of carboxylic acid groups per monomer unit and to change the acid strength of acrylic acid carboxylic acid group. None of these changes improved the salt rejection of these membranes over that of commercially used poly(acrylic acid). Improvement in rejection was found when a hydrophobic comonomer, vinyl acetate, was used in conjunction with acrylic acid in a copolymer dynamic membrane. 16 refs., 6 figs., 1 tab

  12. Method of separating hafnium from zirconium

    International Nuclear Information System (INIS)

    Megy, J.A.

    1980-01-01

    English. A new anhydrous method was developed for separating zirconium and hafnium, which gives higher separation factors and is more economical than previous methods. A molten phase, comprising a solution of unseparated zirconium and hafnium and a solvent metal, is first prepared. The molten metal phase is contacted with a fused salt phase which includes a zirconium salt. Zirconium and hafnium separation is effected by mutual displacement with hafnium being transported from the molten metal phase to the fused salt phase, while zirconium is transported from the fused salt phase to the molten metal phase. The solvent metal is less electropositive than zirconium. Zinc was chosen as the solvent metal, from a group which also included cadmium, lead, bismuth, copper, and tin. The fused salt phase cations are more electropositive than zirconium and were selected from a group comprising the alkali elements, the alkaline earth elements, the rare earth elements, and aluminum. A portion of the zirconium in the molten metal phase was oxidized by injecting an oxidizing agent, chlorine, to form zirconium tetrachlorid

  13. A thermally robust and thickness independent ferroelectric phase in laminated hafnium zirconium oxide

    Directory of Open Access Journals (Sweden)

    S. Riedel

    2016-09-01

    Full Text Available Ferroelectric properties in hafnium oxide based thin films have recovered the scaling potential for ferroelectric memories due to their ultra-thin-film- and CMOS-compatibility. However, the variety of physical phenomena connected to ferroelectricity allows a wider range of applications for these materials than ferroelectric memory. Especially mixed HfxZr1-xO2 thin films exhibit a broad compositional range of ferroelectric phase stability and provide the possibility to tailor material properties for multiple applications. Here it is shown that the limited thermal stability and thick-film capability of HfxZr1-xO2 can be overcome by a laminated approach using alumina interlayers.

  14. Microarc oxidation discharge types and bio properties of the coating synthesized on zirconium.

    Science.gov (United States)

    Cengiz, Sezgin; Azakli, Yunus; Tarakci, Mehmet; Stanciu, Lia; Gencer, Yucel

    2017-08-01

    This study is an attempt for gaining a better understanding on relationship between microarc oxidation (MAO) coating discharge types and bioactivity of an oxide-based coating synthesized on a Zr substrate. The discharge types and the coating growth mechanism were identified by the examination of the real cross-section image of the coating microstructure. The coating was conducted by using MAO in an electrolyte containing Na 2 SiO 3 , Ca(CH 3 COO) 2 and C 3 H 7 Na 2 O 6 P, for different durations of 2.5, 5, 15, and 30mins. The effect of the process duration on the different discharge model types (Type-A, B, and C) and bioactivity of the coatings were investigated by using X-ray Diffractometry (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy-Energy-Dispersive X-ray spectroscopy measurements (SEM-EDS) and Optical Surface Profilometry (OSP). It was found that the increasing MAO duration resulted in thicker and rougher coatings. The XRD data revealed that all the samples prepared at different process durations contained the t-ZrO 2 (tetragonal zirconia) phase. During the MAO process, non-crystalline hydroxyapatite (HA) formed, which was confirmed from the FTIR data. The surface morphology, the amount and distribution of the features of the coating surface were modified by increasing voltage. The simulated body fluid (SBF) tests showed that the more bioactive surface with more HA crystals formed owing to chemical composition and high surface roughness of the coating. The pore, crack and discharge structures played a key role in apatite nucleation and growth, and provided ingrowth of apatite into discharge channels on the coating surface. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. PROCESS OF DISSOLVING ZIRCONIUM ALLOYS

    Science.gov (United States)

    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.

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

    Science.gov (United States)

    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.

  17. Biocorrosion resistance of coated magnesium alloy by microarc oxidation in electrolyte containing zirconium and calcium salts

    Science.gov (United States)

    Wang, Ya-Ming; Guo, Jun-Wei; Wu, Yun-Feng; Liu, Yan; Cao, Jian-Yun; Zhou, Yu; Jia, De-Chang

    2014-09-01

    The key to use magnesium alloys as suitable biodegradable implants is how to adjust their degradation rates. We report a strategy to prepare biocompatible ceramic coating with improved biocorrosion resistance property on AZ91D alloy by microarc oxidation (MAO) in a silicate-K2ZrF6 solution with and without Ca(H2PO4)2 additives. The microstructure and biocorrosion of coatings were characterized by XRD and SEM, as well as electrochemical and immersion tests in simulated body fluid (SBF). The results show that the coatings are mainly composed of MgO, Mg2SiO4, m-ZrO2 phases, further Ca containing compounds involve the coating by Ca(H2PO4)2 addition in the silicate-K2ZrF6 solution. The corrosion resistance of coated AZ91D alloy is significantly improved compared with the bare one. After immersing in SBF for 28 d, the Si-Zr5-Ca0 coating indicates a best corrosion resistance performance.

  18. Effect of nano-sized cerium-zirconium oxide solid solution on far-infrared emission properties of tourmaline powders

    Science.gov (United States)

    Guo, Bin; Yang, Liqing; Hu, Weijie; Li, Wenlong; Wang, Haojing

    2015-10-01

    Far-infrared functional nanocomposites were prepared by the co-precipitation method using natural tourmaline (XY3Z6Si6O18(BO3)3V3W, where X is Na+, Ca2+, K+, or vacancy; Y is Mg2+, Fe2+, Mn2+, Al3+, Fe3+, Mn3+, Cr3+, Li+, or Ti4+; Z is Al3+, Mg2+, Cr3+, or V3+; V is O2-, OH-; and W is O2-, OH-, or F-) powders, ammonium cerium(IV) nitrate and zirconium(IV) nitrate pentahydrate as raw materials. The reference sample, tourmaline modified with ammonium cerium(IV) nitrate alone was also prepared by a similar precipitation route. The results of Fourier transform infrared spectroscopy show that tourmaline modified with Ce and Zr has a better far-infrared emission property than tourmaline modified with Ce alone. Through characterization by transmission electron microscopy (TEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS), the mechanism for oxygen evolution during the heat process in the two composite materials was systematically studied. The XPS spectra show that Fe3+ ratio inside tourmaline modified with Ce alone can be raised by doping Zr. Moreover, it is showed that there is a higher Ce3+ ratio inside the tourmaline modified with Ce and Zr than tourmaline modified with Ce alone. In addition, XRD results indicate the formation of CeO2 and Ce1-xZrxO2 crystallites during the heat treatment and further TEM observations show they exist as nanoparticles on the surface of tourmaline powders. Based on these results, we attribute the improved far-infrared emission properties of Ce-Zr doped tourmaline to the enhanced unit cell shrinkage of the tourmaline arisen from much more oxidation of Fe2+ to Fe3+ inside the tourmaline caused by the change in the catalyst redox properties of CeO2 brought about by doping with Zr4+. In all samples, tourmaline modified with 7.14 wt.% Ce and 1.86 wt.% Zr calcined at 800∘C for 5 h has the best far-infrared emission property with the maximum emissivity value of 98%.

  19. Effect of zirconium oxide nanoparticles addition on the optical and tensile properties of polymethyl methacrylate denture base material.

    Science.gov (United States)

    Gad, Mohammed M; Abualsaud, Reem; Rahoma, Ahmed; Al-Thobity, Ahmad M; Al-Abidi, Khalid S; Akhtar, Sultan

    2018-01-01

    Polymethyl methacrylate (PMMA) is widely used for the fabrication of removable prostheses. Recently, zirconium oxide nanoparticles (nano-ZrO 2 ) have been added to improve some properties of PMMA, but their effect on the optical properties and tensile strength are neglected. The aim of this study was to investigate the effect of nano-ZrO 2 addition on the translucency and tensile strength of the PMMA denture base material. Eighty specimens (40 dumbbell-shaped and 40 discs) were prepared out of heat-polymerized acrylic resin and divided into four groups per test (n=10). The control group for each test included unreinforced acrylic, while the test groups were reinforced with 2.5, 5, and 7.5 wt% nano-ZrO 2 . Acrylic resin was mixed according to manufacturer's instructions, packed, and processed by conventional method. After polymerization, all specimens were finished, polished, and stored in distilled water at 37°C for 48±2 hours. Tensile strength (MPa) was evaluated using the universal testing machine while the specimens' translucency was examined using a spectrophotometer. Statistical analysis was carried out by SPSS using the paired sample t -test ( p ≤0.05). A scanning electron microscope was used to analyze the morphological changes and topography of the fractured surfaces. This study showed that the mean tensile strength of the PMMA in the test groups of 2.5%NZ, 5%NZ, and 7.5%NZ was significantly higher than the control group. The tensile strength increased significantly after nano-ZrO 2 addition, and the maximum increase seen was in the 7.5%NZ group. The translucency values of the experimental groups were significantly lower than those of the control group. Within the reinforced groups, the 2.5%NZ group had significantly higher translucency values when compared to the 5%NZ and 7.5%NZ groups. The addition of nano-ZrO 2 increased the tensile strength of the denture base acrylic. The increase was directly proportional to the nano-ZrO 2 concentration. The

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

    Science.gov (United States)

    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

  1. Pull-test adhesion measurements of diamondlike carbon films on silicon carbide, silicon nitride, aluminum oxide, and zirconium oxide

    International Nuclear Information System (INIS)

    Erck, R.A.; Nichols, F.A.; Dierks, J.F.

    1994-01-01

    Hydrogenated amorphous carbon or diamondlike carbon (DLC) films were formed by 400 eV methane (CH 4 ) ion bombardment of various smooth and rough ceramics, as well as ceramics coated with a layer of Si or Ti. Adhesion was measured by a bonded-pin method. Excellent adhesion was measured for smooth SiC and Si 3 N 4 , but adhesion of DLC to smooth Al 2 O 3 and ZrO 2 was negligible. The use of a Si bonding interlayer produced good adhesion to all the substrates, but a Ti layer was ineffective due to poor bonding between the DLC film and Ti. Bulk thermodynamic calculations are not directly applicable to bonding at the interface because the interface is two dimensional and the compositions of interfacial phases are generally not known. If the standard enthalpy ΔH degree for the reaction between CH 4 and the substrate material is calculated under the assumption that a carbide phase is produced, a relationship is seen between the reaction enthalpy and the relative adhesion. Large positive enthalpies are associated with poor adhesion; negative or small positive enthalpies are associated with good adhesion. This relation between enthalpy and adhesion was also observed for DLC deposited on Si. The lack of adhesion to the Ti was attributed to inadvertent formation of a surface oxide layer that rendered the enthalpy for the reaction with CH 4 positive

  2. Pull-test adhesion measurements of diamondlike carbon films on silicon carbide, silicon nitride, aluminum oxide, and zirconium oxide

    Energy Technology Data Exchange (ETDEWEB)

    Erck, R.A.; Nichols, F.A. [Argonne National Lab., IL (United States); Dierks, J.F. [North Dakota State Univ., Fargo, ND (United States)

    1993-10-01

    Hydrogenated amorphous carbon films or diamondlike carbon (DLC) films were formed by ion-beam deposition of 400 eV methane (CH{sub 4}) ions on several smooth and rough ceramics, as well as on ceramics coated with a layer of Si and Ti. Adhesion was measured by the pin-pull method. Excellent adhesion was measured for smooth SiC and Si{sub 3}N{sub 4}, but adhesion of DLC to Al{sub 2}O{sub 3} and ZrO{sub 2} was negligible. The use of a Si bonding interlayer produced good adhesion to all the substrates, but a Ti layer was ineffective because bonding between the DLC film and Ti was poor. The presence of surface roughness appeared to greatly increase the measured adhesion in all cases. Bulk thermodynamic calculations are not directly applicable to bonding at the interface. If the standard enthalpy of formation for reaction between CH{sub 4} and substrate is calculated assumpting a carbide or carbon phase is produced, a relation is seen between reaction enthalpy and relative adhesion. Large positive enthalpies are associated with poor adhesion; negative or small positive enthalpies are associated with good adhesion. This relation between enthalpy and adhesion was also observed for DLC deposited on Si. Lack of adhesion to Ti was attributed to inadvertent formation of a surface oxide layer that rendered the enthalpy for reaction with CH{sub 4} strongly positive and similar in magnitude to that for Al{sub 2}O{sub 3} and ZrO{sub 2}.

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

    Science.gov (United States)

    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.

  4. Extractive metallurgy of zirconium--1945 to the present

    International Nuclear Information System (INIS)

    Franklin, D.G.; Adamson, R.B.

    1984-01-01

    Although the history of the reduction of zirconium dates from 1824 and the first ductile zirconium metal was produced in the laboratory in 1914, modern reduction practice was pioneered by the U.S. Bureau of Mines starting in 1945. This paper reviews the history of the extractive metallurgy of zirconium from the early work of W. J. Kroll and co-workers at the Bureau of Mines in Albany, Ore., through the commercial development of the production of reactor-grade zirconium metal which was spurred by the requirements of the Naval Reactor Program and the development of commercial nuclear power. Technical subjects covered include processes for opening the ore, zirconium-hafnium separation, chlorination of zirconium oxide, reduction processes, and electrowinning of zirconium metal. Proposed new processes and process modifications are reviewed

  5. Titanium(IV), zirconium, hafnium and thorium

    International Nuclear Information System (INIS)

    Brown, Paul L.; Ekberg, Christian

    2016-01-01

    Titanium can exist in solution in a number of oxidation states. The titanium(IV) exists in acidic solutions as the oxo-cation, TiO 2+ , rather than Ti 4+ . Zirconium is used in the ceramics industry and in nuclear industry as a cladding material in reactors where its reactivity towards hydrolysis reactions and precipitation of oxides may result in degradation of the cladding. In nature, hafnium is found together with zirconium and as a consequence of the contraction in ionic radii that occurs due to the 4f -electron shell, the ionic radius of hafnium is almost identical to that of zirconium. All isotopes of thorium are radioactive and, as a consequence of it being fertile, thorium is important in the nuclear fuel cycle. The polymeric hydrolysis species that have been reported for thorium are somewhat different to those identified for zirconium and hafnium, although thorium does form the Th 4 (OH) 8 8+ species.

  6. Preparation and characterization of sugar cane bagasse fiber modified with nanoparticles of zirconium oxide; Preparacao e caracterizacao de fibras de bagaco de cana modificadas com nanoparticulas de oxido de zirconio

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, K.C.C. de; Mulinari, D.R.; Voorwald, H.C.J.; Cioffi, M.O.H., E-mail: kcccarvalho@hotmail.com.b [UNESP, Guaratingueta, SP (Brazil). Fac. de Engenharia. Dept. de Materiais e Tecnologia(FEG)

    2010-07-01

    The sugar cane bagasse fiber are renewable materials and have great application potential when used as reinforcement in a polymer matrix to give rise to composite materials and as supports for adsorption of heavy metals. This paper therefore describes the preparation and characterization of bleached and hydrated zirconium oxide modified sugar cane bagasse fiber by conventional precipitation method. Through the technique of electron microscopy we observed the presence of oxide nanoparticles on the fiber surface, proving the efficiency of the conventional precipitation method. With the X-ray diffraction analysis it was determined a decrease of 6.2% in the crystallinity index of modified fibers when compared to the bleached fibers showing the deposition of amorphous zirconium oxide on the fiber surface. (author)

  7. Formation and reduction behaviors of zirconium oxide compounds in LiCl–Li{sub 2}O melt at 923 K

    Energy Technology Data Exchange (ETDEWEB)

    Sakamura, Yoshiharu, E-mail: sakamura@criepi.denken.or.jp [Central Research Institute of Electric Power Industry (CRIEPI), 2-11-1 Iwadokita, Komae-shi, Tokyo 201-8511 (Japan); Iizuka, Masatoshi [Central Research Institute of Electric Power Industry (CRIEPI), 2-11-1 Iwadokita, Komae-shi, Tokyo 201-8511 (Japan); Kitawaki, Shinichi; Nakayoshi, Akira; Kofuji, Hirohide [International Research Institute for Nuclear Decommissioning (IRID), 2-23-1 Nishi-shimbashi, Minato-ku, Tokyo 105-0003 (Japan); Japan Atomic Energy Agency (JAEA), 4-33 Muramatsu, Tokai-mura, Naka-gun, Ibaraki 319-1194 (Japan)

    2015-11-15

    The reduction behaviors of ZrO{sub 2}, Li{sub 2}ZrO{sub 3} and (U,Pu,Zr)O{sub 2} in a LiCl–Li{sub 2}O 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)O{sub 2} with various ZrO{sub 2} contents could be reduced to the metallic form and that part of the zirconium was converted to Li{sub 2}ZrO{sub 3}. Zirconium metal and Li{sub 2}ZrO{sub 3} were obtained by the reduction of ZrO{sub 2}. The reduction of Li{sub 2}ZrO{sub 3} did not proceed even in LiCl containing no Li{sub 2}O. Moreover, the stable chemical forms of the ZrO{sub 2}–Li{sub 2}O complex oxide were investigated as a function of the Li{sub 2}O concentration in LiCl. ZrO{sub 2} was converted to Li{sub 2}ZrO{sub 3} at a Li{sub 2}O concentration of 0.018 wt%. As the Li{sub 2}O concentration was increased, Li{sub 2}ZrO{sub 3} was converted to Li{sub 6}Zr{sub 2}O{sub 7} and then to Li{sub 8}ZrO{sub 6}. It is suggested that the removal of Li{sub 2}ZrO{sub 3} from the reduction product is a key point in the pyrochemical treatment of corium. - Highlights: • The uranium in (U,Pu,Zr)O{sub 2} could be reduced to the metallic form in LiCl–Li{sub 2}O. • Part of the zirconium was converted to Li{sub 2}ZrO{sub 3} during electrolytic reduction. • Li{sub 6}Zr{sub 2}O{sub 7} and Li{sub 8}ZrO{sub 6} formed at high Li{sub 2}O concentrations in LiCl.

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

    Science.gov (United States)

    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.

  9. Cathodic behavior of zirconium in aqueous solutions

    International Nuclear Information System (INIS)

    Hine, F.; Yasuda, M.; Sato, H.

    1977-01-01

    The electrochemical behavior of Zr was studied by polarization measurements. The surface oxide and zirconium hydride formed by cathodic polarization of Zr have been examined by X-ray, SEM, and a hardness tester. Zirconium hydride would form on Zr cathode after the surface oxide is reduced at the potential, which is several hundred mV more noble than the predicted value shown by the Pourbaix diagram. The parameters for the hydrogen evolution reaction on the hydride formed Zr cathode differs from that on the oxide covered surface, which means that hydrogen evolution takes place on both surfaces under a different mechanism, while details are still veiled at present

  10. Electrochemical properties of the hexacyanoferrate(II)–ruthenium(III) complex immobilized on silica gel surface chemically modified with zirconium(IV) oxide

    International Nuclear Information System (INIS)

    Panice, Lucimara B.; Oliveira, Elisangela A. de; Filho, Ricardo A.D. Molin; Oliveira, Daniela P. de; Lazarin, Angélica M.; Andreotti, Elza I.S.; Sernaglia, Rosana L.; Gushikem, Yoshitaka

    2014-01-01

    Highlights: • The cyano-bridged mixed valence ruthenium composite material was synthesized. • This newly synthesized compound was incorporated into a carbon paste electrode. • The electrode did not show significant changes in response after six months of use. • The modified electrode is very stable and reproducible. • The electrode sensor was successfully applied for ascorbic acid determination. - Abstract: The chemically modified silica gel with zirconium(IV) oxide was used to immobilize the [Fe(CN) 6 ] 4− complex ion initially. The reaction of this material with [Ru(edta)H 2 O] − complex ion formed the immobilized cyano-bridged mixed valence ruthenium complex, (≡Zr) 5 [(edta)RuNCFe(CN) 5 ]. This material was incorporated into a carbon paste electrode and, its electrochemical properties were investigated. However, for an ascorbic acid solution, an enhancement of the anodic peak current was detected due to electrocatalytic oxidation. The electrode presented the same response for at least 150 successive measurements, with a good repeatability. The modified electrode is very stable and reproducible. The sensor was applied for ascorbic acid determination in pharmaceutical preparation with success

  11. Modification of structural phase state in superficial layers of fuel tubes made of Zirconium alloys

    International Nuclear Information System (INIS)

    Volkov, N.; Kalin, B.; Pimenov, Y.; Timoshin, S.

    2011-01-01

    The paper presents the results obtained in developing the method for introduction of the required changes into states and properties of outer surface on fuel rod cladding made of zirconium alloys E110 and E635 through irradiation by radial Ar + ion beam with a broad energy spectrum. In particular, the paper demonstrates that ion beam treatment of the claddings surface, at the final stage of their fabrication, can upgrade substantially quality of outer tubular surface after mechanical polishing (the cleaner surface, the lower roughness, removal of technological transversal scratches). In addition, the ion beam irradiation results in higher micro-hardness of the modified layer and in better tribological parameters. Kinetic effects in growth of oxide films were studied for the tubular samples of zirconium alloys after ion-beam treatment (cleaning and polishing by radial Ar + ion beam). Also, corrosion tests of the tubular samples were carried out in water (at 350 0 C) and steam (at 350, 375 and 400 0 C) with duration up to 3000 hours. It was revealed that oxide layer consisting mainly of zirconium dioxide in monoclinic modification was formed on tubular surface after oxidation at 3500 0 C in water or steam. The oxidizing process in the pressurized steam created thicker oxide layer on tubular surface than that in the pressurized water. Experimental data were used to determine optimal conditions for ion-beam treatment of outer fuel tube surface. The tubular samples with the following geometrical parameters were investigated: length - up to 500 mm, diameter - 9,15 mm. Optimal regimes for ion-beam cleaning and polishing of the tubular samples were studied up to the process rate of 1 meter per minute. Within the frames of linear approximation, analytical relationships were derived for time dependent growth of oxide films and used to evaluate thickness of oxide film under test conditions (duration . up to 10000 hours). Thickness of oxide films can cover the range from 6

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

    Science.gov (United States)

    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.

  13. Oxide characterization and hydrogen behaviors of Zr-based alloys

    International Nuclear Information System (INIS)

    Kim, Y. S.; Kim, D. J.; Kwon, S. H.; Lee, H. S.; Oh, S. J.; Yim, B. J.; Son, S. B.; Yun, S. P.

    2006-03-01

    The work scope and contents of the research are as follows : basic properties of zirconium alloys, hydrogen pick-up mechanism of zirconium alloy, effects of hydride on the corrosion behaviors of zirconium alloys, estimation on stress of oxide layer in the zirconium alloy, microstructure and characteristic of oxide in pre-hydrided zirconium alloys

  14. Fluency over the monoclinic zirconia indentation

    International Nuclear Information System (INIS)

    Pereira, A.S.; Jornada, J.A.H. da

    1992-01-01

    It was investigated the environment and the time dependence of the Vickers microhardness of monoclinic zirconia single-crystals. The samples were kept at room temperature and the identifications were performed for different environments (air, toluene and water). An indentation creep process was observed for the samples indented is moist media, indicating for a water activated plastic relaxation mechanism. The possible influence of such effect in the fatigue and phase transformations mechanisms of zirconia based ceramics is discussed. (author)

  15. 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.

    Science.gov (United States)

    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.

  16. In situ oxidation of zirconium binary alloys by environmental SEM and analysis by AFM, FIB, and TEM

    International Nuclear Information System (INIS)

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

    2010-01-01

    Binary Zr-alloys containing 1%Fe and 1% Ni (large precipitates) and 1% Cr and 0.6% Nb (small precipitates), as well as a pure Zr sample were exposed in situ at 130 Pa water vapour pressure at 415 o C in an environmental SEM. The surface topography and composition of each sample was characterised before in situ experiments, during and after oxidation. After oxidation the surface was characterised by SEM and EDS, AFM and TEM combined with EDS. Focused ion beam was used to prepare cross sections of the metal-oxide interface and for the preparation of TEM thin foils. The oxidation behaviour of precipitates for these alloying elements can be characterised into two large families, those which show a rapid oxidation and those which induce a delayed oxidation in comparison with the Zr-matrix. At 415 o C after 1 h of oxidation for Zr1%Fe and Zr1%Ni, the formation of protrusions could be detected at the surface, being related to underlying SPP in the oxide. On Zr1%Cr and Zr0.6%Nb unoxidised SPPs were observed in the oxide, close to the metal-oxide interface. These SPPs were, however, oxidised close to the outer surface of the oxide. The surface roughness was increased for all materials after in situ oxidation, however, only for Zr1%Fe and Zr1%Ni protrusions appeared on the surface during oxidation. It was subsequently demonstrated that these latter correspond to the position of SPPs. For Zr1%Fe the surface roughness increased more than in the other materials and on these protrusions small iron oxide crystals have been observed at the surface. These observations confirm that Fe has a different behaviour compared to the other SPP forming elements, and it diffuses out to the free surface of the material. These alloying elements being the constituents of the commercial alloys (Fe and Cr for Zircaloy-4; Fe, Cr and Ni for Zircaloy-2 and Nb for all Nb-containing alloys), this study allows to separate their individual influence and can allow a subsequent comparison to the behaviour

  17. Method of reducing zirconium

    International Nuclear Information System (INIS)

    Megy, J.A.

    1980-01-01

    A method was developed for making nuclear-grade zirconium from a zirconium compound, which ismore economical than previous methods since it uses aluminum as the reductant metal rather than the more expensive magnesium. A fused salt phase containing the zirconium compound to be reduced is first prepared. The fused salt phase is then contacted with a molten metal phase which contains aluminum and zinc. The reduction is effected by mutual displacment. Aluminum is transported from the molten metal phase to the fused salt phase, replacing zirconium in the salt. Zirconium is transported from the fused salt phase to the molten metal phase. The fused salt phase and the molten metal phase are then separated, and the solvent metal and zirconium are separated by distillation or other means. (DN)

  18. Zirconium Phosphate Supported MOF Nanoplatelets.

    Science.gov (United States)

    Kan, Yuwei; Clearfield, Abraham

    2016-06-06

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

  19. PLUTONIUM-ZIRCONIUM ALLOYS

    Science.gov (United States)

    Schonfeld, F.W.; Waber, J.T.

    1960-08-30

    A series of nuclear reactor fuel alloys consisting of from about 5 to about 50 at.% zirconium (or higher zirconium alloys such as Zircaloy), balance plutonium, and having the structural composition of a plutonium are described. Zirconium is a satisfactory diluent because it alloys readily with plutonium and has desirable nuclear properties. Additional advantages are corrosion resistance, excellent fabrication propenties, an isotropie structure, and initial softness.

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

    Science.gov (United States)

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

    2017-06-27

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

  1. Lithium uptake and the accelerated corrosion of zirconium alloys

    International Nuclear Information System (INIS)

    Ramasubramanian, N.; Precoanin, N.; Ling, V.C.

    1989-01-01

    The corrosion of zirconium alloys in aqueous lithiated solutions is sensitive to the concentration of the alkali and the temperature. In concentrated solutions, >10 -1 M in lithium hydroxide (LiOH) (700-ppm lithium) and at temperatures >573 K, accelerated corrosion occurs at quite an early stage. Our investigations indicate that the accelerated corrosion is caused by the generation of porosity, rather than the dissolution of lithium, in the growing oxide. Specimens of standard Zircaloy-4 fuel cladding and Zr-2.5 wt% Nb pressure tube materials were corroded in lithium hydroxide solutions, 10 -3 to 1 M in concentration, at 589 K. Impedance measurements, polarizations in molten lithium nitrate-lithium hydroxide (LiNO 3 -LiOH) and scanning electron microscopy of the alloy-oxide interface indicated a high level of porosity, right from the initial stages, for oxide films grown in the concentrated solutions. The oxides, when analyzed by atomic absorption spectroscopy, revealed the presence of a few 100 ppm of lithium, too small to account for the accelerated corrosion by a mechanism of solid solution of lithium in zirconia. X-ray powder patterns of the oxides showed peaks for only monoclinic zirconia, but occasionally peaks for LiOH · H 2 O and LiOH were also observed. The counts for lithium, detected by secondary ion mass spectrometry, decreased when specimens cut from the same corroded samples were leached in nitric acid. It is concluded from these observations that a major part of lithium is physically held in the porous oxide. Lithium hydroxide is not completely dissociated in aqueous solutions; with increasing concentration and temperature, an increasingly larger proportion of the alkali remains undissociated. It is suggested that the accelerated corrosion in concentrated solutions is caused by the participation of the undissociated alkali in the reactions occurring on the surfaces of the zirconia crystallites. The undissociated LiOH and hydroxyl ions react at an

  2. High-temperature steam-oxidation behavior of Zr-1Nb-1Sn-0.1Fe cladding tube at temperatures of 800-1000

    International Nuclear Information System (INIS)

    Lee, Cheol Min; Cho, Tae Won; Jeong, Gwan Yoon; Kim, Mi Jin; Kim, Ji Hyeon; Lee, Hee Jae; Sohn, Dong Seong; Mok, Yong Kyoon

    2016-01-01

    To prevent cladding failure, NRC issued a regulation Title 10 § 50.46, which specifies cladding temperature of 1204 .deg. C and 17% ECR should not be exceeded. The fundamental reason of the mechanical degradation of cladding is the formation of the oxide which is brittle. Theoretically, the oxide layer is formed following parabolic rate. However, from many experiments, sub-parabolic rates are often observed. There have been many suggestions so far; chemical and stress gradient across the oxide layer could initiate the sub-parabolic rate, the phase transformation of Zirconium dioxide from tetragonal to monoclinic could be the reason, change of the grain size of Zirconium dioxide could cause the cubic oxidation rate, and there is a suggestion that if electron migration is the major mechanism of the oxide growth, then the subparabolic rate can show up. However, the reason why the sub-parabolic rate appears is still not certain. Another important degradation mechanism is breakaway oxidation. A clear explanation that why the breakaway oxidation appears is still not clear. Most of the people believe the phase transformation of Zirconium dioxide cause instability within the oxide, which causes breakaway oxidation to appear. However, how much effect is caused from the phase transformation is not so sure. In this study, detailed analysis about the oxidation kinetics and the breakaway oxidation of Zr-1Nb-1Sn- 0.1Fe were carried out at temperatures between 800 - 1000 .deg. C.

  3. Determination of hydrogen in zirconium hydride and uranium-zirconium hydride by inert gas exraction-gravimetric method

    International Nuclear Information System (INIS)

    Hoshino, Akira; Iso, Shuichi

    1976-01-01

    An inert gas extraction-gravimetric method has been applied to the determination of hydrogen in zirconium hydride and uranium-zirconium hydride which are used as neutron moderator and fuel of nuclear safety research reactor (NSRR), respectively. The sample in a graphite-enclosed quartz crucible is heated inductively to 1200 0 C for 20 min in a helium stream. Hydrogen liberated from the sample is oxidized to water by copper(I) oxide-copper(II) oxide at 400 0 C, and the water is determined gravimetrically by absorption in anhydrone. The extraction curves of hydrogen for zirconium hydride and uranium-zirconium hydride samples are shown in Figs. 2 and 3. Hydrogen in the samples is extracted quantitatively by heating at (1000 -- 1250) 0 C for (10 -- 40) min. Recoveries of hydrogen in the case of zirconium hydride were examined as follows: a weighed zirconium rod (5 phi x 6 mm, hydrogen -5 Torr. After the chamber was filled with purified hydrogen to 200 Torr, the rod was heated to 400 0 C for 15 h, and again weighed to determine the increase in weight. Hydrogen in the rod was then determined by the proposed method. The results are in excellent agreement with the increase in weight as shown in Table 1. Analytical results of hydrogen in zirconium hydride samples and an uranium-zirconium hydride sample are shown in Table 2. (auth.)

  4. The monoclinic polymorph of dimethylarsinic acid

    Directory of Open Access Journals (Sweden)

    Richard Betz

    2011-08-01

    Full Text Available The title compound, C2H7AsO2 or [As(CH32O(OH], is an organic derivative of arsinic acid, and is also known by its trivial name cacodylic acid. In contrast to the first polymorph (triclinic, space group Poverline{1}, Z = 2, the current study revealed monoclinic symmetry (space group C2/c, Z = 8 for the second polymorph. The configuration of the tetrahedral molecule shows approximate Cs symmetry. Strong O—H...O hydrogen bonds connect the molecules to infinite zigzag chains along [010], which are further connected by weak intermolecular C—H...O contacts into a three-dimensional network.

  5. Influence of cerium, zirconium and boron on the oxidation resistance of heat-resistant steels in air

    International Nuclear Information System (INIS)

    Gala, A.; Schendler, W.

    1981-01-01

    Isothermal and cyclic oxidation experiments were carried out in air to investigate the influence of the minor elements such as Cerium, Zirkonium and Boron on the oxidation resistance of heat resistant ferritic and austenitic steels like X10Cr18, X10CrAl18 and X15CrNiSi2012. In the case of cyclicexperiments samples were exposed at constant temperatures for 100 h and then cooled to R.T. This cycle was repeated 10 times. The corrosion was determined as weight change and was continuously measured by a thermo-balance. The distribution of the alloying elements on the phase boundary scale/steel was examined by Scanning-Electron-Microscope. Addition of small amounts of Ce (0.3 wt-% max.) could reduce the oxidation rate in the case of isothermal and cyclic conditions. Zirkonium concentrations below 0.1 wt-% could have a beneficial effect, but at higher concentrations the oxidation rate increases with increasing amounts of Zr. Small Boron concentrations of 0.02 wt-% lead to catastrophic oxidation at temperatures above 1000 0 C. (orig.) [de

  6. Co/Zr substitution in a cerium-zirconium oxide by catalytic steam reforming of bio-ethanol

    International Nuclear Information System (INIS)

    Vargas, J.C.; Thomas, S.; Roger, A.C.; Kiennemann, A.; Vargas, J.C.

    2006-01-01

    This work deals with the production of hydrogen by bio-ethanol catalytic steam reforming. The aim is to develop a catalyst active in ethanol conversion, selective in hydrogen and resistant to deactivation, particularly those induced by the formation of carbon deposition. The metal-support interaction being one of the keys of this challenge, catalysts in which a transition metal is inserted into an oxide by a liquid synthesis method (by the precursor method) have been developed. The initial insertion of cobalt into a cerium oxide-zirconia structure presents the advantages to increase the redox properties of the host oxide and to allow a stable reduction of a cobalt part while favoring the metal-support interaction. (O.M.)

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

    Energy Technology Data Exchange (ETDEWEB)

    Filippov, V. P., E-mail: vpfilippov@mephi.ru; Bateev, A. B.; Lauer, Yu. A. [National Research Nuclear University “MEPhI” (Moscow Engineering Physics Institute) (Russian Federation)

    2016-12-15

    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 {sub 2}O{sub 3} and Fe {sub 3}O{sub 4} 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.

  8. Thermofluency in zirconium alloys

    International Nuclear Information System (INIS)

    Orozco M, E.A.

    1976-01-01

    A summary is presented about the theoretical and experimental results obtained at present in thermofluency under radiation in zirconium alloys. The phenomenon of thermofluency is presented in a general form, underlining the thermofluency at high temperature because this phenomenon is similar to the thermofluency under radiation, which ocurrs in zirconium alloys into the operating reactor. (author)

  9. Determination of impurities in zirconium by emission spectrograph method

    International Nuclear Information System (INIS)

    Simbolon, S.; Masduki, B.; Aryadi

    2000-01-01

    Analysis of B, Cd, Si and Cr elements in zirconium oxide was carried out. Zirconium oxide was made by precipitating zirconium solution with oxalic acid and calcination was at temperature 900 oC for four hours. Silver chloride compound as much as 10% was used as a distillation carrier and 7 step filtration was used to reduce the impurities element spectra having high density. It was found that B concentration is between 3.80 and 7.44 ppm, Cd less then 0.5 ppm, Si between 74.38-150.33 ppm and Cr between 19.90-45.76 ppm. (author)

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

    Science.gov (United States)

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

    2016-10-01

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

  11. Multiwall carbon nanotube- zirconium oxide nanocomposite hollow fiber solid phase microextraction for determination of polyaromatic hydrocarbons in water, coffee and tea samples.

    Science.gov (United States)

    Yazdi, Mahnaz Nozohour; Yamini, Yadollah; Asiabi, Hamid

    2018-06-15

    The purpose of this study was to evaluate the application of hollow fiber solid-phase microextraction (HF-SPME) followed by HPLC-UV to determine the ultra-trace amounts of polycyclic aromatic hydrocarbons (PAHs) as model analytes in complex coffee and tea samples. HF-SPME can be effectively used as an alternative to the direct immersion SPME (DI-SPME) method in complex matrices. The DI-SPME method suffers from serious limitation in dirty and complicated matrices with low sample clean-up, while the HF-SPME method has high clean-up and selectivity due to the high porosity of hollow fiber that can pick out analyte from complicated matrices. As a hollow fiber sorbent, a novel multiwall carbon nanotube/zirconium oxide nanocomposite (MWCNT/ZrO 2 ) was fabricated. The excellent adsorption of PAHs on the sorbent was attributed to the dominant roles of π-π stacking interaction and hydrophobic interaction. Under the optimized extraction conditions, the wide linear range of 0.1-200 μg L -1 with coefficients of determination better than 0.998 and low detection limits of 0.033-0.16 μg L -1 with satisfactory precision (RSD tea samples were in the range of 92.0-106.0%. Compared to other methods, MWCNT/ZrO 2 hollow fiber solid phase microextraction demonstrated a good capability for determination of PAHs in complex coffee and tea samples. Copyright © 2018 Elsevier B.V. All rights reserved.

  12. Study of top reflooding in case of severe accident and in particular oxidation of Uranium, Zirconium, Oxygen melts

    International Nuclear Information System (INIS)

    Brunet-Thibault, E.

    2006-12-01

    In 1979, the Three Mile Island (TMI) accident occurred in United States and accelerated research activities in the field of severe accidents. Severe accident management procedures imply massive water injections to flood the core. The work of this thesis bent principally over this reflooding. The first part of the study concerns the core oxidation enhancement during the reflooding phase which leads to a rough increase of the concentration of burnable hydrogen in the containment. This is why the study carried on the analysis of the contribution of the oxidation of U-Zr-O mixtures, towards the total production of hydrogen during reflooding. In the second part, the study concerns top flooding modelling i.e.: with injection of water in the hot legs. Here, we attempted to define bases and realize a model allowing to describe this type of reflooding. These models were validated on the simulation of the parameter with MAAP4 code. (author)

  13. Corrosion resistance of zirconium in nitric acid

    International Nuclear Information System (INIS)

    Kajimura, H.; Morikawa, H.; Nagano, H.

    1987-01-01

    Slow strain rate tests are effected on zirconium in boiling nitric acid to study the influence of nitric acid concentration, of oxidizing ions (Cr and Ce) and of electric potential. Corrosion resistance is excellent and stress corrosion cracking occurs only for severe conditions: 350 mV over electric potential for corrosion with nitric acid concentration of 40 % [fr

  14. Interactions of NO{sub 2} at ambient temperature with cerium-zirconium mixed oxides supported on SBA-15

    Energy Technology Data Exchange (ETDEWEB)

    Levasseur, Benoit; Ebrahim, Amani M. [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States); Burress, Jacob [NIST Center for Neutron Research, National Institute of Standards and Technology 100 Bureau Drive, Gaithersburg, MD 20899 (United States); Bandosz, Teresa J., E-mail: tbandosz@ccny.cuny.edu [The City College of New York and The Graduate School of CUNY 160 Convent Ave, New York, NY 10031 (United States)

    2011-12-15

    Highlights: Black-Right-Pointing-Pointer Ce{sub 1-y}Zr{sub y}O{sub 2-x} mixed oxides were highly dispersed in mesoporous silica SBA-15. Black-Right-Pointing-Pointer A strong increase in the NO{sub 2} adsorption capacity was observed on composites. Black-Right-Pointing-Pointer The insertion of Zr{sup 4+} in ceria fluorite structure promotes the reduction of Ce{sup 4+} into Ce{sup 3+}. Black-Right-Pointing-Pointer Ce{sup 3+} and -OH groups were found to be the main active centers for NO{sub x} retention. Black-Right-Pointing-Pointer The structure remains quite stable after exposure to NO{sub 2} in ambient conditions. - Abstract: New silica-based composites were obtained using a slow precipitation of mixed oxide Ce{sub 1-x}Zr{sub x}O{sub 2} on the surface of mesoporous silica, SBA-15. The samples were tested as NO{sub 2} adsorbents in dynamic conditions at room temperature. The surface of the initial and exhausted materials was characterized using N{sub 2} sorption, XRD, TEM, potentiometric titration, and thermal analysis before and after exposure to NO{sub 2}. In comparison with unsupported Ce{sub 1-x}Zr{sub x}O{sub 2} mixed oxides, a significant increase in the NO{sub 2} adsorption capacity was observed. This is due to the high dispersion of active oxide phase on the surface of SBA-15. A linear trend was found between the NO{sub 2} adsorption capacity and the amount of Zr(OH){sub 4} added to the structure. Introduction of Zr{sup 4+} cations to ceria contributes to an increase in the amount of Ce{sup 3+}, which is the active center for the NO{sub 2} adsorption, and to an increase in the density of -OH groups. These groups are found to be involved in the retention of both NO{sub 2} and NO on the surface. After exposure to NO{sub 2}, an acidification of the surface caused by the oxidation of the cerium as well as the formation of nitrite and nitrates took place. The structure of the composites appears not to be affected by reactive adsorption of NO{sub 2}.

  15. Electron microscopy of nuclear zirconium alloys

    International Nuclear Information System (INIS)

    Versaci, R.A.; Ipohorski, Miguel

    1986-01-01

    Transmission electron microscopy observations of the microstructure of zirconium alloys used in fuel sheaths of nuclear power reactors are reported. Specimens were observed after different thermal and mechanical treatment, similar to those actually used during fabrication of the sheaths. Electron micrographs and electron diffraction patterns of second phase particles present in zircaloy-2 and zircaloy-4 were also obtained, as well as some characteristic parameters. Images of oxides and hydrides most commonly present in zirconium alloys are also shown. Finally, the structure of a Zr-2,5Nb alloy used in CANDU reactors pressure tubes, is observed by electron microscopy. (Author) [es

  16. Metallurgy of zirconium and hafnium

    International Nuclear Information System (INIS)

    Baryshnikov, N.V.; Geger, V.Eh.; Denisova, N.D.; Kazajn, A.A.; Kozhemyakin, V.A.; Nekhamkin, L.G.; Rodyakin, V.V.; Tsylov, Yu.A.

    1979-01-01

    Considered are those properties of zirconium and of hafnium, which are of practical interest for the manufacture of these elements. Systematized are the theoretical and the practical data on the procedures for thermal decomposition of zirconia and for obtaining zirconium dioxide and hafnium dioxide by a thermal decomposition of compounds and on the hydrometallurgical methods for extracting zirconium and hafnium. Zirconium and hafnium fluorides and chlorides production procedures are described. Considered are the iodide and the electrolytic methods of refining zirconium and hafnium

  17. Experiments on interactions between zirconium-containing melt and water (ZREX). Hydrogen generation and chemical augmentation of energetics

    Energy Technology Data Exchange (ETDEWEB)

    Cho, D.H.; Armstrong, D.R.; Gunther, W.H. [Argonne National Lab., IL (United States); Basu, S.

    1998-01-01

    The results of the first data series of experiments on interactions between zirconium-containing melt and water are described. These experiments involved dropping 1-kg batches of pure zirconium or zirconium-zirconium dioxide mixture melt into a column of water. A total of nine tests were conducted, including four with pure zirconium melt and five with Zr-ZrO{sub 2} mixture melt. Explosions took place only in those tests which were externally triggered. While the extent of zirconium oxidation in the triggered experiments was quite extensive, the estimated explosion energetics were found to be very small compared to the combined thermal and chemical energy available. (author)

  18. Isothermal oxidation behavior of ternary Zr-Nb-Y alloys at high temperature

    Energy Technology Data Exchange (ETDEWEB)

    Prajitno, Djoko Hadi, E-mail: djokohp@batan.go.id [Research Center for Nuclear Materials and Radiometry, Jl. Tamansari 71, Bandung 40132 (Indonesia); Soepriyanto, Syoni; Basuki, Eddy Agus [Metallurgy Engineering, Institute Technology Bandung, Jl. Ganesha 10, Bandung 40132 (Indonesia); Wiryolukito, Slameto [Materials Engineering, Institute Technology Bandung, Jl. Ganesha 10, Bandung 40132 (Indonesia)

    2014-03-24

    The effect of yttrium content on isothermal oxidation behavior of Zr-2,5%Nb-0,5%Y, Zr-2,5%Nb-1%Y Zr-2,5%Nb-1,5%Y alloy at high temperature has been studied. High temperature oxidation carried out at tube furnace in air at 600,700 and 800°C for 1 hour. Optical microscope is used for microstructure characterization of the alloy. Oxidized and un oxidized specimen was characterized by x-ray diffraction. In this study, kinetic oxidation of Zr-2,5%Nb with different Y content at high temperature has also been studied. Characterization by optical microscope showed that microstructure of Zr-Nb-Y alloys relatively unchanged and showed equiaxed microstructure. X-ray diffraction of the alloys depicted that the oxide scale formed during oxidation of zirconium alloys is monoclinic ZrO2 while unoxidised alloy showed two phase α and β phase. SEM-EDS examination shows that depletion of Zr composition took place under the oxide layer. Kinetic rate of oxidation of zirconium alloy showed that increasing oxidation temperature will increase oxidation rate but increasing yttrium content in the alloys will decrease oxidation rate.

  19. Some recent trends in the use of zirconium alloys for nuclear service

    International Nuclear Information System (INIS)

    Balaramamoorthy, K.

    1992-01-01

    Without any exception nuclear power reactors particularly the water cooled ones, operating in the World use natural or slightly enriched uranium oxide fuel pellets with zirconium alloy cladding. While the zirconium alloys have proven to be successful in their designed usage, a desire for longer lifetimes of core components and increased duty cycle puts more demand on materials performance. This demand has led to more in depth studies of phenomena associated with zirconium alloy corrosion mechanism, fine tuning of the zirconium alloy composition, development of fabrication techniques and to the evaluation of newer zirconium alloys for critical applications. (author). 5 refs., 32 figs

  20. 2-(4-Fluorobenzylidenepropanedinitrile: monoclinic polymorph

    Directory of Open Access Journals (Sweden)

    Ahmed M. El-Agrody

    2013-04-01

    Full Text Available The title compound, C10H5FN2, is a monoclinic (P21/c polymorph of the previously reported triclinic (P-1 form [Antipin et al. (2003. J. Mol. Struct. 650, 1–20]. The 13 non-H atoms in the title polymorph are almost coplanar (r.m.s. deviation = 0.020 Å; a small twist between the fluorobenzene and dinitrile groups [C—C—C—C torsion angle = 175.49 (16°] is evident in the triclinic polymorph. In the crystal, C—H...N interactions lead to supramolecular layers parallel to (-101; these are connected by C—F...π interactions.

  1. Techniques for chemical characterization of zirconium and its alloys

    International Nuclear Information System (INIS)

    Iyer, K.V.; Bassan, M.K.T.; Sudersanan, M.

    2002-01-01

    Chemical characterization of zirconium and its alloys such as zircaloy, Zr-Nb, etc for minor and trace constituents like Nb, Ti, Fe, Cr, Ni, Sn, Al etc has been carried out. Zirconium, being a major constituent, has been determined by gravimetry as zirconium oxide while other constituents like Nb, Ti, Fe have been determined by spectrophotometric methods. Other metals of importance at trace level have been estimated by AAS or ICPAES. The judicious use of both conventional and modern instrumental methods of analysis helps in the characterization of zirconium and its alloys for various major and minor constituents. The role of matrix effect in the determination was also investigated and methods have been worked out based on a preliminary separation of zirconium by a hydroxide precipitation. (author)

  2. Determination of microquantities of zirconium and thorium in uranium dioxide

    International Nuclear Information System (INIS)

    Weber de D'Alessio, Ana; Zucal, Raquel.

    1975-07-01

    A method for the determination of 10 to 50 ppm of zirconium and thorium in uranium IV oxide of nuclear purity is established. Zirconium and thorium are retained in a strong cation-exchange resin Dowex 50 WX8 in 1 M HCl. Zirconium is eluted with 0,5% oxalic acid solution and thorium with 4% ammonium oxalate. The colorimetric determination of zirconium with xilenol orange is done in perchloric acid after destructtion of oxalic acid and thorium is determined with arsenazo III in 5 M HCl. 10 μg of each element were determined with a standard deviation of 2,1% for thorium and 3,4% for zirconium. (author) [es

  3. Analysis of hafnium in zirconium alloys

    International Nuclear Information System (INIS)

    Kondo, Isao; Sakai, Fumiaki; Ohuchi, Yoshifusa; Nakamura, Hisashi

    1977-01-01

    It is required to analyse alloying components and impurity elements in the acceptance analysis of zirconium alloys as the material for fuel cladding tubes and pressure tubes for advanced thermal reactors. Because of extreme similarity in chemical properties between zirconium and hafnium, about 100 ppm of hafnium is usually contained in zirconium alloys. Zircaloy-2 alloy and 2.5% Nb-zirconium with the addition of hafnium had been prepared as in-house standard samples for rapid analysis. Study was made on fluorescent X-ray analysis and emission spectral analysis to establish the analytical method. By using these in-house standard samples, acceptance analysis was successfully carried out for the fuel cladding tubes for advanced thermal reactors. Sulfuric acid solution was prepared from JAERI-Z 1, 2 and 3, the standard sample for zircaloy-2 prepared by the Analytical Committee on Nuclear Fuel and Reactor Materials, JAERI, and zirconium oxide (Hf 1 ppm/Zr). Standard Hf solution was added to the sulfuric acid solution step by step, to make up a series of the standard oxide samples by the precipitation process. By the use of these standard samples, the development of the analytical method and joint analysis were made by the three-member analytical technique research group including PNC. The analytical precision for the fluorescent X-ray analysis was improved by attaching a metallic yttrium filter to the window of an X-ray tube so as to suppress the effect due to zirconium matrix. The variation factor of the joint analysis was about 10% to show good agreement, and the indication value was determined. (Kobatake, H.)

  4. SEPARATING HAFNIUM FROM ZIRCONIUM

    Science.gov (United States)

    Lister, B.A.J.; Duncan, J.F.

    1956-08-21

    A dilute aqueous solution of zirconyl chloride which is 1N to 2N in HCl is passed through a column of a cation exchange resin in acid form thereby absorbing both zirconium and associated hafnium impurity in the mesin. The cation exchange material with the absorbate is then eluted with aqueous sulfuric acid of a O.8N to 1.2N strength. The first portion of the eluate contains the zirconium substantially free of hafnium.

  5. Crystallite size effect on the monoclinic deformation of the bcc crystal structure of chromium

    Science.gov (United States)

    Przeniosło, R.; Fabrykiewicz, P.; Sosnowska, I.; Wardecki, D.; Sławiński, W. A.; Playford, H. Y.; Hempelmann, R.; Bukowski, M.

    2018-02-01

    The modulated spin density wave magnetic orderings observed in chromium suggests that the crystal structure of chromium cannot be described by the cubic space group Im 3 bar m. Our experimental studies of polycrystalline and nanocrystalline chromium by synchrotron radiation (SR) and neutron powder diffraction show a hkl-dependent Bragg peak broadening which can be interpreted by the low-symmetry monoclinic space group P21 / n instead of the high symmetry cubic space group Im 3 bar m. The monoclinic angle is βm = 90.05(1)° and 90.29(1)° for polycrystalline Cr and nanocrystalline Cr, respectively. The relative monoclinic distortion observed in chromium is 5 times larger than those reported for several oxides: BiFeO3, α-Fe2O3, Cr2O3 and calcite. The symmetry of the magnetic transverse spin density wave (TSDW) and the longitudinal spin density wave (LSDW) observed in Cr are described by using the superspace groups P21 / n(0 β 0) 00 and P 21‧ /n‧(0 β 0) 00, respectively. These superspace groups describe both the magnetic modulations and the atomic position modulations reported in the literature. The monoclinic symmetry of chromium is a robust effect which is observed in the paramagnetic as well as in the TSDW and LSDW phases.

  6. Comprehensive profiling of ribonucleosides modification by affinity zirconium oxide-silica composite monolithic column online solid-phase microextraction - Mass spectrometry analysis.

    Science.gov (United States)

    Jiang, Han-Peng; Chu, Jie-Mei; Lan, Meng-Dan; Liu, Ping; Yang, Na; Zheng, Fang; Yuan, Bi-Feng; Feng, Yu-Qi

    2016-09-02

    More than 140 modified ribonucleosides have been identified in RNA. Determination of endogenous modified ribonucleosides in biological fluids may serve as non-invasive disease diagnostic strategy. However, detection of the modified ribonucleosides in biological fluids is challenging, especially for the low abundant modified ribonucleosides due to the serious matrix interferences of biological fluids. Here, we developed a facile preparation strategy and successfully synthesized zirconium oxide-silica (ZrO2/SiO2) composite capillary monolithic column that exhibited excellent performance for the selective enrichment of cis-diol-containing compounds. Compared with the boronate-based affinity monolith, the ZrO2/SiO2 monolith showed ∼2 orders of magnitude higher extraction capacity and can be used under physiological pH (pH 6.5-7.5). Using the prepared ZrO2/SiO2 composite monolith as the trapping column and reversed-phase C18 column as the analytical column, we further established an online solid-phase microextraction (SPME) in combination with liquid chromatography-mass spectrometry (online SPME-LC-MS/MS) analysis for the comprehensive profiling of ribonucleosides modification in human urine. Our results showed that 68 cis-diol-containing ribosylated compounds were identified in human urine, which is, to the best of our knowledge, the highest numbers of cis-diol-containing compounds were determined in a single analysis. It is worth noting that four modified ribonucleosides were discovered in the human urine for the first time. In addition, the quantification results from the pooled urine samples showed that compared to healthy controls, the contents of sixteen ribose conjugates in the urine of gastric cancer, eleven in esophagus cancer and seven in lymphoma increased more than two folds. Among these ribose conjugates, four ribose conjugates increased more than two folds in both gastric cancer and esophagus cancer; three ribose conjugates increased more than two

  7. Analysis of the deconvolution of the thermoluminescent curve of the zirconium oxide doped with graphite; Analisis de la deconvolucion de la curva termoluminiscente del oxido de zirconio dopado con grafito

    Energy Technology Data Exchange (ETDEWEB)

    Salas C, P. [IMP, 07000 Mexico D.F. (Mexico); Estrada G, R. [Depto. de Fisica y Matematicas, UIA, Unidad Stanta Fe, 01000 Mexico D.F. (Mexico); Gonzalez M, P.R.; Mendoza A, D. [ININ, A.P. 18-1027, 11801 Mexico D.F. (Mexico)

    2003-07-01

    In this work, we present a mathematical analysis of the behavior of the thermoluminescent curve (Tl) induced by gamma radiation in samples made of zirconium oxide doped with different amounts of graphite. In accordance with the results gamma radiation induces a Tl curve with two maximum of emission localized in the temperatures at 139 and 250 C, the area under the curve is increasing as a function of the time of exposition to the radiation. The analysis of curve deconvolution, in accordance with the theory which indicates that this behavior must be obey a Boltzmann distribution, we found that each one of them has a different growth velocity as the time of exposition increase. In the same way, we observed that after the irradiation was suspended each one of the maximum decrease with different velocity. The behaviour observed in the samples is very interesting because the zirconium oxide has attracted the interest of many research groups, this material has demonstrated to have many applications in thermoluminescent dosimetry and it can be used in the quantification of radiation. (Author)

  8. Preparation of high-purity zirconium dioxide from baddeleyite

    International Nuclear Information System (INIS)

    Voskobojnikov, N.B.; Skiba, G.S.

    1996-01-01

    Interaction of baddeleyite concentrate with calcium oxide and calcium chloride in the process of caking is studied. The influence of grain size on calcium zirconate formation is tested. Conditions for cake leaching by hydrochloric acid and zirconium(4) oxychloride purification from calcium and silicon compounds by recrystallization are reported. Zirconium dioxide corresponding to specifications (6-2 special purity) is obtained with a high (more than 90%) chemical yield. 9 refs., 1 tab

  9. Dielectric properties of zirconium dioxide-based ceramics

    International Nuclear Information System (INIS)

    Vladimirova, O.S.; Gruzdev, A.I.; Koposova, Z.L.; Lyutsareva, L.A.

    1985-01-01

    This paper studies the dielectric properties of materials based on stabilized zirconium dioxide with Co 3 O 4 additions possessing a high temperature-coefficient of resistance. These materials are promising for manufacturing resistance temperature gages that work under an oxidizing atmosphere at 370-1270 degrees K. The obtained results indicate the possibility of developing temperature gases possessing highsensitivity from stabilized zirconium dioxide with Co 3 O 4 additions

  10. Alkylation of isobutane by butenes on zirconium sulfate catalysts

    International Nuclear Information System (INIS)

    Lavrenov, A.V.; Perelevskij, E.V.; Finevich, V.P.; Zajkovskij, V.I.; Paukshtis, E.A.; Duplyakiv, V.K.; Bal'zhinimaev, B.S.

    2003-01-01

    Preparation of applied zirconium sulfate catalysts obtained by the method of impregnation is investigated. Results of comparative study of structural, acid-base and catalytic properties of sulfated zirconium dioxide applied on silica gel and aluminium oxide are represented. Intervals of values of synthesis basic parameters and characteristics of catalysts properties providing achievement of high activity and selectivity in isobutane alkylation by butenes in liquid phase are determined [ru

  11. Phase transformations during machining and properties of surface layers in zirconium dioxide ceramics

    International Nuclear Information System (INIS)

    Grigor'ev, O.N.; Krivoshej, G.S.; Stel'mashenko, N.A.; Trefilov, V.I.; Shevchenko, A.V.

    1991-01-01

    The methods of X-ray allow studying phase composition and inner stresses in the surface layers of partially stabilized zirconium dioxide after mashining. It is shown that under conditions of abrasive treatment transitions from tetragonal into rhomboedric and monoclinic phases initiate. As a result of phase transitions fields of compressible stresses achieving 900 MPa under grinding with ACM abrasive are created on the surface. An essential increase of hardness due to growth of the brittle fauilure resistance and deformation hardening is revealed

  12. One-pot hydrothermal synthesis of zirconium dioxide nanoparticles decorated reduced graphene oxide composite as high performance electrochemical sensing and biosensing platform

    International Nuclear Information System (INIS)

    Teymourian, Hazhir; Salimi, Abdollah; Firoozi, Somayeh; Korani, Aazam; Soltanian, Saied

    2014-01-01

    Graphical abstract: - Highlights: • One pot hydrothermal synthesis used for preparing of ZrO 2 NPs reduced graphene oxide. • Electrocatalytic activity of ZrO 2 /rGO improved in compared to ZrO 2 based C- materials. • ZrO 2 NPs/rGO modified GCE was used for electrocatalytic reduction of O 2 and H 2 O 2 . • ZrO 2 NPs/rGO/GCE shows excellent ability to simultaneous detection of AA,UA and DP. • With immobilization of GOX onto ZrO 2 NPs/rGO a sensitive glucose biosensor fabricated. - Abstract: We report on the synthesis of zirconium dioxide-reduced graphene oxide composite (ZrO 2 -rGO) and its application as a novel architecture for electrochemical sensing and biosensing purposes. ZrO 2 -rGO hybrid is synthesized through a simple one-step hydrothermal route, where the reduction of GO and the in-situ generation of ZrO 2 nanoparticles (NPs) occurred simultaneously. Characterization of the resultant hybrid material using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD) and Raman spectroscopy clearly indicated the homogeneous dispersion of ZrO 2 NPs with particle sizes of ∼5 nm on rGO sheets. The potential application of ZrO 2 -rGO modified glassy carbon electrode (ZrO 2 -rGO/GC) for electroanalytical purposes was demonstrated by using several important electroactive compounds as representative examples (i.e., O 2 , hydrogen peroxide (H 2 O 2 ), glucose, ascorbic acid (AA), dopamine (DA) and uric acid (UA)). Electrochemical control experiments by using different composites of ZrO 2 /graphite, ZrO 2 /Active Carbon and ZrO 2 electrodeposited on activated GC electrode revealed that the ZrO 2 -rGO composite possessed superior electrocatalytic activitiy towards the catalytic reduction of O 2 and H 2 O 2 at more reduced overpotentials. The linear range of H 2 O 2 concentration was from 0.10 to 1340 μM with the detection limit of 20 nM (S/N = 3). Furthermore, via immobilization of glucose oxidase (GOx) enzyme onto the

  13. Zirconium isotope separation process

    International Nuclear Information System (INIS)

    Peterson, S.H.; Lahoda, E.J.

    1988-01-01

    A process is described for reducing the amount of zirconium 91 isotope in zirconium comprising: forming a first solution of (a) a first solvent, (b) a scavenger, and (c) a zirconium compound which is soluble in the first solvent and reacts with the scavenger when exposed to light of a wavelength of 220 to 600 nm; irradiating the first solution with light at the wavelength for a time sufficient to photoreact a disproportionate amount of the zirconium compound containing the zirconium 91 isotope with the scavenger to form a reaction product in the first solution; contacting the first solution, while effecting the irradiation, with a second solvent which is immiscible with the first solvent, which the second solvent is a preferential solvent for the reaction product relative to the first solvent, such that at least a portion of the reaction product is transferred to the second solvent to form a second solution; and separating the second solution from the first solution after the contacting

  14. ZIRCONIUM-CLADDING OF THORIUM

    Science.gov (United States)

    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)

  15. Environmentally Friendly Zirconium Oxide Pretreatment

    Science.gov (United States)

    2013-05-01

    Society for Testing and Materials AVCRAD Aviation Classification Repair Activity Depot Chrome (VI) Hexavalent Chromium CRS Cold Rolled Steel...are being used commercially in automotive and other industrial operations as replacements to hexavalent chromium-based and zinc phosphate...application over CRS and aluminum with water-borne and solvent-borne Mil-Spec primers gave results in corrosion performance similar to the chrome

  16. Photo-, thermo- and optically stimulated luminescence of monoclinic zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Kiisk, Valter, E-mail: valter.kiisk@ut.ee [Institute of Physics, University of Tartu, Ravila 14c, 50411 Tartu (Estonia); Puust, Laurits; Utt, Kathriin; Maaroos, Aarne; Mändar, Hugo [Institute of Physics, University of Tartu, Ravila 14c, 50411 Tartu (Estonia); Viviani, Erica; Piccinelli, Fabio [Department of Biotechnology, University of Verona, Strada Le Grazie 15, 37134 Verona (Italy); Saar, Rando; Joost, Urmas; Sildos, Ilmo [Institute of Physics, University of Tartu, Ravila 14c, 50411 Tartu (Estonia)

    2016-06-15

    We carried out a careful photoluminescence (PL) and thermoluminescence (TL) characterization of nominally pure monoclinic ZrO{sub 2} nanopowders subject to oxidative vs reductive annealing (up to 1450 °C). The two kinds of studied zirconia (sol-gel-prepared vs commercial powder) exhibited virtually identical 490 nm PL emission band and 280 nm PL excitation band with slight, but clearly detectable variations in the spectral shape. The TL glow peaks, recorded over the temperature range −100 to 300 °C, showed an interplay depending on the type and treatment of sample. There is a strong evidence that the −35 and 205 °C glow peaks are due to oxygen vacancies whereas the 5 °C glow peak may relate to oxygen interstitials and the 110 °C glow peak to surface defects. Although a number of distinct glow peaks emerge, the material still seems to contain a quasi-continuous distribution of trap depths. In comparison to TL, we also demonstrate effective optically stimulated luminescence (OSL) from this polymorph of ZrO{sub 2} under red and NIR illumination at ~1 W/cm{sup 2}. All traps responsible for the principal TL peaks were also found to be OSL-active, which widens the applied importance of the material.

  17. Purification of zirconium concentrates

    International Nuclear Information System (INIS)

    Brown, A.E.P.

    1976-01-01

    A commercial grade ZrO 2 and an ammonium uranate (yellow cake) are obtained from the caldasito ore processing. This ore is found in the Pocos de Caldas Plateau, State of Minas Gerais, Brazil. Caldasito is an uranigerous zirconium ore, a mixture of zircon and baddeleyite and contains 60% ZrO 2 and 0,3% U 3 O 8 . The chemical opening of the ore was made by alkaline fusion with NaOH at controlled temperature. The zirconium-uranium separation took place by a continuous liquid-liquid extraction in TBP-varsol-HNO 3 -H 2 O system. The raffinate containing zirconium + impurities (aluminium, iron and titanium) was purified by an ion exchange operation using a strong cationic resin [pt

  18. Waterside corrosion of zirconium alloys in nuclear power plants

    International Nuclear Information System (INIS)

    1998-01-01

    Technically the study of corrosion of zirconium alloys in nuclear power reactors is a very active field and both experimental work and understanding of the mechanisms involved are going through rapid changes. As a result, the lifetime of any publication in this area is short. Because of this it has been decided to revise IAEA-TECDOC-684 - Corrosion of Zirconium Alloys in Nuclear Power Plants - published in 1993. This updated, revised and enlarged version includes major changes to incorporate some of the comments received about the first version. Since this review deals exclusively with the corrosion of zirconium and zirconium based alloys in water, and another separate publication is planned to deal with the fuel-side corrosion of zirconium based fuel cladding alloys, i.e. stress corrosion cracking, it was decided to change the original title to Waterside Corrosion of Zirconium Alloys in Nuclear Power Plants. The rapid changes in the field have again necessitated a cut-off date for incorporating new data. This edition incorporates data up to the end of 1995; including results presented at the 11 International Symposium on Zirconium in the Nuclear Industry held in Garmisch-Partenkirchen, Germany, in September 1995. The revised format of the review now includes: Introductory chapters on basic zirconium metallurgy and oxidation theory; A revised chapter discussing the present extent of our knowledge of the corrosion mechanism based on laboratory experiments; a separate and revised chapter discussing hydrogen uptake; a completely reorganized chapter summarizing the phenomenological observations of zirconium alloy corrosion in reactors; a new chapter on modelling in-reactor corrosion; a revised chapter devoted exclusively to the manner in which irradiation might influence the corrosion process; finally, a summary of our present understanding of the corrosion mechanisms operating in reactor

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

    Science.gov (United States)

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

    2018-02-01

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

  20. Investigation on the corrosion resistance of zirconium in nitric acid

    International Nuclear Information System (INIS)

    Fauvet, P.; Mur, P.

    1990-01-01

    Zirconium in nitric solutions exhibits an excellent corrosion resistance in the passive state, and a mediocre corrosion resistance in the unpassive state with risk of stress corrosion cracking. Results of the influence of some parameters (medium, potential, temperature, stress, friction, metallurgical structure and surface state) on zirconium passivation are presented. Zirconium remains passive in a large range of HNO 3 concentration (at least up to 14.4N), in the presence of oxidizing ions (Cr 4 , Ce 4 ), in a spent fuel dissolution solution. Zirconium is depassived by friction at high speed and pressure, by platinum coupling in boiling 14.4N HNO 3 with or without stress, or by imposed deformation speed under high potential. (A.B.)

  1. Solvent extraction of zirconium

    International Nuclear Information System (INIS)

    Kim, S.S.; Yoon, J.H.

    1981-01-01

    The extraction of zirconium(VI) from an aqueous solution of constant ionic strength with versatic acid-10 dissolved in benzen was studied as a function of pH and the concentration of zirconium(VI) and organic acid. The effects of sulphate and chlorine ions on the extraction of the zirconium(VI) were briefly examined. It was revealed that (ZrOR 2 .2RH) is the predominant species of extracted zirconium(VI) in the versatic acid-10. The chemical equation and the apparent equilibrium constants thereof have been determined as follows. (ZrOsup(2+))aq+ 2(R 2 H 2 )sub(org) = (ZrOR 2 .2RH)sub(org)+2(H + )aq Ksub(Zr) = (ZrOR 2 .2RH)sub(org)(H + ) 2 /(ZrOsup(2+))sub(aq)(R 2 H 2 )sup(2)sub(org) = 3.3 x 10 -7 . The synergistic effects of TBP and D2EHPA were also studied. In the mixed solvent with 0.1M TBP, the synergistic effect was observed, while the mixed solvent with D2EHPA showed the antisynergistic effect. (Author)

  2. Methods for determination of zirconium in titanium alloys

    International Nuclear Information System (INIS)

    1985-01-01

    Two methods for determining zirconium content in titanium alloys are specified in this standard. One is the ion-exchange/mandelic acid gravimetry for Zr content below 20 % down to 1 % while the other is the mandelic acid gravimetry for Zr content below 20 % down to 0.5 %. In the former, a specimen is decomposed by hydrochloric acid and hydrofluoric acid. After substances such as titanium are oxidized by adding nitric acid, the liquid is adjusted into a 4N hydrochloric acid - gN hydrofluoric acid solution, which is them passed through an ion-exchange column. The niobium and tantalum contents are absorbed while the titanium and zirconium contents flow out. Perchloric acid and sulfuric acid are poured in the solution to remove hydrofluoric acid. Aqueous ammonia is added to produce hydroxide of titanium and zirconium, which is then filtered out. The hydroxyde is dissolved in hydrochloric acid, and mandelic acid is poured to precipitate the zirconium content. The precipitate is ignited and the weight of the oxide formed is measured. The coprecipitated titanium content is determined by the absorptiometric method using hydrogen peroxide. Finally, the weight of the oxide is corrected. In the latter determination method, on the other hand, only several steps of the above procedure are used, namely, decomposition by hydrochloric acid, precipitation of zirconium, ignition of precipitate, measurement of oxide weight and weight correction. (Nogami, K.)

  3. Solute redistribution studies in oxidised zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Khera, S K; Kale, G B; Gadiyar, H S [Bhabha Atomic Research Centre, Bombay (India). Metallurgy Div.

    1977-01-01

    Electron microprobe studies on solute distribution in oxide layers and in the regions near oxide metal interface have been carried out in the case of zircaloy-2 and zirconium binary alloys containing niobium, tin, iron, copper, chromium and nickel and oxidised in steam at 550 deg C. In the case of alloys having higher oxidation rates, the oxide of solute element was found to dissolve in ZrO/sub 2/ without any composition variation. However, for solute addition with limited solubility like Cr, Cu and Fe, solute enrichment at metal/oxide interface and depletion of the same matrix has been observed. The intensity profiles for nickel distribution were also found to be identical to Fe or Cr distribution. The mode of solute distribution has been discussed in relation to oxidation behaviour of these alloys.

  4. Study of the zirconium passive layer in nitric medium, by the means of electrochemical impedance spectrometry

    International Nuclear Information System (INIS)

    Musy, C.

    1996-01-01

    Although zirconium exhibits a very low corrosion rate in nitric medium at 100 C, electrochemical impedance spectrometry enabled the in-situ monitoring of the zirconium oxide growth in theses conditions. The growth curve shows a very clear deceleration of the oxide growth kinetics after the first hundred hours of immersion in hot nitric medium. The initial thickness of the native oxide film is also examined

  5. Zirconium - an imported mineral commodity

    International Nuclear Information System (INIS)

    1983-10-01

    This report examines Canada's position in regard to the principal zirconium materials: zircon; fusion-cast zirconium-bearing refractory products; zirconium-bearing chemicals; and zirconium metal, master alloys, and alloys. None of these is produced in Canada except fused alumina-zirconia and certain magnesium-zirconium alloys and zirconium-bearing steels. Most of the 3 000-4 000 tonnes of the various forms of zircon believed to be consumed in Canada each year is for foundry applications. Other minerals, notably chromite, olivine and silica sand are also used for these purposes and, if necessary, could be substituted for zircon. Zirconium's key role in Canada is in CANDU nuclear power reactors, where zirconium alloys are essential in the cladding for fuel bundles and in capital equipment such as pressure tubes, calandria tubes and reactivity control mechanisms. If zirconium alloys were to become unavailable, the Canadian nuclear power industry would collapse. As a contingency measure, Ontario Hydro maintains at least nine months' stocks of nuclear fuel bundles. Canada's vulnerability to short-term disruptions to supplies of nuclear fuel is diminished further by the availability of more expensive electricity from non-nuclear sources and, given time, from mothballed thermal plants. Zirconium minerals are present in many countries, notably Australia, the Republic of South Africa and the United States. Australia is Canada's principal source of zircon imports; South Africa is its sole source of baddeleyite. At this time, there are no shortages of either material. Canada has untapped zirconium resources in the Athabasca Oil Sands (zircon) and at Strange Lake along the ill-defined border between Quebec and Newfoundland (gittinsite). Adequate metal and alloy production facilities exist in France, Japan and the United States. No action by the federal government in regard to zirconium supplies is called for at this time

  6. Hot zirconium cathode sputtered layers for useful surface modification

    International Nuclear Information System (INIS)

    Duckworth, R.G.

    1986-01-01

    It has been found that multilayer zirconium based sputtered coatings can greatly improve the wear properties of a wide variety of mechanical components, machine tools, and metal surfaces. Although a hot (approximately 1000 0 C) cathode is employed, temperature sensitive components can be beneficially treated, and for precision parts a total coating thickness of only 0.5μm is often perfectly effective. Even at the highest coating rates substrate temperatures are below 300 0 C. For the corrosion protection of less well finished surfaces thicker layers are usually required and it is important that relatively stress free layers are produced. The authors employed a variety of tailored zirconium/zirconium nitride/zirconium oxide mixed layers to solve a number of tribological problems for some 5 or 6 years. However, it is only recently that they designed, built, and commissioned rapid cycle, multiple cathode, load-lock plant for economic production of such coatings. This paper provides an introduction to this method of depositing pure zirconium and pure synthetic zirconium nitride films

  7. Synthesis of Zirconium Lower Chlorides

    International Nuclear Information System (INIS)

    Gaviria, Juan P.

    2002-01-01

    This research is accurately related to the Halox concept of research reactor spent fuel element treatment.The aim of this project is to work the conditioning through selected chlorination of the element that make the spent fuel element. This research studied the physical chemistry conditions which produce formation of the lower zirconium chlorides through the reaction between metallic Zr and gaseous ZrCl 4 in a silica reactor.This work focused special attention in the analysis and confrontation of the published results among the different authors in order to reveal coincidences and contradictions.Experimental section consisted in a set of synthesis with different reaction conditions and reactor design. After reaction were analyzed the products on Zr shavings and the deposit growth on wall reactor.The products were strongly dependent of reactor design. It was observed that as the distance between Zr and wall reactor increased greater was tendency to lower chlorides formation.In reactors with small distance the reaction follows other way without formation of lower chlorides.Analysis on deposit growth on reactor showed that may be formed to a mixture of Si x Zr y intermetallics and zirconium oxides.Presence of oxygen in Zr and Zr-Si compounds on wall reactor reveals that there is an interaction between quartz and reactants.This interaction is in gaseous phase because contamination is observed in experiences where Zr was not in contact with reactor.Finally, it was made a global analysis of all experiences and a possible mechanism that interprets reaction ways is proposed

  8. Plasma arc melting of zirconium

    International Nuclear Information System (INIS)

    Tubesing, P.K.; Korzekwa, D.R.; Dunn, P.S.

    1997-01-01

    Zirconium, like some other refractory metals, has an undesirable sensitivity to interstitials such as oxygen. Traditionally, zirconium is processed by electron beam melting to maintain minimum interstitial contamination. Electron beam melted zirconium, however, does not respond positively to mechanical processing due to its large grain size. The authors undertook a study to determine if plasma arc melting (PAM) technology could be utilized to maintain low interstitial concentrations and improve the response of zirconium to subsequent mechanical processing. The PAM process enabled them to control and maintain low interstitial levels of oxygen and carbon, produce a more favorable grain structure, and with supplementary off-gassing, improve the response to mechanical forming

  9. Zirconium microstructures: uncharted possibilities

    International Nuclear Information System (INIS)

    Samajdar, I.; Kumar, Gulshan; Singh, Jaiveer; Lodh, Arijit; Srivastava, D.; Tewari, R.; Dey, G.K.; Saibaba, N.

    2015-01-01

    The 'conventional' Zirconium microstructures can be significantly extended with information on: (i) microtexture, (ii) residual stresses and (iii) local mechanical properties. Though these involve different tools, but a consolidated microstructure can be crated. This is the theme of this presentation. Examples of this consolidated picture will be made from deformation twinning, recovery-recrystallization, burst ductility and orientation versus solid solution hardening. (author)

  10. Zirconium elasticity modules

    International Nuclear Information System (INIS)

    Vavra, G.

    1978-01-01

    Considered are the limit and the intermediate values of the Young modulus E, modulus of shear G and of linear modulus of compression K obtainable at various temperatures (4.2 to 1133 K) for single crystals of α-zirconium. Determined and presented are the corrected isotropic elasticity characteristics of E, G, K over the above range of temperatures of textured and non-textured α-Zr

  11. Beryllium and zirconium

    International Nuclear Information System (INIS)

    Salesse, Marc

    1959-01-01

    Pure beryllium and zirconium, both isolated at about the same date but more than a century ago remained practically unused for eighty years. Fifteen years ago they were released from this state of inactivity by atomic energy, which made them into current metal a with an annual production which runs into tens of tons for the one and thousands for the other. The reasons for this promotion promise well for the future of the two metals, which moreover will probably find additional uses in other branches of industry. The attraction of beryllium and zirconium for atomic energy is easily explained. The curve of figure 1 gives the price per gram of uranium-235 as a function of enrichment: this price increases by about a factor of 3 on passing from natural uranium (0, 7 percent 235 U) to almost pure uranium-235. Because of their tow capture cross-section beryllium and zirconium make it possible, or at least easier, to use natural uranium and they thus enjoy an advantage the extent of which must be calculated for each reactor or fuel element project, but which is generally considerable. It will be seen later that this advantage should be based on figures which are even more favourable that would appear from the simple ratio 3 of the price of pure uranium- 235 contained in natural uranium. Reprint of a paper published in 'Industries Atomiques' - n. 1-2, 1959

  12. Sensitivity analysis on the zirconium ignition in a postulated SFP loss of coolant accident

    International Nuclear Information System (INIS)

    Park, Sanggil; Lee, Jaeyoung; Kim, Sun-ki; Chun, Tae-hyun; Bang, Je-geon

    2016-01-01

    From both SFP complete LOCA experiments, it was observed that zirconium alloy cladding temperature was abruptly increased at a certain point and the cladding was almost fully oxidized. To capture this phenomenon, the concept of air oxidation breakaway model was adopted in MELCOR code. This paper examines this air oxidation breakaway model by comparing the SFP project test data and MELCOR code calculation results by using this model. The air oxidation model parameters are slightly altered to see their sensitivities on the occurrence of the zirconium ignition. Through such sensitivity analysis, limitations of the air oxidation breakaway model are revealed in comparison to the actual zirconium ignition phenomenon during air ingress scenarios. In addition, ways to overcome the identified limitations of the air oxidation model are recommended to estimate better the zirconium ignition phenomenon in SFP sequences. In this paper, the zirconium ignition phenomenon was reviewed and the model to capture this phenomenon was investigated. The model is the air oxidation breakaway model in MELCOR code, and its sensitivity of the model parameters on the time to ignition was studied. From the sensitivity analysis, the slight change of model parameters induce the large variation of the time to ignition. The model itself includes its weakness to fully represent both the air oxidation breakaway phenomenon and the followed zirconium ignition behavior. Furthermore, this model considers no effect of N2 on the cladding degradation and its promoted exothermic heat release

  13. Sensitivity analysis on the zirconium ignition in a postulated SFP loss of coolant accident

    Energy Technology Data Exchange (ETDEWEB)

    Park, Sanggil; Lee, Jaeyoung [Handong Global Univ., Pohang (Korea, Republic of); Kim, Sun-ki; Chun, Tae-hyun; Bang, Je-geon [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2016-10-15

    From both SFP complete LOCA experiments, it was observed that zirconium alloy cladding temperature was abruptly increased at a certain point and the cladding was almost fully oxidized. To capture this phenomenon, the concept of air oxidation breakaway model was adopted in MELCOR code. This paper examines this air oxidation breakaway model by comparing the SFP project test data and MELCOR code calculation results by using this model. The air oxidation model parameters are slightly altered to see their sensitivities on the occurrence of the zirconium ignition. Through such sensitivity analysis, limitations of the air oxidation breakaway model are revealed in comparison to the actual zirconium ignition phenomenon during air ingress scenarios. In addition, ways to overcome the identified limitations of the air oxidation model are recommended to estimate better the zirconium ignition phenomenon in SFP sequences. In this paper, the zirconium ignition phenomenon was reviewed and the model to capture this phenomenon was investigated. The model is the air oxidation breakaway model in MELCOR code, and its sensitivity of the model parameters on the time to ignition was studied. From the sensitivity analysis, the slight change of model parameters induce the large variation of the time to ignition. The model itself includes its weakness to fully represent both the air oxidation breakaway phenomenon and the followed zirconium ignition behavior. Furthermore, this model considers no effect of N2 on the cladding degradation and its promoted exothermic heat release.

  14. Atomic profile imaging of ceramic oxide surfaces

    International Nuclear Information System (INIS)

    Bursill, L.A.; Peng JuLin; Sellar, J.R.

    1989-01-01

    Atomic surface profile imaging is an electron optical technique capable of revealing directly the surface crystallography of ceramic oxides. Use of an image-intensifier with a TV camera allows fluctuations in surface morphology and surface reactivity to be recorded and analyzed using digitized image data. This paper reviews aspects of the electron optical techniques, including interpretations based upon computer-simulation image-matching techniques. An extensive range of applications is then presented for ceramic oxides of commercial interest for advanced materials applications: including uranium oxide (UO 2 ); magnesium and nickel oxide (MgO,NiO); ceramic superconductor YBa 2 Cu 3 O 6.7 ); barium titanate (BaTiO 3 ); sapphire (α-A1 2 O 3 ); haematite (α-Fe-2O 3 ); monoclinic, tetragonal and cubic monocrystalline forms of zirconia (ZrO 2 ), lead zirconium titanate (PZT + 6 mol.% NiNbO 3 ) and ZBLAN fluoride glass. Atomic scale detail has been obtained of local structures such as steps associated with vicinal surfaces, facetting parallel to stable low energy crystallographic planes, monolayer formation on certain facets, relaxation and reconstructions, oriented overgrowth of lower oxides, chemical decomposition of complex oxides into component oxides, as well as amorphous coatings. This remarkable variety of observed surface stabilization mechanisms is discussed in terms of novel double-layer electrostatic depolarization mechanisms, as well as classical concepts of the physics and chemistry of surfaces (ionization and affinity energies and work function). 46 refs., 16 figs

  15. Corrosion Behavior and Oxide Properties of Zr-Nb-Cu and Zr-Nb-Sn Alloy in High Dissolved Hydrogen Primary Water Chemistry

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Yun Ju; Kim, Tae Ho; Kim, Ji Hyun [UNIST, Ulsan (Korea, Republic of)

    2016-05-15

    The water-metal interface is regarded as rate-controlling site governing the rapid oxidation transition in high burn-up fuel. And the zirconium oxide is made in water-metal interface and its structure and phase do an important role in terms of oxide properties. During oxidation process, the protective tetragonal oxide layer develops at the interface due to accumulated high stress during oxide growth, and it turns into non-protective monoclinic oxide with increasing oxide thickness, thus decreasing the stress. It has been reported that Nb addition was proven to be very beneficial for increasing the corrosion resistance of the zirconium alloys. From a more recent study, Cu addition in Nb containing Zirconium alloy was reported to be effective for increasing corrosion resistance in water containing B and Li. According to the previous research conducted, Zr-Nb-Cu shows better corrosion resistance than Zircaloy-4. The dissolved hydrogen (DH) concentration is the key issue of primary water chemistry, and the effect of DH concentration on the corrosion rate of nickel based alloy has been researched. However, the effect of DH on the zirconium alloy corrosion mechanism was not fully investigated. In this study, the weight gain measurement, FIB-SEM analysis, and Raman spectroscopic measurement were conducted to investigate the effects of dissolved hydrogen concentration and the chemical composition on the corrosion resistance and oxide phase of Zr-Nb-Cu alloy and Zr-Nb-Sn alloy after oxidizing in a primary water environment for 20 d. The corrosion rate of Zr-Nb-Cu alloy is slow, when it is compared to Zr-Nb-Sn alloy. In SEM images, the oxide thickness of Zr-Nb-Cu alloy is measured to be around 1.06 μm it of Zr-Nb-Sn alloy is measured to be 1.15 μm. It is because of the Segregation made by Sn solute element when Sn solute element oxidized. And according to ex situ Raman spectra, Zr-Nb-Cu alloy oxide has more tetragonal zirconium oxide fraction than Zr-Nb-Sn alloy oxide.

  16. Fluorometric determination of zirconium in minerals

    Science.gov (United States)

    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.

  17. Process for purifying zirconium sponge

    International Nuclear Information System (INIS)

    Abodishish, H.A.M.; Kimball, L.S.

    1992-01-01

    This patent describes a Kroll reduction process wherein a zirconium sponge contaminated with unreacted magnesium and by-product magnesium chloride is produced as a regulus, a process for purifying the zirconium sponge. It comprises: distilling magnesium and magnesium chloride from: a regulus containing a zirconium sponge and magnesium and magnesium chloride at a temperature above about 800 degrees C and at an absolute pressure less than about 10 mmHg in a distillation vessel to purify the zirconium sponge; condensing the magnesium and the magnesium chloride distilled from the zirconium sponge in a condenser; and then backfilling the vessel containing the zirconium sponge and the condenser containing the magnesium and the magnesium chloride with a gas; recirculating the gas between the vessel and the condenser to cool the zirconium sponge from above about 800 degrees C to below about 300 degrees C; and cooling the recirculating gas in the condenser containing the condensed magnesium and the condensed magnesium chloride as the gas cools the zirconium sponge to below about 300 degrees C

  18. Spectroscopic studies of dynamically compacted monoclinic ZrO2

    NARCIS (Netherlands)

    Maczka, M.; Lutz, E.T.G.; Verbeek, H.J.; Oskam, K.; Meijerink, A.; Hanuza, J.; Stuivinga, M.E.C.

    1999-01-01

    The properties of dynamically compacted monoclinic zirconia have been studied by X-ray powder diffraction, IR, Raman, EPR and luminescence spectroscopy. Compaction introduces a large number of defects into the sample, which leads to a broadening of the X-ray lines, and IR and Raman bands. Besides,

  19. Modelling of zirconium alloys corrosion in LWRs

    International Nuclear Information System (INIS)

    Kritskij, V.G.; Berezina, I.G.; Kritskij, A.V.; Stjagkin, P.S.

    1999-01-01

    Chemical parameters, that exerted effect on Zr+1%Nb alloy corrosion and deserved consideration during reactor operation, were defined and a model was developed to describe the influence of physical and chemical parameters on zirconium alloys corrosion in nuclear power plants. The model is based on the correlation between the zirconium oxide solubility in high-temperature water under the influence of the chemical parameters and the measured values of fuel cladding corrosion under LWR conditions. The intensity of fuel cladding corrosion in the primary circuits depends on the coolant water quality, growth of iron oxide deposits and vaporization portion. Mathematically, the oxidation rate can be expressed as a sum of heat and radiation components. The temperature dependence on the oxidation rate can be described by the Arrenius equation. The radiation component of Zr uniform corrosion equation is a function of several factors such as neutron fluency, the temperature the metallurgical composition and et. We assume that the main factor is the changing of water chemistry and the H 2 O 2 concentration play the determinative role. Probably, the influence of H 2 O 2 is based on the formation of unstable compound ZrO 3 ·nH 2 O and Zr(OH) 4 with high solubility. The validity of the used formulae was confirmed by corrosion measurements on WWER and RBMK fuel cladding. The model can be applied for calculating the reliability of nuclear fuel operation. (author)

  20. Study of propane partial oxidation on vanadium-containing catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Komashko, G.A.; Khalamejda, S.V.; Zazhigalov, V.A. [AN Ukrainskoj SSR, Kiev (Ukraine). Inst. Fizicheskoj Khimii

    1998-12-31

    The present results indicate that maximum selectivity to acrylic acid can be reached over V-P-Zr-O catalysts. When the hydrocarbon concentration is 5.1 vol.% the selectivity is about 30% at quite high paraffin conversion. Conclusively, some explanations to the observed facts can be given. The V-P-O catalyst promotion with lanthanum by means of mechanochemical treatment is distinguished by the additive uniform spreading all over the matrix surface. Such twophase system is highly active in propane conversion (lanthanum oxide) and further oxidation of the desired products. The similar properties are attributed to V-P-Bi-La-O catalyst. Bismuth, tellurium and zirconium additives having clearly defined acidic properties provoke the surface acidity strengthening and make easier desorption of the acidic product (acrylic acid) from the surface lowering its further oxidation. Additionally, since bismuth and zirconium are able to form phosphates and, according to, to create space limitations for the paraffin molecule movement out of the active group boundaries, this can be one more support in favour of the selectivity increase. With this point of view very interesting results were obtained. It has been shown that the more limited the size of the vanadium unit, the higher the selectivity is. Monoclinic phase AV{sub 2}P{sub 2}O{sub 10} which consists in clusters of four vanadium atoms is sensibly more reactive than the orthorhombic phase consists in V{sub {infinity}} infinite chains. (orig.)

  1. ZIRCONIUM PHOSPHATE ADSORPTION METHOD

    Science.gov (United States)

    Russell, E.R.; Adamson, A.S.; Schubert, J.; Boyd, G.E.

    1958-11-01

    A method is presented for separating plutonium values from fission product values in aqueous acidic solution. This is accomplished by flowing the solutlon containing such values through a bed of zirconium orthophosphate. Any fission products adsorbed can subsequently be eluted by washing the column with a solution of 2N HNO/sub 3/ and O.lN H/sub 3/PO/sub 4/. Plutonium values may subsequently be desorbed by contacting the column with a solution of 7N HNO/sub 3/ .

  2. Silica intercalated crystalline zirconium phosphate-type materials

    NARCIS (Netherlands)

    1988-01-01

    The present invention relates to intercalated crystalline zirconium phosphate-types compositions wherein the interlayers of said composition have been intercalated with three-dimensional silicon oxide pillars whereby the pillars comprise at least two silicon atom layers parallel to the clay

  3. Corrosion resistance of zirconium: general mechanisms, behaviour in nitric acid

    International Nuclear Information System (INIS)

    Pinard Legry, G.

    1990-01-01

    Corrosion resistance of zirconium results from the strong affinity of this metal for oxygen; as a result a thin protective oxide film is spontaneously formed in air or aqueous media, its thickness and properties depending on the physicochemical conditions at the interface. This film passivates the underlying metal but obviously if the passive film is partially or completely removed, localised or generalised corrosion phenomena will occur. In nitric acid, this depassivation may be chemical (fluorides) or mechanical (straining, creep, fretting). In these cases it is useful to determine the physicochemical conditions (concentration, temperature, potential, stress) which will have to be observed to use safely zirconium and its alloys in nitric acid solutions [fr

  4. Analytical study of zirconium and hafnium α-hydroxy carboxylates

    International Nuclear Information System (INIS)

    Terra, V.R.

    1991-01-01

    The analytical study of zirconium and hafnium α-hydroxy carboxylates was described. For this purpose dl-mandelic, dl-p-bromo mandelic, dl-2-naphthyl glycolic, and benzilic acids were prepared. These were used in conjunction with glycolic, dl-lactic, dl-2-hydroxy isovaleric, dl-2-hydroxy hexanoic, and dl-2-hydroxy dodecanoic acids in order to synthesize the zirconium(IV) and hafnium(IV) tetrakis(α-hydroxy carboxylates). The compounds were characterized by melting point determination, infrared spectroscopy, thermogravimetric analysis, calcination to oxides and X-ray diffractometry by the powder method. (C.G.C)

  5. Modification in band gap of zirconium complexes

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Mayank, E-mail: mayank30134@gmail.com; Singh, J.; Chouhan, S. [Department of Physics, ISLE, IPS Academy, Indore (M.P.) (India); Mishra, A. [School of Physics, Devi Ahilya Vishwavidyalaya, Indore (M.P.) (India); Shrivastava, B. D. [Govt. P. G. College, Biora (M.P.) (India)

    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.

  6. AC plasma electrolytic oxidation of magnesium with zirconia nanoparticles

    International Nuclear Information System (INIS)

    Arrabal, R.; Matykina, E.; Viejo, F.; Skeldon, P.; Thompson, G.E.; Merino, M.C.

    2008-01-01

    The incorporation of monoclinic zirconia nanoparticles and their subsequent transformation is examined for coatings formed on magnesium by plasma electrolytic oxidation under AC conditions in silicate electrolyte. The coatings are shown to comprise two main layers, with nanoparticles entering the coating at the coating surface and through short-circuit paths to the region of the interface between the inner and outer coating layers. Under local heating of microdischarges, the zirconia reacts with magnesium species to form Mg 2 Zr 5 O 12 in the outer coating layer. Relatively little zirconium is present in the inner coating layer. In contrast, silicon species are present in both coating layers, with reduced amounts in the inner layer

  7. Zirconium for nitric acid solutions

    International Nuclear Information System (INIS)

    Yau, T.L.

    1984-01-01

    The excellent corrosion resistance of zirconium in nitric acid has been known for over 30 years. Recently, there is an increasing interest in using zirconium for nitric acid services. Therefore, an extensive research effort has been carried out to achieve a better understanding of the corrosion properties of zirconium in nitric acid. Particular attention is paid to the effect of concentration, temperature, structure, solution impurities, and stress. Immersion, autoclave, U-bend, and constant strain-rate tests were used in this study. Results of this study indicate that the corrosion resistance of zirconium in nitric acid is little affected by changes in temperature and concentration, and the presence of common impurities such as seawater, sodium chloride, ferric chloride, iron, and stainless steel. Moreover, the presence of seawater, sodium chloride, ferric chloride, and stainless steel has little effect on the stress corrosion craking (SCC) susceptibility of zirconium in 70% nitric acid at room temperatures. However, zirconium could be attacked by fluoride-containing nitric acid and the vapors of chloride-containing nitric acid. Also, high sustained tensile stresses should be avoided when zirconium is used to handle 70% nitric acid at elevated temperatures or > 70% nitric acid

  8. Zirconium intermetallics and hydrogen uptake during corrosion

    International Nuclear Information System (INIS)

    Cox, B.

    1987-04-01

    The routes by which hydrogen can enter zirconium alloys containing second phase particles during corrosion are discussed. Both direct diffusion through the bulk of the oxide film, and migration through second phase particles that intersect the surface are considered. An examination of results for hydrogen uptake by zirconium alloys during the early stages of oxidation, when the oxide film is still coherent, suggests that for Zr, Zr-1%Cu and Zr-1%Fe the hydrogen enters by diffusing through the bulk ZrO 2 film, whereas for the Zircaloys the primary migration route may be through the intermetallics. The steps in the latter process are discussed and the evidence available on the properties of the intermetallics collated. A comparison of these data with results for hydrogen uptake by two series of ternary alloys (Zr-1%Nb - 1%X, Zr-1%Cu - 1%X) suggests that high hydrogen uptakes often correlate with intermetallics with high hydrogen solubilities and vice versa. The properties of Zr(Fe/Cr) 2+x intermetallics are examined in an attempt to understand the behaviour of the Zircaloys, and it is concluded that present data establishing composition and unit cell dimensions for such intermetallic particles are not of sufficient accuracy to permit a correlation

  9. SEPARATION OF HAFNIUM FROM ZIRCONIUM

    Science.gov (United States)

    Overholser, L.B.; Barton, C.J. Sr.; Ramsey, J.W.

    1960-05-31

    The separation of hafnium impurities from zirconium can be accomplished by means of organic solvent extraction. The hafnium-containing zirconium feed material is dissolved in an aqueous chloride solution and the resulting solution is contacted with an organic hexone phase, with at least one of the phases containing thiocyanate. The hafnium is extracted into the organic phase while zirconium remains in the aqueous phase. Further recovery of zirconium is effected by stripping the onganic phase with a hydrochloric acid solution and commingling the resulting strip solution with the aqueous feed solution. Hexone is recovered and recycled by means of scrubbing the onganic phase with a sulfuric acid solution to remove the hafnium, and thiocyanate is recovered and recycled by means of neutralizing the effluent streams to obtain ammonium thiocyanate.

  10. Zirconium nitride hard coatings

    International Nuclear Information System (INIS)

    Roman, Daiane; Amorim, Cintia Lugnani Gomes de; Soares, Gabriel Vieira; Figueroa, Carlos Alejandro; Baumvol, Israel Jacob Rabin; Basso, Rodrigo Leonardo de Oliveira

    2010-01-01

    Zirconium nitride (ZrN) nanometric films were deposited onto different substrates, in order to study the surface crystalline microstructure and also to investigate the electrochemical behavior to obtain a better composition that minimizes corrosion reactions. The coatings were produced by physical vapor deposition (PVD). The influence of the nitrogen partial pressure, deposition time and temperature over the surface properties was studied. Rutherford backscattering spectrometry (RBS), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), scanning electron microscopy (SEM) and corrosion experiments were performed to characterize the ZrN hard coatings. The ZrN films properties and microstructure changes according to the deposition parameters. The corrosion resistance increases with temperature used in the films deposition. Corrosion tests show that ZrN coating deposited by PVD onto titanium substrate can improve the corrosion resistance. (author)

  11. Oxidation behaviour of Zr-based bulk metallic glasses

    International Nuclear Information System (INIS)

    Wang, Bin

    2011-01-01

    The Zr-based bulk metallic glasses, developed since the late 1980's, have very interesting mechanical properties, which can be considered for many applications including working under oxidizing atmosphere conditions at high temperatures. It is therefore interesting to study their oxidation resistance and to characterize the oxide scale formed on alloys surface. The fundamental objective of this thesis is to enhance the understanding of the role of various thermodynamic and chemistry parameters on the oxidation behaviour of the Zr-based bulk metallic glasses at high temperature under dry air, to determine the residual stresses in the oxide layer, in comparison with their crystalline alloys with the same chemical composition after an annealing treatment. The oxidation kinetics of these glasses and the crystalline structure of oxide scale ZrO 2 depend on the temperature and the oxidation duration: for short periods of oxidation or at a temperature below Tg, the kinetics follows a parabolic law, whereas, if the sample is oxidized at T ≥ Tg, the kinetics can be divided into two parts. The crystalline counterparts are oxidized by a parabolic rule whatever the temperature; for long oxidation duration at a temperature close to Tg, the kinetics becomes more complex because of the crystallisation of the glasses during the oxidation tests. Also the crystalline structure of the oxide layers depends on the oxidation temperature: the oxide layer consists only in tetragonal Zirconia at T ≤ Tg, while monoclinic Zirconia was formed at higher temperature. The mechanism of the formation of the oxide scale is due to both the interior diffusion of Oxygen ions and the external diffusion of Zirconium ions. However the diffusion of Zirconium ions slows gradually during the crystallisation process of the glass matrix. When the crystallisation is completed, the formation of Zirconia is controlled by only the internal diffusion of oxygen ions. The corresponding residual stresses

  12. Mechanism of the monoclinic-to-tetragonal phase transition induced in zirconia and hafnia by swift heavy ions

    International Nuclear Information System (INIS)

    Benyagoub, Abdenacer

    2005-01-01

    Recent results demonstrated that defect formation or amorphization are not the only structural changes induced by swift heavy ions in crystalline materials and that under certain circumstances crystalline-to-crystalline phase transitions can also occur. For instance, it was found that both zirconia and hafnia transform from the monoclinic to the tetragonal phase with a kinetics involving a double ion impact process. In order to understand the origin of this ion-beam induced phase transition, the behavior of these twin oxides was analyzed and compared. In fact, the likeness of these materials offered the unique opportunity to impose drastic constraints on the possible models proposed to explain the creation of atomic displacements in the wake of swift heavy ions. This comparison clearly suggests that the thermal spike is the most appropriate process which governs the transition from the monoclinic to the tetragonal phase in zirconia and hafnia

  13. Corrosion resistance of high-performance materials titanium, tantalum, zirconium

    CERN Document Server

    2012-01-01

    Corrosion resistance is the property of a material to resist corrosion attack in a particular aggressive environment. Although titanium, tantalum and zirconium are not noble metals, they are the best choice whenever high corrosion resistance is required. The exceptionally good corrosion resistance of these high–performance metals and their alloys results from the formation of a very stable, dense, highly adherent, and self–healing protective oxide film on the metal surface. This naturally occurring oxide layer prevents chemical attack of the underlying metal surface. This behavior also means, however, that high corrosion resistance can be expected only under neutral or oxidizing conditions. Under reducing conditions, a lower resistance must be reckoned with. Only very few inorganic and organic substances are able to attack titanium, tantalum or zirconium at ambient temperature. As the extraordinary corrosion resistance is coupled with an excellent formability and weldability these materials are very valua...

  14. Recovery of zirconium from pickling solution, regeneration and its reuse

    Energy Technology Data Exchange (ETDEWEB)

    Bhattacharjee, D. [Nuclear Fuel Complex, Hyderabad 500062 (India); Mandal, D., E-mail: dmandal10@gmail.com [Alkali Material & Metal Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Visweswara Rao, R.V.R.L.; Sairam, S.; Thakur, S. [Nuclear Fuel Complex, Hyderabad 500062 (India)

    2017-05-15

    Graphical abstract: The following compares the performance of fresh pickling solution (PS) and regenerated and used pickling solution (UPS). - Highlights: • Pickling of zircaloy tubes and appendages is carried out to remove oxide layer. • The pickling solution become saturated with zirconium due to reuse. • As NaNO{sub 3} concentration increases, conc. of Zr in pickling solution decreases. • Experimental results shows that, used pickling solution can be regenerated. • Regenerated solution may be reused by adding makeup quantities of HF-HNO{sub 3}. - Abstract: The pressurized heavy water reactors use natural uranium oxide (UO{sub 2}) as fuel and uses cladding material made up of zircaloy, an alloy of zirconium. Pickling of zircaloy tubes and appendages viz., spacer and bearing pads is carried out to remove the oxide layer and surface contaminants, if present. Pickling solution, after use for many cycles i.e., used pickling solution (UPS) is sold out to vendors, basically for its zirconium value. UPS, containing a relatively small concentration of hydrofluoric acid. After repeated use, pickling solution become saturated with zirconium fluoride complex and is treated by adding sodium nitrate to precipitate sodium hexafluro-zirconate. The remaining solution can be recycled after suitable makeup for further pickling use. The revenue lost by selling UPS is very high compared to its zirconium value, which causes monetary loss to the processing unit. Experiments were conducted to regenerate and reuse UPS which will save a good amount of revenue and also protect the environment. Experimental details and results are discussed in this paper.

  15. A study of a production process for hafnium-free zirconium from zircon

    International Nuclear Information System (INIS)

    Ratanalert, N.

    1985-01-01

    The purpose of this experiment was to extract and purify the zirconium from zircon. The effects of time of extraction and stripping of zirconium, concentration of feed solution, concentration of hydrochloric acid in stripping process, equilibrium curve of extraction of zirconium and hafnium and equilibrium curve of stripping zirconium or scrubbing hafnium were studied from standard zirconium and hafnium. The results, subsequently were applied to the extraction procedures for zirconium from zircon. Minus 100 mesh zircon was fused with sodium hydroxide in the ratio of 1 : 6 at 700 degree C for l hour. After fusion the zirconate was leached with water and dissolved in hot concentrated hydrochloric acid. Zirconyl chloride octahydrate crystallized out when the solution was cooled. An agueons solution of zirconyl chloride was used as the feed to the hexone - thiocyanate solvent extraction process. This was prepared by dissolving zirconyl chloride octahydrate crystal in waster. This zirconium feed solution in 1 M HCl and 1 M N H 4 CNS was extracted with 2.7 m N H 4 CNS in hexone and then stripped with 3.6 M HCl the aqueous phase was got rid of thiocyanate ion by extracting with pure hexone, then the zirconium in aqueous phase was precipitated with sulfuric acid and ammonium hydroxide at pH 1.8 - 2.0 and zirconium oxide was obtained by ignition at 700 degree C. The process could be modified to improve the purity of zirconium by using cation exchange resin to get rid of thiocyanate ion after solvent extraction process

  16. Precipitation of γ-zirconium hydride in zirconium

    International Nuclear Information System (INIS)

    Carpenter, G.J.C.

    1978-01-01

    A mechanism for the precipitation of γ-zirconium hydride in zirconium is presented which does not require the diffusion of zirconium. The transformation is completed by shears caused by 1/3 (10 anti 10) Shockley partial dislocations on alternate zirconium basal planes, either by homogeneous nucleation or at lattice imperfections. Homogeneous nucleation is considered least likely in view of the large nucleation barrier involved. Hydrides may form at dislocations by the generation of partials by means of either a pole or ratchet mechanism. The former requires dislocations with a component of Burgers vector along the c-axis, but contrast experiments show that these are not normally observed in annealed zirconium. It is therefore most likely that intragranular hydrides form at the regular 1/3 (11 anti 20) dislocations, possibly by means of a ratchet mechanism. Contrast experiments in the electron microscope show that the precipitates have a shear character consistent with the mechanism suggested. The possibility that the shear dislocations associated with the hydrides are emissary dislocations is considered and a model suggested in which this function is satisfied together with the partial relief of misfit stresses. The large shear strains associated with the precipitation mechanism may play an important role in the preferential orientation of hydrides under stress

  17. Fine-grained zirconium-base material

    Science.gov (United States)

    Van Houten, G.R.

    1974-01-01

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

  18. Evaluation of thermodynamic data on zirconium and hafnium halides and oxyhalides by means of transport experiments

    International Nuclear Information System (INIS)

    Dittmer, G.; Niemann, U.

    1987-01-01

    A consistent set of thermodynamic data for zirconium and hafnium halides, oxides and oxyhalides was achieved. It was found that formation enthalpies of gaseous compounds could be derived from solubility measurements together with theoretical estimations and a revision of literature data. Free energy functions were calculated employing statistical mechanics. Data for liquid and solid compounds were obtained via sublimation and vaporization data. Chemical equilibria of zirconium and hafnium with halogens are discussed. 51 refs.; 16 figs.; 14 tabs

  19. Investigation of chlorination of zirconium and hafnium and their compounds in discharge from hollow cathode

    International Nuclear Information System (INIS)

    Ioffe, R.B.; Korovin, Yu.I.

    1978-01-01

    The possibility is investigated of chlorinating various zirconium and hafnium compounds (metal, oxide, carbide) in a hot discharge from a hollow cathode with various chlorinating reagents: copper monochloride, nickel chloride, magnesium chloride, for the purpose of accelerating their entrance into the excitation zone. It has been shown thermodynamically and experimentally that chlorination of metal zirconium and hafnium and their carbides with copper monochloride in hot hollow cathode conditions provides a sharp increase in the intensity of the lines of these elements

  20. Assembly of crosslinked oxo-cyanoruthenate and zirconium oxide bilayers: Application in electrocatalytic films based on organically modified silica with templated pores

    International Nuclear Information System (INIS)

    Rutkowska, Iwona A.; Sek, Jakub P.; Mehdi, B. Layla; Kulesza, Pawel J.; Cox, James A.

    2014-01-01

    Electrochemical deposition of crosslinked oxo-cyanoruthenate, Ru-O/CN-O, from a mixture of RuCl 3 and K 4 Ru(CN) 6 is known to yield a film on glassy carbon that promotes oxidations by a combination of electron and oxygen transfer. Layer-by-layer (LbL) deposition of this species at a film formed by cycling of the electrode potential in a ZrO 2 solution systematically increases the number of catalytically active sites of the Ru-O/CN-O on the electrode. The evaluation of the electrocatalytic activity was by cyclic voltammetric oxidation of cysteine at pH 2. Plots of the anodic peak current vs. the square root of scan rate were indicative of linear diffusion control of this oxidation, even in the absence of ZrO 2 , but the slopes of these linear plots increased with bilayer number, n, of (ZrO 2 | Ru-O/CN-O) n . The latter observation is hypothesized to be due to an increased number of active sites for a given geometric electrode area, but proof requires further study. To optimize utilization of the catalyst and to provide a size-exclusion characteristic to the electrode, the study was extended to LbL deposition of the composite in 50-nm pores of an organically modified silica film deposited by electrochemically assisted sol-gel processing using surface-bound poly(styrene sulfonate) nanospheres as a templating agent

  1. Problems of zirconium metal production in Czechoslovakia

    International Nuclear Information System (INIS)

    Vareka, J.; Vaclavik, E.

    1975-01-01

    The problems are summed up of the production and quality control of zirconium sponge. A survey is given of industrial applications of zirconium in form of pure metal or alloys in nuclear power production, ferrous and non-ferrous metallurgy, chemical engineering and electrical engineering. A survey is also presented of the manufacture of zirconium metal in advanced capitalist countries. (J.B.)

  2. Anisotropy of mechanical properties of zirconium and zirconium alloys

    International Nuclear Information System (INIS)

    Medrano, R.E.

    1975-01-01

    In studies of technological applications of zirconium to fuel elements of nuclear reactor, it was found that the use of plasticity equations for isotropic materials is not in agreement with experimental results, because of the strong anisotropy of zirconium. The present review describes recent progress on the knowledge of the influence of anisotropy on mechanical properties, after Douglass' review in 1971. The review was written to be selfconsistent, changing drastically the presentation of some of the referenced papers. It is also suggested some particular experiments to improve developments in this area

  3. Radiochemical studies on amorphous zirconium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Dyer, A; Moores, G E [Salford Univ. (UK). Dept. of Chemistry and Applied Chemistry

    1981-01-01

    Amorphous zirconium phosphate (ZrP) is used in some hemodialysis machines for the regeneration of dialysate. Its function is to adsorb ammonium ions formed by the pretreatment of urea by urease. It also adsorbs Ca, Mg and K ions but leaches phosphate ions which are then removed (along with F/sup -/ ions) by a bed of hydrous zirconium oxide. The sodium form of ZrP is used although other forms have been suggested for use. The work reported here describes some preliminary radiochemical studies on the mechanism of release of phosphate ions and its possible relationship to sodium ion-exchange. /sup 32/P labelled material (HHZrP) was used for elution experiments with deionized water and buffer solutions having the pH's 4.2, 7.0 and 9.2. Buffer solutions used were as supplied by BDH. Elution was at four different temperatures in the range 293 to 363/sup 0/C. In the second series of experiments HHZrP was suspended in a NaCl solution labelled with /sup 22/Na. From this, /sup 22/Na labelled ZrP (NaHZrP) was prepared and eluted in the same way as the HHZrP. Results are given and discussed.

  4. Process for etching zirconium metallic objects

    International Nuclear Information System (INIS)

    Panson, A.J.

    1988-01-01

    In a process for etching of zirconium metallic articles formed from zirconium or a zirconium alloy, wherein the zirconium metallic article is contacted with an aqueous hydrofluoric acid-nitric acid etching bath having an initial ratio of hydrofluoric acid to nitric acid and an initial concentration of hydrofluoric and nitric acids, the improvement, is described comprising: after etching of zirconium metallic articles in the bath for a period of time such that the etching rate has diminished from an initial rate to a lesser rate, adding hydrofluoric acid and nitric acid to the exhausted bath to adjust the concentration and ratio of hydrofluoric acid to nitric acid therein to a value substantially that of the initial concentration and ratio and thereby regenerate the etching solution without removal of dissolved zirconium therefrom; and etching further zirconium metallic articles in the regenerated etching bath

  5. Aqueous-Phase Acetic Acid Ketonization over Monoclinic Zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Cai, Qiuxia [Institute for Integrated Catalysis, Pacific Northwest; College; Lopez-Ruiz, Juan A. [Institute for Integrated Catalysis, Pacific Northwest; Cooper, Alan R. [Institute for Integrated Catalysis, Pacific Northwest; Wang, Jian-guo [College; Albrecht, Karl O. [Institute for Integrated Catalysis, Pacific Northwest; Mei, Donghai [Institute for Integrated Catalysis, Pacific Northwest

    2017-12-13

    The effect of aqueous phase on the acetic acid ketonization over monoclinic zirconia has been investigated using first-principles based density functional theory (DFT) calculations. To capture the aqueous phase chemistry over the solid zirconia catalyst surface, the aqueous phase is represented by 111 explicit water molecules with a liquid water density of 0.93 g/cm3 and the monoclinic zirconia is modeled by the most stable surface structure . The dynamic nature of aqueous phase/ interface was studied using ab initio molecular dynamics simulation, indicating that nearly half of the surface Zr sites are occupied by either adsorbed water molecules or hydroxyl groups at 550 K. DFT calculations show that the adsorption process of acetic acid from the liquid water phase to the surface is nearly thermodynamically neutral with a Gibbs free energy of -2.3 kJ/mol although the adsorption strength of acetic acid on the surface in aqueous phase is much stronger than in vapor phase. Therefore it is expected that the adsorption of acetic acid will dramatically affects aqueous phase ketonization reactivity over the monoclinic zirconia catalyst. Using the same ketonization mechanism via the β-keto acid intermediate, we have compared acetic acid ketonization to acetone in both vapor and aqueous phases. Our DFT calculation results show although the rate-determining step of the β-keto acid formation via the C-C coupling is not pronouncedly affected, the presence of liquid water molecules will dramatically affect dehydrogenation and hydrogenation steps via proton transfer mechanism. This work was financially supported by the United States Department of Energy (DOE)’s Bioenergy Technologies Office (BETO) and performed at the Pacific Northwest National Laboratory (PNNL). PNNL is a multi-program national laboratory operated for DOE by Battelle Memorial Institute. Computing time and advanced catalyst characterization use was granted by a user proposal at the William R. Wiley

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

    Science.gov (United States)

    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.

  7. Hydroxyapatite: Vibrational spectra and monoclinic to hexagonal phase transition

    Science.gov (United States)

    Slepko, Alexander; Demkov, Alexander A.

    2015-02-01

    Fundamental studies of biomaterials are necessary to deepen our understanding of their degradation and to develop cure for related illnesses. Biomineral hydroxyapatite Ca10(PO4)6(OH)2 is the main mineral constituent of mammal bone, and its synthetic analogues are used in biomedical applications. The mineral can be found in either hexagonal or monoclinic form. The transformation between these two phases is poorly understood, but knowing its mechanism may be critical to reversing processes in bone related to aging. Using density functional theory, we investigate the mechanisms of the phase transformation and estimate the transition temperature to be 680 K in fair agreement with the experimental temperature of 470 K. We also report the heat capacity of hydroxyapatite and a peculiarity in its phonon dispersion that might allow for non-destructive measurements of the crystal composition with applications in preventive medical screening for bone mineral loss.

  8. Management of waste cladding hulls. Part II. An assessment of zirconium pyrophoricity and recommendations for handling waste hulls

    International Nuclear Information System (INIS)

    Kullen, B.J.; Levitz, N.M.; Steindler, M.J.

    1977-11-01

    This report reviews experience and research related to the pyrophoricity of zirconium and zirconium alloys. The results of recent investigations of the behavior of Zircaloy and some observations of industrial handling and treatment of Zircaloy tubing and scrap are also discussed. A model for the management of waste Zircaloy cladding hulls from light water reactor fuel reprocessing is offered, based on an evaluation of the reviewed information. It is concluded that waste Zircaloy cladding hulls do not constitute a pyrophoric hazard if, following the model flow sheet, finely divided metal is oxidized during the management procedure. Steps alternative to the model are described which yield zirconium in deactivated form and also accomplish varying degrees of transuranic decontamination. Information collected into appendixes is (1) a collation of zirconium pyrophoricity data from the literature, (2) calculated radioactivity contents in Zircaloy cladding hulls from spent LWR fuels, and (3) results of a laboratory study on volatilization of zirconium from Zircaloy using HCl or Cl 2

  9. Zirconium ignition in exposed fuel channel

    Energy Technology Data Exchange (ETDEWEB)

    Elias, E., E-mail: merezra@technion.ac.il; Hasan, D.; Nekhamkin, Y.

    2015-05-15

    Highlights: • We demonstrate the idea of runaway zirconium–steam reactions in severe accidents in today's LWRs. • We predict the thermal-hydraulics conditions relevant to cladding oxidation in an exposed fuel channel of a partially uncovered core. • The Semenov theory of metal combustion is extended to define a criterion for runaway oxidation reaction in fuel cladding. - Abstract: A theoretical model based on simultaneous solution of the heat and mass transfer equations is developed for predicting the rate of thermo-chemical reaction between zirconium cladding and a hot steam environment. Ignition conditions relevant to cladding oxidation in an exposed fuel channel of a partially uncovered core are predicted based on the theory of metal combustion. A range of decay power, convective heat transfer coefficients, and initial temperatures leading to uncontrolled runaway cladding oxidation is identified. The model could be readily integrated as part of a fuel channel analysis code for predicting possible outcomes of different accident mitigation procedures in light water nuclear reactors under LOCA conditions.

  10. Zirconium oxide deposits (ZrO{sub 2}) and titanium oxide (TiO{sub 2}) on 304l stainless steel; Depositos de oxido de circonio (ZrO{sub 2}) y oxido de titanio (TiO{sub 2}) sobre acero inoxidable 304L

    Energy Technology Data Exchange (ETDEWEB)

    Davila N, M. L.

    2015-07-01

    This research project aims to carry out the surface and electrochemical characterization to obtain the optimum conditions of the hydrothermal deposits of zirconium oxide ZrO{sub 2} (baddeleyite) and titanium oxide TiO{sub 2} (anatase and rutile phases) on 304l stainless steel, simulating an inhibiting protective layer. 304l steel specimens were cut, pre-oxidized in water at a temperature of 288 degrees Celsius and 8 MPa, similar to those of a typical BWR conditions. From the titanium oxide anatase crystalline phase, the rutile phase was obtained by a heat treatment at 1000 degrees Celsius. The Sigma-Aldrich pre-oxidized powders and steel 304l were characterized using techniques of X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, chemical mapping and Raman spectrometry. The pre-oxidized steel has two oxide layers, an inner layer with nano metric crystals and another outer of larger crystals to 1μm, with the formation of hematite and magnetite, this predominating. The surface that contacted the sample holder has larger crystals. Hydrothermal deposits were carry out from suspensions of 10, 100 and 1000 ppm, of the crystal phases of anatase, rutile and baddeleyite, on the pre-oxidized steel at a temperature of 150 degrees Celsius for 2 and 7 days, samples were analyzed by X-ray diffraction, scanning electron microscopy, X-ray dispersive energy, Raman spectrometry and Tafel polarization. The suspension to 1000 ppm for 7 days coated surface most; the baddeleyite deposit is noticed more homogeneous than anatase and rutile. The deposit is favored when hematite and magnetite crystals are larger. The chemical mapping on deposits show that even after being immersed in water to 288 degrees Celsius during 30 days, the deposits are still present although a loss is observed. A reference electrode was assembled to conduct electrochemical tests of Tafel able to withstand a temperature of 288 degrees Celsius and pressure of 8 MPa. The baddeleyite deposit

  11. Chemistry, spectroscopy and isotope separation of zirconium and its compounds as revealed by laser diagnostics of laser produced metal beams

    International Nuclear Information System (INIS)

    Hackett, P.A.; Humphries, M.; Rayner, D.M.; Bourne, O.L.; Mitchell, A.

    1986-01-01

    Recent work from the author's laboratory on zirconium beams is reviewed. Zirconium metal beams have been produced by laser vaporization of solid zirconium targets coupled with supersonic expansion of helium gas. The resultant supersonic metal beam is shown to present an ideal environment for various spectroscopic techniques. The state distribution of zirconium atoms in the beam is obtained from low resolution laser induced fluorescence (LIF) studies. High resolution LIF studies give information on the hyperfine splitting in the ground state of the zirconium-91 isotope. Information on the hyperfine splitting in the excited state is obtained from quantum beat spectroscopy. Low resolution 2 color multiphoton ionization spectroscopy using a XeCl laser allows isotope separation of all isotopes of zirconium. These metal beams are highly reactive and can be used to produce novel chemical species. The results of two studies in which a reactant is added to the expansion gas are reported here. Zirconium oxide (ZrO), a molecule observed in the emission spectra of cool stars and in laboratory studies at high temperatures, is produced in a low temperature, collision free environment by adding small quantities of oxygen to the expansion gas. Zirconium fluoride (ZrF), a molecule previously unobserved, is produced by the addition of small quantities of CF/sub 4/

  12. Ceramic fiber-reinforced monoclinic celsian phase glass-ceramic matrix composite material

    Science.gov (United States)

    Bansal, Narottam P. (Inventor); Dicarlo, James A. (Inventor)

    1994-01-01

    A hyridopolysilazane-derived ceramic fiber reinforced monoclinic celsian phase barium aluminum silicate glass-ceramic matrix composite material is prepared by ball-milling an aqueous slurry of BAS glass powder and fine monoclinic celsian seeds. The fibers improve the mechanical strength and fracture toughness and with the matrix provide superior dielectric properties.

  13. Reflection of P and SV waves at the free surface of a monoclinic ...

    Indian Academy of Sciences (India)

    R.Narasimhan(krishtel emaging)1461 1996 Oct 15 13:05:22

    The propagation of plane waves in an anisotropic elastic medium possessing monoclinic symmetry is discussed. The expressions for ... Keywords. Anisotropic medium; elastic waves; monoclinic half-space; reflection coefficients. Proc. Indian Acad. Sci. ...... In contrast, for C < 0, the angle of reflec- tion is less than the angle of ...

  14. Corrosion of zirconium alloys in alternating pH environment

    International Nuclear Information System (INIS)

    Mayer, P.; Manolescu, A.V.

    1985-01-01

    Behaviour of two commercial alloys, Zircaloy-2 and zirconium-2.5 wt% niobium were investigated in an environment of alternating pH. Corrosion advancement and scale morphology of coupons exposed to aqueous solution of LiOH (pH 10.2 and 14) were followed as a function of temperature (300-360 degreesC) and time (up to 165 days). The test sequence consisted of short term exposure to high pH and re-exposure to low pH solutions for extended period of time followed by a short term test in high pH. The results of these tests and detailed post-corrosion analysis indicate a fundamental difference between the corrosion behaviour of these two materials. Both alloys corrode fast in high pH environments, but only zirconium-2.5 wt% niobium continues to form detectable new oxide in low pH solution

  15. Neutron activation of chlorine in zirconium and zirconium alloys use of the matrix as comparator

    International Nuclear Information System (INIS)

    Cohen, I.M.; Gomez, C.D.; Mila, M.I.

    1981-01-01

    A procedure is described for neutron activation analysis of chlorine in zirconium and zirconium alloys. Calculation of chlorine concentration is performed relative to zirconium concentration in the matrix in order to minimize effects of differences in irradiation and counting geometry. Principles of the method and the results obtained are discussed. (author)

  16. Spectrophotometric titration of zirconium in siliceous materials

    International Nuclear Information System (INIS)

    Sugawara, K.F.; Su, Y.-S.; Strzegowski, W.R.

    1978-01-01

    An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1 to 5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. (author)

  17. Voltammetric determination of zirconium using azo compounds

    International Nuclear Information System (INIS)

    Orshulyak, O.O.; Levitskaya, G.D.

    2008-01-01

    The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

  18. Applications for zirconium and columbium alloys

    International Nuclear Information System (INIS)

    Condliff, A.F.

    1986-01-01

    Currently, zirconium and columbium are used in a wide range of applications, overlapping only in the field of corrosion control. As a construction material, zirconium is primarily used by the nuclear power industry. The use of zirconium in the chemical processing industry (CPI) is, however, increasing steadily. Columbian alloys are primarily applied as superconducting alloys for research particle accelerators and fusion generators as well as in magnetic resonance imaging for medical diagnosis

  19. Synthesis of monoclinic potassium niobate nanowires that are stable at room temperature.

    Science.gov (United States)

    Kim, Seungwook; Lee, Ju-Hyuck; Lee, Jaeyeon; Kim, Sang-Woo; Kim, Myung Hwa; Park, Sungnam; Chung, Haegeun; Kim, Yong-Il; Kim, Woong

    2013-01-09

    We report the synthesis of KNbO(3) nanowires (NWs) with a monoclinic phase, a phase not observed in bulk KNbO(3) materials. The monoclinic NWs can be synthesized via a hydrothermal method using metallic Nb as a precursor. The NWs are metastable, and thermal treatment at ∼450 °C changed the monoclinic phase into the orthorhombic phase, which is the most stable phase of KNbO(3) at room temperature. Furthermore, we fabricated energy-harvesting nanogenerators by vertically aligning the NWs on SrTiO(3) substrates. The monoclinic NWs showed significantly better energy conversion characteristics than orthorhombic NWs. Moreover, the frequency-doubling efficiency of the monoclinic NWs was ∼3 times higher than that of orthorhombic NWs. This work may contribute to the synthesis of materials with new crystalline structures and hence improve the properties of the materials for various applications.

  20. Microhardness and microplasticity of zirconium nitride

    International Nuclear Information System (INIS)

    Neshpor, V.S.; Eron'yan, M.A.; Petrov, A.N.; Kravchik, A.E.

    1978-01-01

    To experimentally check the concentration dependence of microhardness of 4 group nitrides, microhardness of zirconium nitride compact samples was measured. The samples were obtained either by bulk saturation of zirconium iodide plates or by chemical precipitation from gas. As nitrogen content decreased within the limits of homogeneity of zirconium nitride samples where the concentration of admixed oxygen was low, the microhardness grew from 1500+-100 kg/mm 2 for ZrNsub(1.0) to 27000+-100 kg/mm 2 for ZrNsub(0.78). Microplasticity of zirconium nitride (resistance to fracture) decreased, as the concentration of nitrogen vacancies was growing

  1. Production kinetics of zirconium tetrachloride

    International Nuclear Information System (INIS)

    Sudjoko, D.; Masduki, B.; Sunardjo; Sulistyo, B.

    1996-01-01

    This research was intended to study the kinetics of zirconium tetrachloride production. The process was carried out in semi continuous reactor, equipped with heater, temperature controller, sublimator and scrubber. The variables investigated were time, temperature and the pellet forming pressure. Within the range of variables studied, the expression of the process in the chemical reaction controller region and diffusion controller region were both presented. (author)

  2. Thermodynamic Database for Zirconium Alloys

    International Nuclear Information System (INIS)

    Jerlerud Perez, Rosa

    2003-05-01

    For many decades zirconium alloys have been commonly used in the nuclear power industry as fuel cladding material. Besides their good corrosion resistance and acceptable mechanical properties the main reason of using these alloys is the low neutron absorption. Zirconium alloys are exposed to a very severe environment during the nuclear fission process and there is a demand for better design of this material. To meet this requirement a thermodynamic database is developed to support material designers. In this thesis some aspects about the development of a thermodynamic database for zirconium alloys are presented. A thermodynamic database represents an important facility in applying thermodynamic equilibrium calculations for a given material providing: 1) relevant information about the thermodynamic properties of the alloys e.g. enthalpies, activities, heat capacity, and 2) significant information for the manufacturing process e.g. heat treatment temperature. The basic information in the database is first the unary data, i.e. pure elements; those are taken from the compilation of the Scientific Group Thermodata Europe (SGTE) and then the binary and ternary systems. All phases present in those binary and ternary systems are described by means of the Gibbs energy dependence on composition and temperature. Many of those binary systems have been taken from published or unpublished works and others have been assessed in the present work. All the calculations have been made using Thermo C alc software and the representation of the Gibbs energy obtained by applying Calphad technique

  3. Corium Oxidation at Temperatures Above 2000 K

    International Nuclear Information System (INIS)

    Hagrman, Donald L.; Rempe, Joy L.

    2001-01-01

    A mechanistic model, based on a quasi-equilibrium analysis of oxidation reactions, is proposed for predicting high-temperature corium oxidation. The analysis suggests that oxide forming on the surface of corium containing uranium, zirconium, and iron is similar to the oxides formed on zirconium and uranium as long as there is a small percentage of unoxidized zirconium or uranium in the metallic phase. This is because of the higher affinity of zirconium and uranium for oxygen. Hence, oxidation rates and heat production rates are similar to (U,Zr) compounds until nearly all the uranium and zirconium in the corium oxidizes. Oxidation rates after this point are predicted to be similar to those implied by the oxide thickness present when the forming oxide ceases to be protective, and heat generation rates should be similar to those implied by iron oxidation, i.e., ∼4% of the zirconium oxidation heating rate.The maximum atomic ratio of unoxidized iron to unoxidized liquid zirconium plus uranium for the formation of a solid protective oxide below 2800 K is estimated for a temperature, T (in Kelvin), as follows:(unoxidized iron)/(unoxidized zirconium + turanium) = (1/28){5.7/exp[-(147 061 + 12.08T log(T) - 61.03T - 0.000555T 2 /1.986T)]} 1/2 .As long as this limit is not exceeded, either zirconium or uranium metal oxidation rates and heating describe the corium oxidation rate. If this limit is exceeded, diffusion of steam to the corium surface will limit the oxidation rate, and linear time-dependent growth of a nonprotective, mostly FeO, layer will occur below the protective (Zr,U) O 2 scale. When this happens, the oxidation should be at the constant rate given by the thickness of the protective layer. Heat generation should be similar to that of iron oxidation

  4. Corium Oxidation at Temperatures Above 2000 K

    Energy Technology Data Exchange (ETDEWEB)

    Hagrman, Donald Lee; Rempe, Joy Lynn

    2001-02-01

    A mechanistic model, based on a quasi-equilibrium analysis of oxidation reactions, is proposed for predicting high-temperature corium oxidation. The analysis suggests that oxide forming on the surface of corium containing uranium, zirconium, and iron is similar to the oxides formed on zirconium and uranium as long as there is a small percentage of unoxidized zirconium or uranium in the metallic phase. This is because of the higher affinity of zirconium and uranium for oxygen. Hence, oxidation rates and heat production rates are similar to (U,Zr) compounds until nearly all the uranium and zirconium in the corium oxidizes. Oxidation rates after this point are predicted to be similar to those implied by the oxide thickness present when the forming oxide ceases to be protective, and heat generation rates should be similar to those implied by iron oxidation, i.e., ~4% of the zirconium oxidation heating rate. The maximum atomic ratio of unoxidized iron to unoxidized liquid zirconium plus uranium for the formation of a solid protective oxide below 2800 K is estimated for a temperature, T (in Kelvin), as follows: (unoxidized iron)/(unoxidized zirconium + turanium) = (1/28){5.7/exp[-(147 061 + 12.08T log(T) - 61.03T - 0.000555T2/1.986T)]}1/2. As long as this limit is not exceeded, either zirconium or uranium metal oxidation rates and heating describe the corium oxidation rate. If this limit is exceeded, diffusion of steam to the corium surface will limit the oxidation rate, and linear time-dependent growth of a nonprotective, mostly FeO, layer will occur below the protective (Zr,U) O2 scale. When this happens, the oxidation should be at the constant rate given by the thickness of the protective layer. Heat generation should be similar to that of iron oxidation.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sridharan, Kumar [University of Wisconsin-Madison; Mariani, Robert [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bai, Xianming [Idaho National Lab. (INL), Idaho Falls, ID (United States); Xu, Peng [Westinghouse Electric Company; Lahoda, Ed [Westinghouse Electric Company

    2018-03-31

    Given the long-term goal of developing such coatings for use with nuclear reactor fuel cladding, this work describes results of oxidation and corrosion behavior of bulk zirconium-silicide and fabrication of zirconium-silicide coatings on zirconium-alloy test flats, tube configurations, and SiC test flats. In addition, boiling heat transfer of these modified surfaces (including ZrSi2 coating) during clad quenching experiments is discussed in detail. Oxidation of bulk ZrSi2 was found to be negligible compared to Zircaloy-4 (a common Zr-alloy cladding material) and mechanical integrity of ZrSi2 was superior to that of bulk Zr2Si at high temperatures in ambient air. Very interesting and unique multi-nanolayered composite of ZrO2 and SiO2 were observed. Physical model for the oxidation has been proposed wherein Zr–Si–O mixture undergoes a spinodal phase decomposition into ZrO2 and SiO2, which is manifested as a nanoscale assembly of alternating layer of the two oxides. Steam corrosion at high pressure (10.3 MPa) led to weight loss of ZrSi2 and produced oxide scale with depletion of silicon, possibly attributed to volatile silicon hydroxide, gaseous silicon monoxide, and a solubility of silicon dioxide in water. Only Zircon phase (ZrSiO4) formed during oxidation of ZrSi2 at 1400°C in air, and allowed for immobilization silicon species in oxide scale in the aqueous environments. Zirconium-silicide coatings (on zirconium-alloy substrates) investigated in this study were deposited primarily using magnetron sputter deposition method and slurry method, although powder spray deposition processes cold spray and thermal spray methods were also investigated. The optimized ZrSi2 sputtered coating exhibited a highly protective nature at elevated temperatures in ambient air by mitigating oxygen permeation to the underlying zirconium alloy substrate. The high oxidation resistance of the coating has been shown to be due to nanocrystalline SiO2 and ZrSiO4 phases in the amorphous

  6. Lifting the geometric frustration through a monoclinic distortion in “114” YBaFe4O7.0: Magnetism and transport

    International Nuclear Information System (INIS)

    Duffort, V.; Sarkar, T.; Caignaert, V.; Pralong, V.; Raveau, B.; Avdeev, M.; Cervellino, A.; Waerenborgh, J.C.; Tsipis, E.V.

    2013-01-01

    The possibility to lift the geometric frustration in the “114” stoichiomeric tetragonal oxide YBaFe 4 O 7.0 by decreasing the temperature has been investigated using neutron and synchrotron powder diffraction techniques. Besides the structural transition from tetragonal to monoclinic symmetry that appears at T S =180 K, a magnetic transition is observed below T N =95 K. The latter corresponds to a lifting of the 3D geometric frustration toward an antiferromagnetic long range ordering, never observed to date in a cubic based “114’” oxide. The magnetic structure, characterized by the propagation vector k 1 =(0,0,½), shows that one iron Fe2 exhibits a larger magnetic moment than the three others, suggesting a possible charge ordering according to the formula YBaFe 3+ Fe 3 2+ O 7.0 . The magnetic M(T) and χ′(T) curves, in agreement with neutron data, confirm the structural and magnetic transitions and evidence the coexistence of residual magnetic frustration. Moreover, the transport measurements show a resistive transition from a thermally activated conduction mechanism to a variable range hopping mechanism at T S =180 K, with a significant increase of the dependence of the resistivity vs. temperature. Mössbauer spectroscopy clearly evidences a change in the electronic configuration of the iron framework at the structural transition as well as coexistence of several oxidation states. The role of barium underbonding in these transitions is discussed. - Graphical abstract: Atomic displacements at the tetragonal-monoclinic transition in YBaFe 4 O 7 . Display Omitted - Highlights: • The structural and magnetic phase transitions of YBaFe 4 O 7 were studied below room temperature. • The tetragonal to monoclinic transition, characterized by NPD and SXRD, was studied using mode crystallography approach. • Monoclinic distortion allows the lifting of the geometrical frustration on the iron sublattice, leading to AF order at T=95 K

  7. Analysis of hydrogen in zirconium metallic

    International Nuclear Information System (INIS)

    Rodrigues, A.N.; Vega Bustillos, J.O.W.

    1991-02-01

    Determination of hydrogen in zirconium metallic have been performed using the hot vacuum extraction system and the gas chromatographic technique. The zirconium metallic samples were hydrieded by electrolitic technique at difference temperatures and times, then the samples were annealing at vacuum and eatching by fluoridric acid solution. The details of the hydrieded process, analytical technique and the data obtained are discussed. (author)

  8. Localized deformation of zirconium-liner tube

    International Nuclear Information System (INIS)

    Nagase, Fumihisa; Uchida, Masaaki

    1988-03-01

    Zirconium-liner tube has come to be used in BWR. Zirconium liner mitigates the localized stress produced by the pellet-cladding interaction (PCI). In this study, simulating the ridging, stresses were applied to the inner surfaces of zirconium-liner tubes and Zircaloy-2 tubes, and, to investigate the mechanism and the extent of the effect, the behavior of zirconium liner was examined. As the result of examination, stress was concentrated especially at the edge of the deformed region, where zirconium liner was highly deformed. Even after high stress was applied, the deformation of Zircaloy part was small, since almost the concentrated stress was mitigated by the deformation of zirconium liner. In addition, stress and strain distributions in the cross section of specimen were calculated with a computer code FEMAXI-III. The results also showed that zirconium liner mitigated the localized stress in Zircaloy, although the affected zone was restricted to the region near the boundary between zirconium liner and Zircaloy. (author)

  9. In situ TEM observation of the growth and decomposition of monoclinic W18O49 nanowires

    International Nuclear Information System (INIS)

    Chen, C L; Mori, H

    2009-01-01

    The growth of monoclinic W 18 O 49 nanowires by heat treatment of a tungsten filament at ∼873 K and the decomposition of these nanowires under 200 keV electron irradiation at ∼1023 K have been investigated using in situ transmission electron microscopy (TEM). In situ TEM observation of the growth confirmed the vapor-solid growth mechanism of the monoclinic W 18 O 49 nanowires. In situ irradiation experiments revealed the formation of metallic bcc tungsten from monoclinic W 18 O 49 nanowires under 200 keV electron irradiation.

  10. Phase coexistence in ferroelectric solid solutions: Formation of monoclinic phase with enhanced piezoelectricity

    Directory of Open Access Journals (Sweden)

    Xiaoyan Lu

    2016-10-01

    Full Text Available Phase morphology and corresponding piezoelectricity in ferroelectric solid solutions were studied by using a phenomenological theory with the consideration of phase coexistence. Results have shown that phases with similar energy potentials can coexist, thus induce interfacial stresses which lead to the formation of adaptive monoclinic phases. A new tetragonal-like monoclinic to rhombohedral-like monoclinic phase transition was predicted in a shear stress state. Enhanced piezoelectricity can be achieved by manipulating the stress state close to a critical stress field. Phase coexistence is universal in ferroelectric solid solutions and may provide a way to optimize ultra-fine structures and proper stress states to achieve ultrahigh piezoelectricity.

  11. Zirconium behaviour in purex process solutions

    International Nuclear Information System (INIS)

    Shu, J.

    1982-01-01

    The extraction behaviour of zirconium, as fission product, in TBP/diluent- HNO 3 -H 2 O systems, simulating Purex solutions, is studied. The main purpose is to attain an increasing in the zirconium decontamination factor by adjusting the extraction parameters. Equilibrium diagram, TBP concentration, aqueous:organic ratio, salting-out effects and, uranium loading in the organic phase were the main factors studied. All these experiments had been made with zirconium in the 10 - 2 - 10 - 3 concentration range. The extractant degradation products influence uppon the zirconium behaviour was also verified. With the obtained data it was possible to introduce some modification in the standard Purex flow-sheet in order to obtain the uranium product with higher zirconium decontamination. (Author) [pt

  12. Methods for the preparation of ultra-pure anhydrous zirconium tetrafluoride from zirconium tetraborohydride, researches in connection with halide glasses

    International Nuclear Information System (INIS)

    Tortevois, R.

    1990-01-01

    The synthesis of ultrapure zirconium tetrafluoride, the main component of fluorozirconate based optical fibers, was successfully attempted from zirconium tetraborohydride. Of the fluorinating agents used, nitrogen trifluoride doesn't react with zirconium tetraborohydride while xenon difluoride reacts too violently and leads to phases which contain boron. The fluorination in a compatible solvent enabled us to minimize the degradation. The best results were obtained with the fluorination of Zr(BH 4 ) 4 dissolved in CFCl 3 at -40 deg C by anhydrous HF. Using several analytical methods such as graphite furnace atomic absorption and proton activation, we analyzed the purity. The degree of transition element impurities is less than the ppm level for ZrF 4 . The dehydration of ZrF 4 ,H 2 O and ZrF 4 ,3H 2 O at room temperature by CIF 3 in gaseous and liquid state was also investigated. At exceptionally low temperature, this process allows oxide and oxyfluoride components to be reduced

  13. Optical properties of zirconium oxynitride films: The effect of composition, electronic and crystalline structures

    Energy Technology Data Exchange (ETDEWEB)

    Carvalho, P. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Borges, J., E-mail: joelborges@fisica.uminho.pt [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Department of Control Engineering, Faculty of Electrical Engineering, Czech Technical University in Prague, Technická 2, Prague 6 (Czech Republic); Rodrigues, M.S. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Barradas, N.P. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139,7), 2695-066 Bobadela LRS (Portugal); Alves, E. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisbon (Portugal); Espinós, J.P.; González-Elipe, A.R. [Instituto de Ciencia de Materiales de Sevilla (CSIC-University Sevilla), Avda. Américo Vespucio 49, 41092 Sevilla (Spain); Cunha, L.; Marques, L.; Vasilevskiy, M.I.; Vaz, F. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal)

    2015-12-15

    Highlights: • Optical behaviour of ZrO{sub x}N{sub y} films were correlated with structural properties. • A continuous depopulation of the d-band and an opening of an energy gap was observed. • Drude–Lorentz parameters changed for the metallic samples. • Optical bandgap of the films increases with non-metallic elements incorporation. - Abstract: This work is devoted to the investigation of zirconium oxynitride (ZrO{sub x}N{sub y}) films with varied optical responses prompted by the variations in their compositional and structural properties. The films were prepared by dc reactive magnetron sputtering of Zr, using Ar and a reactive gas mixture of N{sub 2} + O{sub 2} (17:3). The colour of the films changed from metallic-like, very bright yellow-pale and golden yellow, for low gas flows to red-brownish for intermediate gas flows. Associated to this colour change there was a significant decrease of brightness. With further increase of the reactive gas flow, the colour of the samples changed from red-brownish to dark blue or even to interference colourations. The variations in composition disclosed the existence of four different zones, which were found to be closely related with the variations in the crystalline structure. XRD analysis revealed the change from a B1 NaCl face-centred cubic zirconium nitride-type phase for films prepared with low reactive gas flows, towards a poorly crystallized over-stoichiometric nitride phase, which may be similar to that of Zr{sub 3}N{sub 4} with some probable oxygen inclusions within nitrogen positions, for films prepared with intermediate reactive gas flows. For high reactive gas flows, the films developed an oxynitride-type phase, similar to that of γ-Zr{sub 2}ON{sub 2} with some oxygen atoms occupying some of the nitrogen positions, evolving to a ZrO{sub 2} monoclinic type structure within the zone where films were prepared with relatively high reactive gas flows. The analysis carried out by reflected electron energy

  14. Nanoscale monoclinic domains in epitaxial SrRuO3 thin films deposited by pulsed laser deposition

    Science.gov (United States)

    Ghica, C.; Negrea, R. F.; Nistor, L. C.; Chirila, C. F.; Pintilie, L.

    2014-07-01

    In this paper, we analyze the structural distortions observed by transmission electron microscopy in thin epitaxial SrRuO3 layers used as bottom electrodes in multiferroic coatings onto SrTiO3 substrates for future multiferroic devices. Regardless of the nature and architecture of the multilayer oxides deposited on the top of the SrRuO3 thin films, selected area electron diffraction patterns systematically revealed the presence of faint diffraction spots appearing in forbidden positions for the SrRuO3 orthorhombic structure. High-resolution transmission electron microscopy (HRTEM) combined with Geometric Phase Analysis (GPA) evidenced the origin of these forbidden diffraction spots in the presence of structurally disordered nanometric domains in the SrRuO3 bottom layers, resulting from a strain-driven phase transformation. The local high compressive strain (-4% ÷ -5%) measured by GPA in the HRTEM images induces a local orthorhombic to monoclinic phase transition by a cooperative rotation of the RuO6 octahedra. A further confirmation of the origin of the forbidden diffraction spots comes from the simulated diffraction patterns obtained from a monoclinic disordered SrRuO3 structure.

  15. Hydrogen desorption kinetics from zirconium hydride and zirconium metal in vacuum

    International Nuclear Information System (INIS)

    Hu, Xunxiang; Terrani, Kurt A.; Wirth, Brian D.

    2014-01-01

    The kinetics of hydrogen desorption from zirconium hydride is important in many nuclear design and safety applications. In this paper, a coordinated experimental and modeling study has been used to explicitly demonstrate the applicability of existing kinetic theories for hydrogen desorption from zirconium hydride and α-zirconium. A static synthesis method was used to produce δ-zirconium hydride, and the crystallographic phases of the zirconium hydride were confirmed by X-ray diffraction (XRD). Three obvious stages, involving δ-zirconium hydride, a two-phase region, and α-zirconium, were observed in the hydrogen desorption spectra of two zirconium hydride specimens with H/Zr ratios of 1.62 and 1.64, respectively, which were obtained using thermal desorption spectroscopy (TDS). A continuous, one-dimensional, two-phase moving boundary model, coupled with the zero- and second-order kinetics of hydrogen desorption from δ-zirconium hydride and α-zirconium, respectively, has been developed to reproduce the TDS experimental results. A comparison of the modeling predictions with the experimental results indicates that a zero-order kinetic model is valid for description of hydrogen flux away from the δ-hydride phase, and that a second-order kinetic model works well for hydrogen desorption from α-Zr if the activation energy of desorption is optimized to be 70% of the value reported in the literature

  16. Strengthening and elongation mechanism of Lanthanum-doped Titanium-Zirconium-Molybdenum alloy

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Ping, E-mail: huping1985@126.com [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Jinduicheng Molybdenum Co., Ltd., Xi’an 710068 (China); Hu, Bo-liang; Wang, Kuai-she; Song, Rui; Yang, Fan [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Yu, Zhi-tao [Ruifulai Tungsten & Molybdenum Co., Ltd., Xi’an 721914 (China); Tan, Jiang-fei [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Cao, Wei-cheng; Liu, Dong-xin; An, Geng [Jinduicheng Molybdenum Co., Ltd., Xi’an 710068 (China); Guo, Lei [Ruifulai Tungsten & Molybdenum Co., Ltd., Xi’an 721914 (China); Yu, Hai-liang [School of Mechanical, Materials and Mechatronics Engineering, University of Wollongong, NSW 2522 (Australia)

    2016-12-15

    The microstructural contributes to understand the strengthening and elongation mechanism in Lanthanum-doped Titanium-Zirconium-Molybdenum alloy. Lanthanum oxide particles not only act as heterogeneous nucleation core, but also act as the second phase to hinder the grain growth during sintering crystallization. The molybdenum substrate formed sub-grain under the effect of second phase when the alloy rolled to plate.

  17. Passivation of mechanically polished, chemically etched and anodized zirconium in various aqueous solutions: Impedance measurements

    International Nuclear Information System (INIS)

    Abo-Elenien, G.M.; Abdel-Salam, O.E.

    1987-01-01

    Zirconium and its alloys are finding increasing applications especially in water-cooled nuclear reactors. Because of the fact that zirconium is electronegative (E 0 = -1.529V) its corrosion resistance in aqueous solutions is largely determined by the existence of a thin oxide film on its surface. The structure and properties of this film depend in the first place on the method of surface pre-treatment. This paper presents an experimental study of the nature of the oxide film on mechanically polished, chemically etched and anodized zirconium. Ac impedance measurements carried out in various acidic, neutral and alkaline solutions show that the film thickness depends on the method of surface pre-treatment and the type of electrolyte solution. The variation of the potential and impedance during anodization of zirconium at low current density indicates that the initial stages of polarization consist of oxide build-up at a rate dependent on the nature of the electrode surface and the electrolyte. Oxygen evolution commences at a stage where oxide thickening starts to decline. The effect of frequency on the measured impedance indicates that the surface reactivity, and hence the corrosion rate, decreases in the following order: mechanically polished > chemically etched > anodized

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

    Science.gov (United States)

    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.

  19. Synthesis of zirconium dioxide by ultrasound assisted precipitation: effect of calcination temperature.

    Science.gov (United States)

    Prasad, Krishnamurthy; Pinjari, D V; Pandit, A B; Mhaske, S T

    2011-09-01

    Nanostructured zirconium dioxide was synthesized from zirconyl nitrate using both conventional and ultrasound assisted precipitation in alkaline medium. The synthesized samples were calcinated at temperatures ranging from 400°C to 900°C in steps of 100°C. The ZrO(2) specimens were characterized using X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The thermal characteristics of the samples were studied via Differential Scanning Calorimetry-Thermo-Gravimetry Analysis (DSC-TGA). The influence of the calcination temperature on the phase transformation process from monoclinic to tetragonal to cubic zirconia and its consequent effect on the crystallite size and % crystallinity of the synthesized ZrO(2) was studied and interpreted. It was observed that the ultrasound assisted technique helped to hasten to the phase transformation and also at some point resulted in phase stabilization of the synthesized zirconia. Copyright © 2011 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

    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).

  1. X-ray K-absorption edge of zirconium in some perovskite type zirconates

    Energy Technology Data Exchange (ETDEWEB)

    Chougule, B K; Patil, R N [Shivaji Univ., Kolhapur (India). Dept. of Physics

    1979-01-01

    The chemical shifts in the X-ray K-absorption edges of zirconium in the zirconates of calcium, strontium, barium and lead and zirconium oxide have been investigated employing a 400 mm bent crystal X-ray spectrograph. It has been found that the discontinuity shifts towards the high energy side with respect to that in the pure metal and that the chemical shift depends upon the size of the next nearest cation. The larger the size of the cation, smaller is the chemical shift. Dependence of the shift on the crystal structure and the packing factor of the perovskite is also reported.

  2. Dissolution of anodic zirconium dioxide films in aqueous media

    International Nuclear Information System (INIS)

    Merati, A.; Cox, B.

    1999-01-01

    Zirconium with a low thermal neutron cross section, good corrosion resistance in high-temperature water, and high thermal conductivity is an ideal material for nuclear reactors. Its good resistance to water and steam at reactor temperatures is of the greatest interest to nuclear fuel designers. Dissolution of zirconium dioxide (ZrO 2 ) films in aggressive media was investigated. The extent of uniform and localized dissolution was measured by ultraviolet-visible (UV-VIS) spectrometry and an alternating current (AC) impedance test, respectively. Scanning electron microscopy (SEM) showed the extent of dissolution of ZrO 2 was a function only of the fluoride ion content and pH of the medium. Cathodic polarization was used to identify the preferred sites for localized dissolution of the oxide film. In 0.1 M potassium bifluoride (KHF 2 ), both uniform thinning and local breakdown of the oxide were observed. Within the limits of the investigating techniques, no evidence of dissolution was observed in the other solutions tested: 0.5 M sulfuric acid (H 2 SO 4 ). 1.0 M nitric acid (HNO 3 ), 5 M hydrochloric acid (HCl), or 0.1 M potassium fluoride (KF). In areas around iron-containing particles, fine cracks in the anodic oxide at prior metal grain boundaries and arrays of cracks in the oxide associated with residual scratches from the initial specimen preparation were the preferred spots for localized dissolution of the oxide film. Iron precipitates immediately below the surface of the oxide layer increased the local electrical conductivity. Enrichment of iron in the oxide matrix around these precipitates during the anodization process appeared to cause prospective spots, acting as anodic sites for pH formation

  3. Preparation and thermochemical stability of uranium-zirconium-carbonitrides

    International Nuclear Information System (INIS)

    Kouhsen, C.

    1975-08-01

    This investigation deals with the preparation and the thermochemical stability of uranium-zirconium-carbonitrides as well as with the mechanism of (U,Zr) (C,N)-preparation by carbothermic reduction of uranium-zirconium-oxide. Single-phase (U,Zr) (C,N)-solid solutions with U:Zr-propertions of 3:1, 1:1, and 1:3 were prepared from oxide powder. The thermochemical stability of the (U,Zr) (C,N)-solid solutions against carbon was measured for varying Zr- and N-contents and for several temperatures; the results indicate an increase of the uranium carbide stability potential by the formation of (U,Zr) (C,N)-solid solutions. The thermodynamic properties ΔG 0 , ΔH 0 , and ΔS 0 were calculated and the correlation between the M(C,N)-lattice constant and the N-content was evaluated. Through an intensive investigation of the reaction mechanism, several different reaction paths were found; for each of them the characteristical diffusion of matter was explained by means of the microsections. It was shown that the Zr-concentration of the oxide reactant and the heating rate during the carbothermic reduction influence the species of the reaction product, especially the homogeneity of the (U,Zr) (C,N)-solid solution. (orig.) [de

  4. Inhibitors for the corrosion of reactive metals: titanium and zirconium and their alloys in acid media

    International Nuclear Information System (INIS)

    Petit, J.A.; Chatainier, G.; Dabosi, F.

    1981-01-01

    The search for effective corrosion inhibitors for titanium and zirconium in acid media is growing because of the considerable increase in the use of these materials in chemical process equipment. It still remains limited, as appears from this review, because of the exceptionally high corrosion resistance of the metals. Titanium has received the greater attention. Its corrosion rate can be lowered by introduction in the medium of multivalent ions, inorganic and organic oxidants. Care should be taken to hold the concentration at a level exceeding some critical value, otherwise the corrosion rate increases. Complexing organic agents do not show such hazardous behaviour. The very rapid corrosion of titanium and zirconium in fluoride media may be lessened by complexing the fluoride ions. Though rarely encountered, localized corrosion may be avoided by using inhibitors. In some cases good corrosion inhibitors for titanium are dissolution accelerators for zirconium. (author)

  5. URANIUM DECONTAMINATION WITH RESPECT TO ZIRCONIUM

    Science.gov (United States)

    Vogler, S.; Beederman, M.

    1961-05-01

    A process is given for separating uranium values from a nitric acid aqueous solution containing uranyl values, zirconium values and tetravalent plutonium values. The process comprises contacting said solution with a substantially water-immiscible liquid organic solvent containing alkyl phosphate, separating an organic extract phase containing the uranium, zirconium, and tetravalent plutonium values from an aqueous raffinate, contacting said organic extract phase with an aqueous solution 2M to 7M in nitric acid and also containing an oxalate ion-containing substance, and separating a uranium- containing organic raffinate from aqueous zirconium- and plutonium-containing extract phase.

  6. Chemistry of titanium, zirconium and thorium picramates

    International Nuclear Information System (INIS)

    Srivastava, R.S.; Agrawal, S.P.; Bhargava, H.N.

    1976-01-01

    Picramates of titanium, zirconium and thorium are prepared by treating the aqueous sulphate, chloride and nitrate solutions with sodium picramate. Micro-analysis, colorimetry and spectrophotometry are used to establish the compositions (metal : ligand ratio) of these picramates as 1 : 2 (for titanium and zirconium) and 1 : 4 (for thorium). IR studies indicate H 2 N → Me coordination (where Me denotes the metal). A number of explosive properties of these picramates point to the fact that the zirconium picramate is thermally more stable than the picramates of titanium and thorium. (orig.) [de

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

    Science.gov (United States)

    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.

  8. Production of nuclear grade zirconium: A review

    Energy Technology Data Exchange (ETDEWEB)

    Xu, L., E-mail: L.Xu-2@tudelft.nl [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands); Xiao, Y. [Department of Metallurgical Engineering, Anhui University of Technology, Ma' anshan 243002 (China); Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Sandwijk, A. van [Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Xu, Q. [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Yang, Y. [Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands)

    2015-11-15

    Zirconium is an ideal material for nuclear reactors due to its low absorption cross-section for thermal neutrons, whereas the typically contained hafnium with strong neutron-absorption is very harmful for zirconium as a fuel cladding material. This paper provides an overview of the processes for nuclear grade zirconium production with emphasis on the methods of Zr–Hf separation. The separation processes are roughly classified into hydro- and pyrometallurgical routes. The known pyrometallurgical Zr–Hf separation methods are discussed based on the following reaction features: redox characteristics, volatility, electrochemical properties and molten salt–metal equilibrium. In the present paper, the available Zr–Hf separation technologies are compared. The advantages and disadvantages as well as future directions of research and development for nuclear grade zirconium production are discussed.

  9. Towards an understanding of zirconium alloy corrosion

    International Nuclear Information System (INIS)

    Cox, B.

    1976-08-01

    A brief historical summary is given of the development of a programme for understanding the corrosion mechanisms operating for zirconium alloys. A general summary is given of the progress made, so far, in carrying through this programme. (author)

  10. Zirconium determination in refractories (gravimetric method)

    International Nuclear Information System (INIS)

    Capiotto, N.; Narahashi, Y.; Perish, C.G.; Souza, J.R.

    1991-01-01

    The zirconium determination in refractories is described, consisting in two separation methods for eliminating the interferences. The formatted product is calcined at 1100 0 C and determined gravimetrically as Zr P z 07. (author)

  11. Joint titrimetric determination of zirconium and hafnium

    International Nuclear Information System (INIS)

    Vazquez, Cristina; Botbol, Moises; Bianco de Salas, G.N.; Cornell de Casas, M.I.

    1980-01-01

    A method for the joint titrimetric determination of zirconium and hafnium, which are elements of similar chemical behaviour, is described. The disodic salt of the ethylendiaminetetracetic acid (EDTA) is used for titration, while xilenol orange serves as final point indicator. Prior to titration it is important to evaporate with sulfuric acid, the solution resulting from the zirconium depolymerization process, to adjust the acidity and to eliminate any interferences. The method, that allows the quick and precise determination of zirconium and hafnium in quantities comprised between 0.01 and mg, was applied to the analysis of raw materials and of intermediate and final products in the fabrication of zirconium sponge and zircaloy. (M.E.L.) [es

  12. Zirconium determination in refractories (gravimetric method)

    International Nuclear Information System (INIS)

    Capiotto, N.; Narahashi, Y.; Perish, P.G.; Souza, J.R. de

    1991-01-01

    A gravimetric method for zirconium determination in refractories is described. X-ray fluorescence analysis is also employed in this experiment and considerations about interfering elements are presented. (M.V.M.)

  13. DISSOLUTION OF ZIRCONIUM AND ALLOYS THEREFOR

    Science.gov (United States)

    Swanson, J.L.

    1961-07-11

    The dissolution of zirconium cladding in a water solution of ammonium fluoride and ammonium nitrate is described. The method finds particular utility in processing spent fuel elements for nuclear reactors. The zirconium cladding is first dissolved in a water solution of ammonium fluoride and ammonium nitrate; insoluble uranium and plutonium fiuorides formed by attack of the solvent on the fuel materiai of the fuel element are then separated from the solution, and the fuel materiai is dissolved in another solution.

  14. METHOD OF IMPROVING CORROSION RESISTANCE OF ZIRCONIUM

    Science.gov (United States)

    Shannon, D.W.

    1961-03-28

    An improved intermediate rinse for zirconium counteracts an anomalous deposit that often results in crevices and outof-the-way places when ordinary water is used to rinse away a strong fluoride etching solution designed to promote passivation of the metal. The intermediate rinse, which is used after the etching solution and before the water, is characterized by a complexing agent for fluoride ions such as aluminum or zirconium nitrates or chlorides.

  15. Difference in surface reactions between titanium and zirconium in Hanks' solution to elucidate mechanism of calcium phosphate formation on titanium using XPS and cathodic polarization

    International Nuclear Information System (INIS)

    Tsutsumi, Y.; Nishimura, D.; Doi, H.; Nomura, N.; Hanawa, T.

    2009-01-01

    Titanium and zirconium were immersed in Hanks' solution with and without calcium and phosphate ions, and the surfaces were characterized with X-ray photoelectron spectroscopy (XPS) to determine the mechanism of calcium phosphate formation on titanium in simulated body fluids and in a living body. In addition, they were cathodically polarized in the above solutions. XPS characterization and cathodic polarization revealed differences in the surface properties in the ability of calcium phosphate formation between titanium and zirconium. The surface oxide film on titanium is not completely oxidized and is relatively reactive; that on zirconium is more passive and protective than that on titanium. Neither calcium nor phosphate stably exists alone on titanium, and calcium phosphate is naturally formed on it; calcium phosphate formed on titanium is stable and protective. On the other hand, calcium is never incorporated on zirconium, while zirconium phosphate, which is easily formed on zirconium, is highly stable and protective. Our study presents new information regarding the surface property of titanium and demonstrates that the characteristics of titanium and zirconium may be applied to various medical devices and new surface modification techniques.

  16. Corrosion resistance and biocompatibility of zirconium oxynitride thin film growth by RF sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Cubillos, G. I.; Olaya, J. J.; Clavijo, D.; Alfonso, J. E. [Universidad Nacional de Colombia, Carrera 45 No. 26-85, AA 14490 Bogota D. C. (Colombia); Bethencourt, M., E-mail: jealfonsoo@unal.edu.co [Universidad de Cadiz, Centro Andaluz de Ciencia y Tecnologia Marinas, Departamento de Ciencia de los Materiales e Ingenieria Metalurgica y Quimica Inorganica, Av. Republica de Saharaui, Puerto Real, E-11510 Cadiz (Spain)

    2012-07-01

    Thin films of zirconium oxynitride were grown on common glass, silicon (100) and stainless steel 316 L substrates using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (Sem) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The corrosion resistance studies were made on samples of stainless steel 316 L coated and uncoated with Zr{sub x}N{sub y}O films, through of polarization curves. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316 L through proliferation and cellular adhesion. The XRD analysis shows that films deposited at 623 K, with a flow ratio {Phi}N{sub 2}/{Phi}O{sub 2} of 1.25 and a total deposit time of 30 minutes grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The Sem analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. The analysis of the corrosion resistant, shows that the stainless steel coated with the film was increased a factor 10. Finally; through the analysis of the biocompatibility we established that the films have a better surface than the substrate (stainless steel 316 L) in terms of the adhesion and proliferation of bone cells. (Author)

  17. Synthesis and biological characterization of zirconium oxynitride thin film growth by radio-frequency sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Cubillos, G.I. [Departamento de Química, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Olaya, J.J. [Facultad de Ingeniería, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Clavijo, D. [Facultad de Medicina, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Alfonso, J.E., E-mail: jealfonsoo@unal.edu.co [Grupo de materiales con Aplicaciones Tecnológicas, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Cardozo, C. [Instituto de Biotecnología, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia)

    2013-02-01

    Thin films of zirconium oxynitride were grown on common glass, silicon substrates (100) and on stainless steel 316L using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological, and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (SEM) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316L through proliferation and cellular adhesion. The XRD analysis showed that films deposited at 623 K, with a flow ratio ΦN{sub 2}/ΦO{sub 2} of 1.25 and a total deposit time of 30 min grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The SEM analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. Finally, through the analysis of the biocompatibility, we established that the films have a better surface than the substrate (stainless steel 316L) in terms of adhesion and proliferation of bone cells. - Highlights: ►ZrO{sub x}N{sub y} thin films were deposited using reactive radio-frequency magnetron sputtering. ►We studied the effect of deposition parameters on ZrO{sub x}N{sub y} thin films microstructure. ►We have been able to grow bone cells on ZrO{sub x}N{sub y} coated stainless steel 316L.

  18. Atomistic studies of cation transport in tetragonal ZrO2 during zirconium corrosion

    International Nuclear Information System (INIS)

    Bai, Xian-Ming; Zhang, Yongfeng; Tonks, Michael R.

    2015-01-01

    Zirconium alloys are the major fuel cladding materials in current reactors. The water-side corrosion is a significant degradation mechanism of these alloys. During corrosion, the transport of oxidizing species in zirconium dioxide (ZrO 2 ) determines the corrosion kinetics. Previously, it has been argued that the outward diffusion of cations is important for forming protective oxides. In this work, the migration of Zr defects in tetragonal ZrO 2 is studied with temperature accelerated dynamics and molecular dynamics simulations. The results show that Zr interstitials have anisotropic diffusion and migrate preferentially along the [001] or c direction in tetragonal ZrO 2 . The compressive stresses can increase the Zr interstitial migration barrier significantly. The migration of Zr interstitials at a grain boundary is much slower than in a bulk oxide. The implications of these atomistic simulation results in the Zr corrosion are discussed. (authors)

  19. Application of modified multiwall carbon nanotubes as a sorbent for zirconium (IV) adsorption from aqueous solution

    International Nuclear Information System (INIS)

    Yavari, R.; Davarkhah, R.

    2013-01-01

    Modified multiwall carbon nanotubes (MWCNTs) by nitric acid solution were used to investigate the adsorption behavior of zirconium from aqueous solution. Pristine and oxidized MWCNTs were characterized using nitrogen adsorption/desorption isotherm, Boehm's titration method, thermogravimetry analysis, transmission electron microscopy and Fourier transform infrared spectroscopy. The results showed that the surface properties of MWCNTs such as specific surface area, total pore volume, functional groups and the total number of acidic and basic sites were improved after oxidation. These improvements are responsible for their hydrophobic properties and consequently an easy dispersion in water and suitable active sites for more adsorption of zirconium. The adsorption of Zr(IV) as a function of initial concentration of zirconium, contact time, MWCNTs dosage, HCl and HNO 3 concentration and also ionic strength was investigated using a batch technique under ambient conditions. The experimental results indicated that sorption of Zr(IV) was strongly influenced by zirconium concentrations, oxidized MWCNTs content and acid pH values. The calculated correlation coefficient of the linear regressions values showed that Langmuir model fits the adsorption equilibrium data better than the Freundlich model. Kinetic data of sorption indicated that equilibrium was achieved within 60 min and the adsorption process can be described by the pseudo second-order reaction rate model. Based on the experimental results, surface complexation is the major mechanism for adsorption of Zr(IV) onto MWCNTs. Also, Study on the desorption process of zirconium showed that the complete recovery can be obtained using nitric or hydrochloric acids of 4 M. (author)

  20. Study of the cubic - to - monoclinic transformation in magnesia partially stabilized zirconia

    International Nuclear Information System (INIS)

    Muccillo, R.

    1988-01-01

    The transformation of the cubic phase to the stable monoclinic phase in ZrO 2 : 3%MgO quenched from 1450 0 C to RT has been studied by X-ray diffractometry in order to explain the thermal hysteresis in the electrical conductivity. The monoclinic-to-cubic ratio has been measured for samples annealed in the 500 0 C-1000 0 C temperature range. The results show that the decrease in the cubic phase content is the main responsible for the thermal hysteresis in the electrical conductivity of the magnesia partially stabilized zirconia solid electrolytes. (author) [pt

  1. Monoclinic mixed crystals of halogenomethanes CBr4-nCln (n = 0, ..., 4)

    International Nuclear Information System (INIS)

    Negrier, Philippe; Tamarit, Josep Ll.; Barrio, Maria; Pardo, Luis C.; Mondieig, Denise

    2007-01-01

    On the basis of the isostructural relationship between the low-temperature monoclinic (C2/c, Z = 32) phases of the halogenomethane CBr 4-n Cl n (n = 0, ..., 4), a set of mixed crystals has been analysed by means of high-resolution X-ray powder diffraction. It is shown that the monoclinic structure of pure and mixed crystals does not depend of the particularities of the dipolar (or dipole induced) interactions of the pure compound, neither on the composition of the mixed crystal, but on the relative content of the halogen atoms which controls the size of the molecule or the average molecule for the case of mixed crystals

  2. Artefacts in multimodal imaging of titanium, zirconium and binary titanium-zirconium alloy dental implants: an in vitro study.

    Science.gov (United States)

    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.

  3. Artefacts in multimodal imaging of titanium, zirconium and binary titanium–zirconium alloy dental implants: an in vitro study

    Science.gov (United States)

    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

  4. Electrochemical-metallothermic reduction of zirconium in molten salt solutions

    International Nuclear Information System (INIS)

    McLaughlin, D.F.; Talko, F.

    1990-01-01

    This patent describes a method for separating hafnium from zirconium of the type wherein a feed containing zirconium and hafnium chlorides is prepared from zirconium-hafnium chloride and the feed is introduced into a distillation column, which distillation column has a reboiler connected at the bottom and a reflux condenser connected at the top and wherein a hafnium chloride enriched stream is taken from the top of the column and a zirconium enriched chloride stream is taken from the bottom of the column. It comprises: reducing the zirconium enriched chloride stream taken from the distillation column to metal by electrochemically reducing an alkaline earth metal in a molten salt bath with the molten salt in the molten salt bath consisting essentially of a mixture of at least one alkali metal chloride and at least one alkaline earth metal chloride and zirconium chloride, with the reduced alkaline earth metal reacting with the zirconium chloride to produce zirconium metal and alkaline earth metal chloride

  5. A review of the inorganic and organometallic chemistry of zirconium

    International Nuclear Information System (INIS)

    Kalvins, A.K.

    1985-01-01

    The results of a literature review of the inorganic and organometallic chemistry of zirconium are presented. Compounds with physical and chemical properties compatible with the requirements of an ir laser zirconium isotope separation process have been identified

  6. Influence of irradiation and radiolysis on the corrosion rates and mechanisms of zirconium alloys

    International Nuclear Information System (INIS)

    Verlet, Romain

    2015-01-01

    The nuclear fuel of pressurized water reactors (PWR) in the form of uranium oxide UO 2 pellets (or MOX) is confined in a zirconium alloy cladding. This cladding is very important because it represents the first containment barrier against the release of fission products generated by the nuclear reaction to the external environment. Corrosion by the primary medium of zirconium alloys, particularly the Zircaloy-4, is one of the factors limiting the reactor residence time of the fuel rods (UO 2 pellets + cladding). To optimize core management and to extend the lifetime of the fuel rods in reactor, new alloys based on zirconium-niobium (M5) have been developed. However, the corrosion mechanisms of these are not completely understood because of the complexity of these materials, corrosion environment and the presence of radiation from the nuclear fuel. Therefore, this thesis specifically addresses the effects of radiolysis and defects induced by irradiation with ions in the matrix metal and the oxide layer on the corrosion rate of Zircaloy-4 and M5. The goal is to separate the influence of radiation damage to the metal, that relating to defects created in the oxide and that linked to radiolysis of the primary medium on the oxidation rate of zirconium alloys in reactor. 1) Regarding effect of irradiation of the metal on the oxidation rate: type dislocation loops appear and increase the oxidation rate of the two alloys. For M5, in addition to the first effect, a precipitation of fines needles of niobium reduced the solid solution of niobium concentration in the metal and ultimately in the oxide, which strongly reduces the oxidation rate of the alloy. 2) Regarding the effect of irradiation of the oxide layer on the oxidation rate: defects generated by the nuclear cascades in the oxide increase the oxidation rate of the two materials. For M5, germination of niobium enriched zones in irradiated oxide also causes a decrease of the niobium concentration in solid solution

  7. Influence de l’irradiation et de la radiolyse sur la vitesse et les mécanismes de corrosion des alliages de zirconium

    OpenAIRE

    Verlet , Romain

    2015-01-01

    The nuclear fuel of pressurized water reactors (PWR) in the form of uranium oxide UO2 pellets (or MOX) is confined in a zirconium alloy cladding. This cladding is very important because it represents the first containment barrier against the release of fission products generated by the nuclear reaction to the external environment. Corrosion by the primary medium of zirconium alloys, particularly the Zircaloy-4, is one of the factors limiting the reactor residence time of the fuel rods (UO2 pe...

  8. MULTILAYER COMPOSITE PLASMA COATINGS ON SCREEN PROTECTION ELEMENTS BASED ON ZIRCONIUM DIOXIDE

    Directory of Open Access Journals (Sweden)

    V. A. Okovity

    2017-01-01

    Full Text Available The paper contains results of investigations pertaining to an influence of plasma jet parameters (current, spraying distance, consumption of plasma formation gas (nitrogen, fractional composition of initial powder and degree of cooling with compressed air on anti-meteoric coating characteristics. Optimum modes (arc current 600 A; spray distance of 110 mm; consumption of plasma formation gas (nitrogen – 50 l/min; fractional composition of zirconium dioxide powder <50 μm; compressed air consumption for cooling – 1 m3/min; p = 4 bar make it possible to obtain anti-meteoric coatings based on zirconium dioxide with material utilization rate of 62 %, total ceramic layer porosity of 6 %. After exposure of compression plasma flows on a coating in the nitrogen atmosphere a cubic modification of zirconium oxide is considered as the main phase being present in the coating. The lattice parameter of cubic zirconium oxide modification is equal to 0.5174 nm. Taking into consideration usage of nitrogen as plasma formation substance its interaction with zirconium coating atoms occurs and zirconium nitride (ZrN is formed with a cubic crystal lattice (lattice parameter 0.4580 nm. Melting of pre-surface layer takes place and a depth of the melted layer is about 8 μm according to the results of a scanning electron microscopy. Pre-surface layer being crystallized after exposure to compression plasma flows is characterized by a homogeneous distribution of ele-ments and absence of pores formed in the process of coating formation. The coating structure is represented by a set of lar- ge (5–7 μm and small (1–2 μm zirconium oxide particles sintered against each other. Melting of coating surface layer and speed crystallization occur after the impact of compression plasma flows on the formed coating. Cracking of the surface layer arises due to origination of internal mechanical stresses in the crystallized part. While using a scanning electron microscopy a

  9. Minimization of zirconium chlorinator residues

    International Nuclear Information System (INIS)

    Green, G.K.; Harbuck, D.D.

    1995-01-01

    Zirconium chlorinator residues contain an array of rare earths, scandium, unreacted coke, and radioactive thorium and radium. Because of the radioactivity, the residues must be disposed in special waste containment facilities. As these sites become more congested, and with stricter environmental regulations, disposal of large volumes of wastes may become more difficult. To reduce the mass of disposed material, the US Bureau of Mines (USBM) developed technology to recover rare earths, thorium and radium, and unreacted coke from these residues. This technology employs an HCl leach to solubilize over 99% of the scandium and thorium, and over 90% of the rare earths. The leach liquor is processed through several solvent extraction stages to selectively recover scandium, thorium, and rare earths. The leach residue is further leached with an organic acid to solubilize radium, thus allowing unreacted coke to be recycled to the chlorinator. The thorium and radium waste products, which comprise only 2.1% of the original residue mass, can then be sent to the radioactive waste facility

  10. The chemical vapor deposition of zirconium carbide onto ceramic substrates

    International Nuclear Information System (INIS)

    Glass A, John Jr.; Palmisiano, Nick Jr.; Welsh R, Edward

    1999-01-01

    Zirconium carbide is an attractive ceramic material due to its unique properties such as high melting point, good thermal conductivity, and chemical resistance. The controlled preparation of zirconium carbide films of superstoichiometric, stoichiometric, and substoichiometric compositions has been achieved utilizing zirconium tetrachloride and methane precursor gases in an atmospheric pressure high temperature chemical vapor deposition system

  11. Processing fissile material mixtures containing zirconium and/or carbon

    Science.gov (United States)

    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.

  12. 40 CFR 721.9973 - Zirconium dichlorides (generic).

    Science.gov (United States)

    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...

  13. Removal of iron contaminant from zirconium chloride solution

    International Nuclear Information System (INIS)

    Voit, D.O.

    1992-01-01

    This patent describes a process for eliminating iron contaminant from an aqueous zirconium chloride solution that has been contaminated with FeCl 3 in a plant in which zirconium and hafnium chloride solutions are separated by a main MINK solvent extraction system and the FeCl 3 is normally removed from the zirconium chloride solution by a secondary MINK solvent extraction system

  14. Automatic measuring system of zirconium thickness for zirconium liner cladding tubes

    International Nuclear Information System (INIS)

    Matsui, K.; Yamaguchi, H.; Hiroshima, T.; Sakamoto, T.; Murayama, R.

    1985-01-01

    An automatic system of pure zirconium liner thickness for zirconium-zircaloy cladding tubes has been successfully developed. The system consists of three parts. (1) An ultrasonic thickness measuring method for mother tubes before cold rolling. (2) An electromagnetic thickness measuring method for the manufactured tubes. (3) An image processing method for the cross sectional view of the manufactured cut tube samples. In Japanese nuclear industry, zirconium-zircaloy cladding tubes have been tested in order to realize load following operation in the atomic power plant. In order to provide for the practical use in the near future, Sumitomo Metal Industries, Ltd. has been studied and established the practical manufacturing process of the zirconium liner cladding tubes. The zirconium-liner cladding tube is a duplex tube comprising an inner layer of pure zirconium bonded to zircaloy metallurgically. The thickness of the pure zirconium is about 10 % of the total wall thickness. Several types of the automatic thickness measuring methods have been investigated instead of the usual microscopic viewing method in which the liner thickness is measured by the microscopic cross sectional view of the cut tube samples

  15. Radiochemical neutron activation analysis of zirconium and zirconium-niobium alloys

    International Nuclear Information System (INIS)

    Tashimova, F.A.; Sadikov, I.I.; Salimov, M.

    2004-01-01

    Full text: Zirconium and zirconium-niobium alloys are used on nuclear technology, as fuel cladding of nuclear reactors. Their nuclear-physical, mechanical and thermophysical properties are influenced them matrix and impurity composition, therefore determination of matrix and impurity content of these materials is a very important task. Neutron activation analysis is one from multielemental and high sensible techniques that are widely applied in analysis of high purity materials. Investigation of nuclear-physical characteristics of zirconium has shown that instrumental variant NAA is unusable for analysis due to high radioactivity of a matrix. Therefore it is necessary carrying out radiochemical separation of impurity radionuclides from matrix. Study of the literature datum have shown, that zirconium and niobium are very well extracted from muriatic solution with 5% tributyl phosphineoxide (TBPO) solution in toluene and 0,75 M solution of di-2-ethyl hexyl phosphoric acid (HDEHP) in cyclohexanone. Investigation of these elements extraction in these systems has shown that more effective and selective separation of matrix radionuclides is achieved in HDEHP-3M HCI system. This system is also extracted and hafnium, witch is an accompanying element of zirconium and its high content prevented determination of other impurity elements in sample. Therefore we used extraction system HDEHP-3M HCl for analysis of zirconium and zirconium-niobium alloys in chromatographic variant. By measurement of distribution profile of a matrix and of elution curve of determined elements is established, that for effective separation of impurity and matrix radionuclides there is enough chromatographic column with diameter 1 cm and height of a sorbent layer 7 cm, thus volume of elute, necessary for complete elution of determinate elements is 35-40 ml. On the basis of the carried out researches the technique of radiochemical NAA of high purity zirconium and zirconium-niobium alloy, which allows to

  16. Experimental and thermodynamic study of the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems

    International Nuclear Information System (INIS)

    Jourdan, J.

    2009-11-01

    This work is a contribution to the development of innovative concepts for fuel cladding in pressurized water nuclear reactors. This concept implies the insertion of rare earth (erbium and gadolinium) in the zirconium fuel cladding. The determination of phase equilibria in the systems is essential prior to the implementation of such a promising solution. This study consisted in an experimental determination of the erbium-zirconium phase diagram. For this, we used many different techniques in order to obtain diagram data such as solubility limits, solidus, liquidus or invariant temperatures. These data allowed us to present a new diagram, very different from the previous one available in the literature. We also assessed the diagram using the CALPHAD approach. In the gadolinium-zirconium system, we determined experimentally the solubility limits. Those limits had never been determined before, and the values we obtained showed a very good agreement with the experimental and assessed versions of the diagram. Because these alloys are subjected to oxygen diffusion throughout their life, we focused our attention on the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems. The first system has been investigated experimentally. The alloys fabrication has been performed using powder metallurgy. In order to obtain pure raw materials, we fabricated powder from erbium and zirconium bulk metals using hydrogen absorption/desorption. The characterisation of the ternary pellets allowed the determination of two ternary isothermal sections at 800 and 1100 C. For the gadolinium-oxygen-zirconium system, we calculated the phase equilibria at temperatures ranging from 800 to 1100 C, using a homemade database compiled from literature assessments of the oxygen-zirconium, gadolinium-zirconium and gadolinia-zirconia systems. Finally, we determined the mechanical properties, in connexion with the microstructure, of industrial quality alloys in order to identify the influence of

  17. The coercive force of fine particles of monoclinic pyrrhotite (Fe7S8 ...

    African Journals Online (AJOL)

    The temperature dependence of coercive force (Hc) between 77 K and 600 K has been investigated for fine particles of monoclinic pyrrhotite (Fe7S8) of < 1 mm and 1- 30 mm particle sizes. The study has shown that Hc is strongly dependent on temperature, as temperature rises above room temperature (293 K) to near the ...

  18. Reflection of P and SV waves at the free surface of a monoclinic ...

    Indian Academy of Sciences (India)

    The propagation of plane waves in an anisotropic elastic medium possessing monoclinic symmetry is discussed. The expressions for the phase velocity of qP and qSV waves propagating in the plane of elastic symmetry are obtained in terms of the direction cosines of the propagation vector. It is shown that, in general, ...

  19. Crystalline and magnetic ordering in the monoclinic phase of the layered perovskite PAMC

    DEFF Research Database (Denmark)

    Harris, P.; Lebech, B.; Achiwa, N.

    1994-01-01

    A single-crystal elastic neutron scattering experiment between 4.2 and 115 K has been performed on the low-temperature monoclinic zeta phase of the layered perovskite bis(propylammonium) manganesetetrachloride (PAMC). The crystalline structure is commensurately modulated, with a modulation vector...

  20. Possible bicollinear nematic state with monoclinic lattice distortions in iron telluride compounds

    Energy Technology Data Exchange (ETDEWEB)

    Bishop, Christopher B. [Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Herbrych, Jacek W. [Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Dagotto, Elbio R. [Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Moreo, Adriana [Univ. of Tennessee, Knoxville, TN (United States); Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-07-15

    Here, iron telluride (FeTe) is known to display bicollinear magnetic order at low temperatures together with a monoclinic lattice distortion. Because the bicollinear order can involve two different wave vectors (π/2,π/2) and (π/2,–π/2), symmetry considerations allow for the possible stabilization of a nematic state with short-range bicollinear order coupled to monoclinic lattice distortions at a TS higher than the temperature TN where long-range bicollinear order fully develops. As a concrete example, the three-orbital spin-fermion model for iron telluride is studied with an additional coupling ˜λ12 between the monoclinic lattice strain and an orbital-nematic order parameter with B2g symmetry. Monte Carlo simulations show that with increasing ˜λ12 the first-order transition characteristic of FeTe splits and bicollinear nematicity is stabilized in a (narrow) temperature range. In this new regime, the lattice is monoclinically distorted and short-range spin and orbital order breaks rotational invariance. A discussion of possible realizations of this exotic state is provided.

  1. Static deformation of two welded monoclinic elastic half-spaces due ...

    Indian Academy of Sciences (India)

    M. Senthilkumar (Newgen Imaging) 1461 1996 Oct 15 13:05:22

    Static deformation of two monoclinic elastic half-spaces in welded contact due to a long inclined strike-slip fault situated in one of the half-spaces is studied analytically and numerically. Closed- form algebraic expressions for the displacement at any point of the medium are obtained. The variation of the displacement at the ...

  2. Review of zirconium-zircaloy pyrophoricity

    International Nuclear Information System (INIS)

    Cooper, T.D.

    1984-11-01

    Massive zirconium metal scrap can be handled, shipped, and stored with no evidence of combustion or pyrophoricity hazards. Mechanically produced fine scrap such as shavings, turnings, or powders can burn but are not pyrophoric unless the particle diameter is less than 54 μm. Powders with particle diameters less than 54 μm can be both pyrophoric and explosive. Pyrophoric powders should be collected and stored underwater or under inert gas cover to reduce the flammability hazard. Opening sealed containers of zirconium stored underwater should be attempted with caution since hydrogen may be present. The factors that influence the ignition temperature have been explored in depth and recommendations are included for the safe handling, shipping, and storage of pyrophoric or flammable zirconium. 29 refs., 5 figs., 6 tabs

  3. Laser-Based Additive Manufacturing of Zirconium

    Directory of Open Access Journals (Sweden)

    Himanshu Sahasrabudhe

    2018-03-01

    Full Text Available Additive manufacturing of zirconium is attempted using commercial Laser Engineered Net Shaping (LENSTM technique. A LENSTM-based approach towards processing coatings and bulk parts of zirconium, a reactive metal, aims to minimize the inconvenience of traditional metallurgical practices of handling and processing zirconium-based parts that are particularly suited to small volumes and one-of-a-kind parts. This is a single-step manufacturing approach for obtaining near net shape fabrication of components. In the current research, Zr metal powder was processed in the form of coating on Ti6Al4V alloy substrate. Scanning electron microscopy (SEM and energy dispersive spectroscopy (EDS as well as phase analysis via X-ray diffraction (XRD were studied on these coatings. In addition to coatings, bulk parts were also fabricated using LENS™ from Zr metal powders, and measured part accuracy.

  4. Characterization of a Diamond Ground Y-TZP and Reversion of the Tetragonal to Monoclinic Transformation.

    Science.gov (United States)

    Candido, L M; Fais, Lmg; Ferreira, E B; Antonio, S G; Pinelli, Lap

    To characterize the surface of an yttria-stabilized zirconia (Y-TZP) ceramic after diamond grinding in terms of its crystalline phase, morphology, mean roughness (Ra), and wettability as well as to determine a thermal treatment to reverse the resulting tetragonal to monoclinic (t-m) transformation. Y-TZP specimens were distributed into different groups according to the actions (or no action) of grinding and irrigation. Grinding was accomplished using a diamond stone at a low speed. The samples were characterized by x-ray diffraction (XRD), scanning electron microscopy, goniometry, and profilometry. In situ high-temperature XRD was used to determine an annealing temperature to reverse the t-m transformation. Ra was submitted to the Kruskal-Wallis test, followed by the Dunn test (α=0.05). The volume fraction of the monoclinic phase and contact angle were submitted to one-way analysis of variance, followed by the Tukey test (α=0.05). Monoclinic zirconia was observed on the surface of samples after dry and wet grinding with a diamond stone. The volume fraction of the monoclinic phase was smaller on the dry ground samples (3.6%±0.3%) than on the wet ground samples (5.6%±0.3%). High-temperature XRD showed reversion of the t-m phase transformation, which started at 700°C and completed at 800°C in a conventional oven. Grinding with a diamond stone partially transformed the crystalline phase on the surface of a Y-TZP ceramic from tetragonal to monoclinic zirconia while simultaneously increasing the surface roughness and wettability. The t-m transformation could be reversed by heat treatment at 800°C or 900°C for 60 minutes or 1000°C for 30 minutes.

  5. Hydrogen determination in magnesium, zirconium, sodium and lithium using installation, C2532

    International Nuclear Information System (INIS)

    Malikova, E.D.; Velyukhanov, V.P.; Makhinova, L.O.; Kunin, L.L.

    1980-01-01

    Techniques of hydrogen determination in magnesium, lithium, sodium and zirconium using the S 2532 installation are developed. The method of oxidizing melting using lead borate has been used for hydrogen determination in lithium and sodium and the method of vacuum extraction - for hydrogen determination in zirconium and magnesium. Zr and Mg extraction has been carried out in steel reactor at the temperatures of 1000 and 650 deg C, the time of extraction being 30 and 10 minutes respectively. A quartz reactor, temperatures of oxidizing melting of 700-800 deg C, the time of analysis 10 and 20 minutes have been used for sodium and lithium. A possibility to determine volumetric content of hydrogen in magnesium at the existing surface contaminations with hydrogen-containing compounds is shown [ru

  6. Zirconium diselenite microstructures, formation and mechanism

    Science.gov (United States)

    Naik, Chandan C.; Salker, A. V.

    2018-04-01

    In this work, a series of microstructures of zirconium diselenite (Zr(SeO3)2) has been prepared via a simple precipitation method at room temperature without adding any organic surfactants. Phase purity of the sample has been checked by X-ray Diffraction. From the SEM, FESEM, and TEM images spheroid nanoparticles to the starfish-like structure of zirconium diselenite are detected. The morphological evolution processes were investigated carefully following time-dependent experiments and a growth mechanism has been proposed. Two different crystal growth processes, the oriented attachment process accompanying the Ostwald ripening process were held responsible for the formation of a structure resembling starfish having four arms.

  7. Hydrogen outbreak of Zirconium Molybdate Hihydrate

    International Nuclear Information System (INIS)

    Miura, Yasuhiko; Fukuda, Kazuhiro; Ochi, Eiji

    2008-01-01

    JNFL is planning to construct a facility for enclosing the hull and end pieces produced due to reprocessing of spent fuel into stainless canisters after compressing, while those hull and end pieces enclosed into the stainless canisters are called 'compressed hulls'. Since the compressed hulls contain moisture absorbent Zirconium Molybdate Hihydrate accompanying hull and end pieces, there is a risk of outbreak of radiolysisradiolysis gas such as hydrogen, etc. by radiolysisradiolysis. This report intends to state the result of radiation irradiation experiment with the purpose of examining the volume of hydrogen outbreak from Zirconium Molybdate Hihydrate of the compressed hulls. (author)

  8. ICP-AES determination of rare earths in zirconium with prior chemical separation of the matrix

    International Nuclear Information System (INIS)

    Rajeswari, B.; Dhawale, B.A.; Page, A.G.; Sastry, M.D.

    2002-01-01

    Zirconium being one of the most important material in nuclear industry used as a fuel cladding in reactors and an additive in advanced fuels necessitates its characterization for trace metallic contents. Zirconium, as refractory in nature as the rare earth elements, has a complex spectrum comprising of several emission lines. Rare earths, which are high neutron absorbers have to be analysed at very low limits. Hence, to achieve the desired limits, the major matrix has to be separated prior to rare earth determination. The present paper describes the method developed for the separation of rare earths from zirconium by solvent extraction using Trioctyl Phosphine Oxide (TOPO) as the extractant followed by their determination using Inductively Coupled Plasma - Atomic Emission Spectrometric (ICP-AES) method. Initially, radiochemical studies were carried out using known amounts of gamma active tracers of 141 Ce, 152-154 Eu, 153 Gd and 95 Zr for optimisation of extraction conditions using Tl- activated NaI detector. The optimum conditions at 0.5 M TOPO/xylene in 6 M HCl so as to achieve a quantitative recovery of rare earth analytes alongwith a near total extraction of zirconium in the organic phase, was further extended to carry out the studies using ICP-AES method. The recovery of rare earths was found to be quantitative within experimental error with a precision better than 10% RSD. (author)

  9. The separation of plutonium from uranium and fission products on zirconium phosphate columns

    Energy Technology Data Exchange (ETDEWEB)

    Gal, I; Ruvarac, A [Institute of Nuclear Sciences Boris Kidric, Laboratorija za visoku aktivnost, Vinca, Beograd (Serbia and Montenegro)

    1963-12-15

    In recent years special attention has been given to the ion-exchange properties of zirconium phosphate and similar compounds in aqueous solutions. These inorganic cation exchangers are stable in oxidizing media and at elevated temperatures. Their resistance to ionizing radiation makes them particularly suitable for work with radioactive solutions. On account of this we considered ir worthwhile to investigate the separation of plutonium from uranium and fission products on zirconium phosphate columns. We were interested in nitric and solutions containing macro-amounts of uranium (a few grams per litre), and micro-amounts of plutonium and long-lived fission products. To obtain a better insight into the ion-exchange behaviour of the different ionic species towards zirconium phosphate, we first determined the dependence of the distribution coefficients of uranium, plutonium and fission product cations on the aqueous nitric acid concentration. Then, taking the distribution data as a guide, we separated plutonium on small glass columns filled with zirconium phosphate and calculated the decontamination factors (author)

  10. The fluorimetric titration of zirconium in the ppm-range

    International Nuclear Information System (INIS)

    Linden, W.E. von der; Boef, G. den; Ozinga, W.

    1976-01-01

    A fluorimetric titration of zirconium(IV) with EDTA is proposed. The fluorescence intensity of the zirconium-morin complex is used to indicate the end-point. More than twenty other cations were investigated and it was found that they did not interfere, neither did common anions. Mercury(II) can only be tolerated in amount not exceeding that of zirconium. Bismuth(III) interferes and hafnium(IV0 is titrated together with zirconium. The relative standard deviation of the titration of 10ml of a solution containing 1 ppm of zirconium does not exceed 1.5%

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

    Science.gov (United States)

    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).

  12. Contribution to the study of zirconium self-diffusion in zirconium carbide

    International Nuclear Information System (INIS)

    An, Chul

    1972-01-01

    The objective of this research thesis is to determine experimental conditions allowing the measurement of the self-diffusion coefficient of zirconium in zirconium carbide. The author reports the development of a method of preparation of zirconium carbide samples. He reports the use of ion implantation as technique to obtain a radio-tracer coating. The obtained results give evidence of the impossibility to use sintered samples with small grains because of the demonstrated importance of intergranular diffusion. The self-diffusion coefficient is obtained in the case of zirconium carbide with grains having a diameter of few millimetres. The presence of 95 Nb from the disintegration of 95 Zr indicates that these both metallic elements have very close diffusion coefficients at 2.600 C [fr

  13. High purity zirconium obtainment through the iodine compounds transport method

    International Nuclear Information System (INIS)

    Bolcich, J.C.; Zuzek, E.; Dutrus, S.M.; Corso, H.L.

    1987-01-01

    This paper describes the experimental method and the equipment designed, constructed and actually applied for the high purity zirconium obtainment from a zirconium sponge of the nuclear type. The mechanism of purification is based on the impure metal attack with gaseous iodine (at 200 deg C) to obtain zirconium tetra iodine as main product which is then transformed into a pure zirconium base (at 1000-1300 deg C), precipitating the metallic zirconium and releasing the gaseous iodine. From the first experiences carried out, pure zirconium has been obtained from an initial filament of 0.5 mm of diameter as well as wires up to 2.5 mm of diameter. This work presents the results from the studies and analysis made to characterize the material obtained. Finally, the refining methods to which the zirconium produced may be submitted so as to optimize the final purity are discussed. (Author)

  14. Synthesis of zirconium by zirconium tetrachloride reduction by magnesio-thermia. Experimental study and modelling

    International Nuclear Information System (INIS)

    Basin, N.

    2001-01-01

    This work deals with the synthesis of zirconium. The ore is carbo-chlorinated to obtain the tetrachloride which is then purified by selective condensation and extractive distillation. Zirconium tetrachloride is then reduced by magnesium and the pseudo-alloy is obtained according to the global following reaction (Kroll process): ZrCl 4 + 2 Mg = 2 MgCl 2 . By thermodynamics, it has been shown that the volatilization of magnesium chloride and the formation of zirconium sub-chlorides are minimized when the combined effects of temperature and of dilution with argon are limited. With these conditions, the products, essentially zirconium and magnesium chloride, are obtained in equivalence ratio in the magnesio-thermia reaction. The global kinetics of the reduction process has been studied by a thermal gravimetric method. A thermo-balance device has been developed specially for this kinetics study. It runs under a controlled atmosphere and is coupled to a vapor tetrachloride feed unit. The transformation is modelled supposing that the zirconium and magnesium chloride formation result: 1)of the evaporation of magnesium from its liquid phase 2)of the transfer of magnesium and zirconium tetrachloride vapors towards the front of the reaction located in the gaseous phase 3)of the chemical reaction. In the studied conditions, the diffusion is supposed to be the limiting process. The influence of the following parameters: geometry of the reactive zone, temperature, scanning rate of the argon-zirconium tetrachloride mixture, composition of the argon-zirconium tetrachloride mixture has been experimentally studied and confronted with success to the model. (O.M.)

  15. Study on application of zirconium dioxide for upgrading quality of pouring cups used in continuous steel casting technology

    International Nuclear Information System (INIS)

    Pham Ba Kien; Vu Thanh Quang and Ngo Van Tuyen

    2004-01-01

    This theme studies on technology of zirconium oxide powder stabilized by calcium and testing production of steel pouring cup made of the stabilized dioxide zirconium ceramic. As a product of the theme, the steel pouring cup has had the following main characteristics: heat resistance > 1700 o C, density of 4.7 g/cm 3 , apparent sponge degree of 1.63%, compressibility of 3300 kg/cm 2 . The quality of the cup has been tested and highly evaluated during the actual production. (author)

  16. Thermodynamic analysis of thermal plasma process of composite zirconium carbide and silicon carbide production from zircon concentrates

    International Nuclear Information System (INIS)

    Kostic, Z.G.; Stefanovic, P.Lj.; Pavlovic; Pavlovic, Z.N.; Zivkovic, N.V.

    2000-01-01

    Improved zirconium ceramics and composites have been invented in an effort to obtain better resistance to ablation at high temperature. These ceramics are suitable for use as thermal protection materials on the exterior surfaces of spacecraft, and in laboratory and industrial environments that include flows of hot oxidizing gases. Results of thermodynamic consideration of the process for composite zirconium carbide and silicon carbide ultrafine powder production from ZrSiO 4 in argon thermal plasma and propane-butane gas as reactive quenching reagents are presented in the paper. (author)

  17. Experimental studies of relevance on zirconium nitrate raffinate sludge for its disposal as well as zirconium recovery

    International Nuclear Information System (INIS)

    Brahmananda Reddy, G.; Narasimha Murty, B.; Ravindra, H.R.

    2013-01-01

    One of the many routes of production of nuclear grade zirconium dioxide involve separation of zirconium and hafnium by solvent extraction of zirconium nitrate using tri-n-butyl phosphate followed by precipitation of zirconium with ammonia and finally calcination of the so obtained hydrated zirconia at elevated temperature. The zirconium feed solution as is generated from digestion of zirconium washed dried frit (produced by the caustic fusion of zircon sand which is one of the beach sand heavy minerals) in nitric acid contain considerable amount of sludge material and after solvent extraction this whole sludge material rests with raffinate. This sludge material has a scope to contain considerable amounts of zirconium along with other metal ions such as hafnium, aluminium, iron, etc. besides nitric acid and it constitutes one of the important solid wastes that needs to be disposed suitably. One of the disposal means of this sludge material is to use it as a land fill for which two important criteria are to be viz the pH of 10% solid waste solution should be near to neutral pH and the loss on ignition at 550℃ on dry basis of the sludge to be below 20%. In order to study the implications of presence of varying amounts of zirconium nitrate in the sludge on the pH of 10% solution of the sludge various synthetic zirconium nitrate solid waste were prepared using the sludge material generated at the laboratory during the analysis of zirconium washed dried frit. Presence of zirconium in the sludge is expected to decrease the overall pH of the 10% solution of the sludge because zirconium is prone to hydrolyze especially locally when zirconium ion comes into contact with water according to the chemical equation Zr 4+ H 2 O → ZrO 2+ + 2H + . From this equation, it is clear that for every one mole of zirconium ions two moles of hydrogen ions are produced. This is verified experimentally using the synthetically prepared sludge materials with varying amounts of zirconium

  18. On the initial corrosion mechanism of zirconium alloy: Interaction of oxygen and water with Zircaloy at room temperature and 450 C evaluated by x-ray absorption spectroscopy and photoelectron spectroscopy

    International Nuclear Information System (INIS)

    Doebler, U.; Knop, A.

    1994-01-01

    The initial stages of zirconium oxide formation on Zircaloy after water (H 2 O) and oxygen (O 2 ) exposures have been investigated in situ using photoelectron spectroscopy and X-ray-absorption spectroscopy. The reactivity of the zirconium alloy with O 2 at room temperature is about 1,000 times higher than for H 2 O. Up to 100 L (1 L = 1 Langmuir unit = 1 · 10 -6 mbar · s) H 2 O exposure, the reactivity of the zirconium alloy at 450 C is comparable to the room temperature reaction. At higher H 2 O exposure, a sharp increase in the reaction rate for the high-temperature oxidation is observed. From the energy position of the Zr 3d photo emission line and their oxygen-induced chemical shifts, one can really follow the formation of the oxide films. Two different substoichiometric oxides were found during reaction with water. Suboxide (1) is located at the zirconium/zirconium-oxide interface. Subsequently, a Suboxide (2) is concluded from the chemical shift of the zirconium photoelectrons. After an oxide thickness of 2 nm, the stoichiometric ZrO 2 phase is not yet developed

  19. The synthesis, characterization and properties of zirconium-chelating polymers

    International Nuclear Information System (INIS)

    Van Reenen, A.J.

    1985-12-01

    A series of homo- and copolymers based on the monomers : 2-propenoic acid, 2-methyl-2-propenoic acid, 2-chloro-2-propenoic acid, methylene butanedioic acid, ethenyl acetate and ethylene sulphonic acid have been synthesized and characterized. These polyelectrolytes were used with hydrous zirconium oxide to form novel dynamic membranes on Millipore filter substrates. These desalinating membranes were studied in terms of the chemical structure of the polyelectrolytes with regard to the effect of pH on their formation and performance characteristics. The effect of the charge density on the membranes was related to the membranes' figure of merit. Membrane studies were undertaken at pressures of 6 MPa and flow rates of 3,65 litres per minute. 59 figs., 20 tabs., 94 refs

  20. Extraction of zirconium from zircon (A new process)

    International Nuclear Information System (INIS)

    Shahid, K.A.; Saeed, D.; Jan, S.; Masood, A.; Akhtar, J.

    1985-10-01

    A new process has been used for the extraction of zirconium from zircon. Caustic fritting was done in the presence of magnesium hydroxide carbonate and magnesium oxide. These additives decrease the amount of nitric acid soluble silica less than 1000 ppm. Caustic fritting without any additions results in some nitric acid soluble silica, which is removed by dehydration with concentrated sulphuric acid. The present process eliminates the sulphuric acid dissolution and subsequent precipitation with ammonia which involves difficulty in washing of sulphate ions from the geletinous hydroxide cake and hence makes the direct nitric acid dissolution an attractive option. The effect of excess magnesium was studied and extraction does not seem to be effected by excess magnesium. How the reaction proceeds is not exactly understood but a probable mechanism has been postulated. (authors)

  1. Separation of zirconium--hafnium by nitride precipitation

    International Nuclear Information System (INIS)

    Anderson, R.N.; Parlee, N.A.

    1977-01-01

    A method is described for the separation of a light reactive metal (e.g., zirconium) from a heavy reactive metal (e.g., hafnium) by forming insoluble nitrides of the metals in a molten metal solvent (e.g., copper) inert to nitrogen and having a suitable density for the light metal nitride to form a separate phase in the upper portion of the solvent and for the heavy metal nitride to form a separate phase in the lower portion of the solvent. Nitriding is performed by maintaining a nitrogen-containing atmosphere over the bath. The light and heavy metals may be an oxide mixture and carbothermically reduced to metal form in the same bath used for nitriding. The nitrides are then separately removed and decomposed to form the desired separate metals. 16 claims, 1 figure

  2. Thermo-mechanical treatment of zirconium alloys

    International Nuclear Information System (INIS)

    Levy, I.S.

    1975-01-01

    A zirconium alloy comprising at least 95 percent Zr (Zircaloy), which has been thoroughly annealed, is greatly increased in strength without substantial loss in ductility by subjecting it to tensile creep deformation in a temperature range in which creep will occur, yet which is below the temperature for significant recovery. (U.S.)

  3. METHOD AND ALLOY FOR BONDING TO ZIRCONIUM

    Science.gov (United States)

    McCuaig, F.D.; Misch, R.D.

    1960-04-19

    A brazing alloy can be used for bonding zirconium and its alloys to other metals, ceramics, and cermets, and consists of 6 to 9 wt.% Ni, 6 to 9 wn~.% Cr, Mo, or W, 0 to 7.5 wt.% Fe, and the balance Zr.

  4. Structuring of gels of zirconium oxohydrate

    International Nuclear Information System (INIS)

    Sukharev, Yu.I.; Skuratovich, L.P.

    1991-01-01

    Genetic relationship between formation of mesophase states of zirconium oxohydrate gel, coprecipitated with dimethylamine, and ordered macrocrystallites of sorption material after cryogranulation or decryptation granulating is shown. This phenomenon is followed on example of formation of flattened crystallites when preparing granules in the presence of appl. The successive polymerization growth of crystallites leads to the frame ordered aggregation or aggregation of another type

  5. Accelerated irradiation growth of zirconium alloys

    International Nuclear Information System (INIS)

    Griffiths, M.; Gilbert, R.W.; Fidleris, V.

    1989-01-01

    This paper discusses how sponge zirconium and Zr-2.5 wt% Nb, Zircaloy, or Excel alloys all exhibit accelerated irradiation growth compared with high-purity crystal-bar zirconium for irradiation temperatures between 550 to 710 K and fluences between 0.1 to 10 x 10 25 n · m -2 (E > 1 MeV). There is generally an incubation period or fluence before the onset of accelerated or breakaway growth, which is dependent on the particular material being irradiated, its metallurgical condition before irradiation, and the irradiation temperature. Transmission electron microscopy has shown that there is a correlation between accelerated irradiation growth and the appearance of c-component vacancy loops on basal planes. Measurements in some specimens indicate that a significant fraction of the strain can be directly attributed to the loops themselves. There is considerable evidence to show that their formation is dependent both on the specimen purity and on the irradiation temperature. Materials that have a high interstitial-solute content contain c-component loops and exhibit high growth rates even at low fluences ( 2 :5 n · m -2 , E > 1 MeV). For sponge zirconium and the Zircaloys, c-component loop formation and the associated acceleration of growth (breakaway) during irradiation occurs because the intrinsic interstitial solute (mainly, oxygen, carbon and nitrogen) in the zirconium matrix is supplemented by interstitial iron, chromium, and nickel from the radiation-induced dissolution of precipitates. (author)

  6. Zirconium (IV) complexes with some polymethylenediimines | Na ...

    African Journals Online (AJOL)

    The syntheses of zirconium (IV) complexes have been carried out by the reaction of oxozirconium (IV) chloride with the appropriate diimines (Schiff bases). The complexes were isolated as yellow solids which are stable to heat. The complexes were found to be insoluble in most solvents. The infrared spectra, elemental ...

  7. Manufacture of titanium and zirconium hydrides

    International Nuclear Information System (INIS)

    Mares, F.; Hanslik, T.

    1973-01-01

    A method is described of manufacturing titanium and zirconium hydrides by hydrogenation of said metals characterized by the reaction temperature ranging between 250 to 500 degC, hydrogen pressure of 20 to 300 atm and possibly by the presence of a hydride of the respective metal. (V.V.)

  8. Intercalation chemistry of zirconium 4-sulfophenylphosphonate

    International Nuclear Information System (INIS)

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

    2013-01-01

    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. - Graphical abstract: Nitrogen-containing organic compounds can be intercalated into the interlayer space of zirconium 4-sulfophenylphosphonate. - Highlights: • Zirconium 4-sulfophenylphosphonate was examined as a host material in intercalation chemistry. • A wide range of nitrogen-containing organic compounds were intercalated. • Possible arrangement of the intercalated species is described

  9. Studies on inorganic exchanger: zirconium antimonate

    International Nuclear Information System (INIS)

    Dash, A.; Balasubramanian, K.R.

    1992-01-01

    The inorganic exchanger zirconium antimonate has been prepared and its characteristics evaluated. A method has been developed for the separation of 90 Sr and 144 Ce from fission products solution using this exchanger. (author). 23 refs., 18 f igs., 9 tabs

  10. Mechanism for iodine cracking of zirconium claddings

    International Nuclear Information System (INIS)

    Novikov, V.V.

    1991-01-01

    The mechanism of iodine cracking of zirconium cladding is analyzed taking into account the effect of stresses on diffusion. A decisive effect of the stress gradiemt on crack propagation in an agressive medium is shown. The experimental data are compared with the proposed model

  11. Superconductivity in zirconium-rhodium alloys

    Science.gov (United States)

    Zegler, S. T.

    1969-01-01

    Metallographic studies and transition temperature measurements were made with isothermally annealed and water-quenched zirconium-rhodium alloys. The results clarify both the solid-state phase relations at the Zr-rich end of the Zr-Rh alloy system and the influence upon the superconducting transition temperature of structure and composition.

  12. Electrochemical impedance spectroscopic study of passive zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Ai Jiahe; Chen Yingzi [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States); Urquidi-Macdonald, Mirna [Department of Engineering Science and Mechanics, Pennsylvania State University, University Park, PA 16802 (United States); Macdonald, Digby D. [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)], E-mail: ddm2@psu.edu

    2008-09-30

    Spent, unreproccessed nuclear fuel is generally contained within the operational fuel sheathing fabricated from a zirconium alloy (Zircaloy 2, Zircaloy 4, or Zirlo) and is then stored in a swimming pool and/or dry storage facilities until permanent disposal in a licensed repository. During this period, which begins with irradiation of the fuel in the reactor during operation, the fuel sheathing is exposed to various, aggressive environments. The objective of the present study was to characterize the nature of the passive film that forms on pure zirconium in contact with an aqueous phase [0.1 M B(OH){sub 3} + 0.001 M LiOH, pH 6.94] at elevated temperatures (in this case, 250 deg. C), prior to storage, using electrochemical impedance spectroscopy (EIS) with the data being interpreted in terms of the point defect model (PDM). The results show that the corrosion resistance of zirconium in high temperature, de-aerated aqueous solutions is dominated by the outer layer. The extracted model parameter values can be used in deterministic models for predicting the accumulation of general corrosion damage to zirconium under a wide range of conditions that might exist in some repositories.

  13. Obtention of titanium and zirconium metallic

    International Nuclear Information System (INIS)

    Santos, P.R.G.; Rover, C.F.S.; Amaral, F.L.L.

    1988-01-01

    The development works of techniques and equipments for titanium and zirconium sponges obtention are mentioned. The Kroll Process used for the sponges production is described, consisting in the reduction of the metal tetracloride with magnesium in an inert atmosphere of helium or argon. (C.G.C.) [pt

  14. Transmission electron microscopy characterization of Zircaloy-4 and ZIRLO™ oxide layers

    International Nuclear Information System (INIS)

    Gabory, Benoit de; Motta, Arthur T.; Wang, Ke

    2015-01-01

    Waterside corrosion of zirconium alloy nuclear fuel cladding varies markedly from one alloy to another. In addition, for a given alloy, the corrosion rate evolves during the corrosion process, most notably when the oxide loses its stability at the oxide transition. In an effort to understand the mechanism resulting in the variations of corrosion rate observed at the oxide transition, oxide layers formed on Zircaloy-4 and ZIRLO™ in high temperature water autoclave environments, and archived before and after the transition, are characterized using transmission electron microscopy. The study characterizes and compares the oxide morphology in both alloys at different times during the corrosion process, in an effort to understand the oxide growth mechanism for these alloys. Results show that the oxide is mainly composed of monoclinic ZrO 2 , with a preponderance of columnar oxide grains which extend to the oxide/metal interface. The oxide formed right after the transition has occurred, exhibits a 150 nm-wide layer of small equiaxed grains with high tetragonal oxide fraction. This layer has a similar morphology and structure as the first oxide layer formed (observed near the oxide/water interface). A study of the oxygen-rich region near the oxide/metal interface reveals a complex structure of different phases at different stages of corrosion. The interface exhibits an intermediate layer, identified as ZrO, a discontinuous layer of “blocky” Zr 3 O grains embedded in the ZrO layer, and a suboxide layer corresponding to an oxygen saturated solid solution in the metal matrix side. The thickness of this interfacial layer decreased markedly at the transition. Hydrides are also observed in that region, with a definite orientation relationship with the matrix. The observations of the oxide/metal interface are qualitatively similar for the two alloys but quantitatively different. The incorporation of intermetallic precipitates into the oxide layer is also studied, and

  15. Atomic layer deposition of zirconium dioxide from zirconium tetrachloride and ozone

    Energy Technology Data Exchange (ETDEWEB)

    Kukli, Kaupo, E-mail: kaupo.kukli@helsinki.fi [Department of Chemistry, University of Helsinki, P.O. Box 55, FI-00014 Helsinki (Finland); Kemell, Marianna; Köykkä, Joel [Department of Chemistry, University of Helsinki, P.O. Box 55, FI-00014 Helsinki (Finland); Mizohata, Kenichiro [Accelerator Laboratory, Department of Physics, University of Helsinki, P.O. Box 43, FI-00014 Helsinki (Finland); Vehkamäki, Marko; Ritala, Mikko; Leskelä, Markku [Department of Chemistry, University of Helsinki, P.O. Box 55, FI-00014 Helsinki (Finland)

    2015-08-31

    ZrO{sub 2} films were grown by atomic layer deposition using ZrCl{sub 4} and O{sub 3} as precursors. The films were grown on silicon substrates in the temperature range of 220–500 °C. The ALD rate was monotonously decreasing from 0.085 to 0.060 nm/cycle in this temperature range towards the highest temperatures studied. The content of chlorine in the films did not exceed 0.2 at.% as measured by elastic recoil detection analysis. The content of hydrogen was 0.30 and 0.14 at.% in the films grown at 300 and 400 °C, respectively. Structural studies revealed the films consisting of mixtures of stable monoclinic and metastable tetragonal/cubic polymorphs of ZrO{sub 2}, and dominantly metastable phases of ZrO{sub 2} below and above 300 °C, respectively. Permittivity of dielectric layers in Al/Ti/ZrO{sub 2}/(TiN/)Si capacitors with 15–40 nm thick ZrO{sub 2} ranged between 12 and 25 at 100 kHz and the dielectric breakdown fields were in the range of 1.5–3.0 MV/cm. - Highlights: • ZrO{sub 2} thin films were grown by atomic layer deposition from ZrCl{sub 4} and O{sub 3}. • Relatively high substrate temperatures promoted growth of metastable ZrO{sub 2} phases. • ZrO{sub 2} films exhibited electric properties characteristic of dielectric metal oxides. • ZrO{sub 2} grown in hydrogen- and carbon free process contained low amounts of impurities.

  16. Superficial effects during the activation of zirconium AB2 alloys

    International Nuclear Information System (INIS)

    Zerbino, J; Visitin, A; Triaca, W

    2005-01-01

    The activation of zirconium nickel alloys with and without the addition of chromium and titanium is investigated through electrochemical and optical techniques.These alloys show high hydrogen absorption capacity and are extensively used in metal hydride batteries.Recent investigations in aqueous 1 M KOH indicate oxide layer growth and occlusion of hydrogen species in the alloys during the application of different cathodic potential programmes currently used in the activation process.In this research several techniques such as voltammetry, ellipsometry, energy dispersive analysis of X-rays EDAX, and scanning electron microscopy SEM are applied on the polished massive alloy Zr 1 -xTi x , x=0.36 y 0.43, and Zr 1 -xTi x CrNi, x=0.1,0.2 y 0.4.Data analysis shows that the stability, compactness and structure of the passive layers are strongly dependent on the applied potential programme.The alloy activation depends on the formation of deepen crevices that remain after a new polishing. Microscopic observation shows increase in the crevices thickness after the cathodic sweep potential cycling, which produces fragmentation of the grains and oxide growth during the activation process.This indicates metal breaking and intergranular dissolution that take place together with oxide and hydride formation.In some cases the resultant crevice thickness is one or two orders higher than that of the superficial oxide growth indicating intergranular localised corrosion

  17. The degradation of zirconium alloys in nuclear reactors - a review

    International Nuclear Information System (INIS)

    Lim, D.; Graham, N.A.

    1986-01-01

    This report presents the findings of a survey of available non-Canadian literature on the oxidation and hydriding of zirconium alloys. Much of the literature was found to address the Zircaloys, particularly when used as fuel cladding subjected to a radioactive and oxidizing environment. Hydriding of Zircaloys is mainly attributed to oxidation. The survey revealed that Zr-Nb alloys have been included in some investigations; however, data on the long-term degradation of Zr-2.5 wt% Nb, in particular, were scarce. The reviewed literature did not lead to conclusions regarding the potential for accelerated hydriding due to corrosion at crevices and/or second-phase particles, nor did it lead to conclusions as to the potential for a 'breakaway' in oxidation and hydrogen acquisition in long service life of Zr-Nb alloys. Specific information on service experience in U.S.S.R. power reactors could not be obtained; however, most of the information surveyed leads to the conclusion that fuel channels having Zr-2.5 wt% Nb pressure tubes should perform satisfactorily with respect to degradation from corrosion and hydriding provided they are installed correctly and are not operated under conditions that are far removed from those anticipated in design. 91 refs

  18. Anticorrosion ion implantation of fragments of zirconium fuel can specimens

    International Nuclear Information System (INIS)

    Kalin, B.A.; Osipov, V.V.; Volkov, N.V.; Khernov, V.Yu.

    2001-01-01

    Aimed at the study of specific features of oxide film formation in the initial stage of Eh110 and Eh635 alloy fuel can oxidation the modification of tubular specimen surfaces is performed using an ion mixing technique, and the structure of oxide films produced in a steam-water environment is investigated. Using the method of vacuum vapor deposition the outer surface of specimens is coated with alloying element films irradiated by a polyenergetic Ar + ion beam with a 10 keV mean energy up to radiation doses of (7-10) x 10 17 ion/cm 2 . Monatomic (Al, Fe, Cu, Cr, Mo, Sn) or diatomic (Al-Fe, Al-Mo, Al-Sn, Fe-Cu, Fe-Mo, Fe-Sn, Cr-Mo, Cr-Sn) implantation into a zirconium cladding occurs under irradiation effect. The positive influence of combined intrusion of Al and other elements is revealed. The presence of Al atoms enhances the oxide film structure. The least ZeO 2 film thickness is observed when alloying with molybdenum, Al-Fe, Al-Mo and Al-Sn [ru

  19. Autoclave Testing on Zirconium Alloy Materials

    International Nuclear Information System (INIS)

    Hoffmann, Petra-Britt; Sell, Hans-Juergen; Garzarolli, Friedrich

    2012-09-01

    The corrosion of Zirconium components like fuel rod claddings and spacer grids is limiting lifetime and duty of these components. In Pressurized and Boiling Water Reactors (PWR and BWR), different corrosion phenomena are of interest. Although in-pile experience is the final proof for a material development, significant experience was gained by autoclave tests, trying to simulate in-pile conditions but reducing time for return of experience by increased temperatures. For PWR application, the uniform corrosion is studied in water at up to 370 deg. C and in high pressure steam at 400 deg. C, and for BWR, the nodular corrosion is studied in high pressure steam at 500-520 deg. C. Particular attention has to be given to the corrosion media, because oxidative traces in the water can significantly affect the corrosion response. An extensive air removal is thus important for all corrosion tests. This links to the different water chemistry conditions that have been investigated as separate effects otherwise difficult to separate under in-pile conditions. Uniform corrosion in 350 deg. C water is usually a cyclic process with repeated rate transitions. In addition, at high exposure times an acceleration of corrosion can occur, e.g. for Zr-Sn alloys with a high Sn content. In 400 deg. C steam, corrosion rate decreases somewhat with increasing time. Uniform corrosion rate of Zr alloys depends on their Sn- and Fe+Cr contents as well as on their annealing parameters with a similar trend as in PWR and on their yield strength, however with an opposite trend compared to BWR conditions. Nodular corrosion of BWR alloys depends on the annealing parameter with a similar trend as in PWR and out-of-reactor also significantly on the Fe+Cr content. The hydrogen pickup fraction (HPUF) depends largely on details of the water chemistry and can particularly depend on autoclave degassing and probably also on autoclave contaminations. Thus any HPUF value from out-of- pile corrosion tests is only

  20. International strategic minerals inventory summary report; zirconium

    Science.gov (United States)

    Towner, R.R.

    1992-01-01

    Zircon, a zirconium silicate, is currently the most important commercial zirconium-bearing mineral. Baddeleyite, a natural form of zirconia, is less important but has some specific end uses. Both zircon and baddeleyite occur in hard-rock and placer deposits, but at present all zircon production is from placer deposits. Most baddeleyite production is from hard-rock deposits, principally as a byproduct of copper and phosphate-rock mining. World zirconium resources in identified, economically exploitable deposits are about 46 times current production rates. Of these resources, some 71 percent are in South Africa, Australia, and the United States. The principal end uses of zirconium minerals are in ceramic applications and as refractories, abrasives, and mold linings in foundries. A minor amount, mainly of zircon, is used for the production of hafnium-free zirconium metal, which is used principally for sheathing fuel elements in nuclear reactors and in the chemical-processing industry, aerospace engineering, and electronics. Australia and South Africa are the largest zircon producers and account for more than 70 percent of world output; the United States and the Soviet Union account for another 20 percent. South Africa accounts for almost all the world's production of baddeleyite, which is about 2 percent of world production of contained zirconia. Australia and South Africa are the largest exporters of zircon. Unless major new deposits are developed in countries that have not traditionally produced zircon, the pattern of world production is unlikely to change by 2020. The proportions, however, of production that come from existing producing countries may change somewhat.

  1. First-principles study of structural and elastic properties of monoclinic and orthorhombic BiMnO3

    International Nuclear Information System (INIS)

    Mei Zhigang; Shang Shunli; Wang Yi; Liu Zikui

    2010-01-01

    The structural and elastic properties of BiMnO 3 with monoclinic (C 2/c) and orthorhombic (Pnma) ferromagnetic (FM) structures have been studied by first-principles calculations within LDA + U and GGA + U approaches. The equilibrium volumes and bulk moduli of BiMnO 3 phases are evaluated by equation of state (EOS) fittings, and the bulk properties predicted by LDA + U calculations are in better agreement with experiment. The orthorhombic phase is found to be more stable than the monoclinic phase at ambient pressure. A monoclinic to monoclinic phase transition is predicted to occur at a pressure of about 10 GPa, which is ascribed to magnetism versus volume instability of monoclinic BiMnO 3 . The single-crystal elastic stiffness constants c ij s of the monoclinic and orthorhombic phases are investigated using the stress-strain method. The c 46 of the monoclinic phase is predicted to be negative. In addition, the polycrystalline elastic properties including bulk modulus, shear modulus, Young's modulus, bulk modulus-shear modulus ratio, Poisson's ratio, and elastic anisotropy ratio are determined based on the calculated elastic constants. The presently predicted phase transition and elastic properties open new directions for investigation of the phase transitions in BiMnO 3 , and provide helpful guidance for the future elastic constant measurements.

  2. Effects of monoclinic symmetry on the properties of biaxial liquid crystals

    Science.gov (United States)

    Solodkov, Nikita V.; Nagaraj, Mamatha; Jones, J. Cliff

    2018-04-01

    Tilted smectic liquid crystal phases such as the smectic-C phase seen in calamitic liquid crystals are usually treated using the assumption of biaxial orthorhombic symmetry. However, the smectic-C phase has monoclinic symmetry, thereby allowing disassociation of the principal optic and dielectric axes based on symmetry and invariance principles. This is demonstrated here by comparing optical and dielectric measurements for two materials with highly first-order direct transitions from nematic to smectic-C phases. The results show a high difference between the orientations of the principal axes sets, which is interpreted as the existence of two distinct cone angles for optical and dielectric frequencies. Both materials exhibit an increasing degree of monoclinic behavior with decreasing temperature. Due to fast switching speeds, ferroelectric smectic-C* materials are important for fast modulators and LCoS devices, where the dielectric biaxiality influences device operation.

  3. Evidence for photo-induced monoclinic metallic VO2 under high pressure

    International Nuclear Information System (INIS)

    Hsieh, Wen-Pin; Mao, Wendy L.; Trigo, Mariano; Reis, David A.; Andrea Artioli, Gianluca; Malavasi, Lorenzo

    2014-01-01

    We combine ultrafast pump-probe spectroscopy with a diamond-anvil cell to decouple the insulator-metal electronic transition from the lattice symmetry changing structural transition in the archetypal strongly correlated material vanadium dioxide. Coherent phonon spectroscopy enables tracking of the photo-excited phonon vibrational frequencies of the low temperature, monoclinic (M 1 )-insulating phase that transforms into the metallic, tetragonal rutile structured phase at high temperature or via non-thermal photo-excitations. We find that in contrast with ambient pressure experiments where strong photo-excitation promptly induces the electronic transition along with changes in the lattice symmetry, at high pressure, the coherent phonons of the monoclinic (M 1 ) phase are still clearly observed upon the photo-driven phase transition to a metallic state. These results demonstrate the possibility of synthesizing and studying transient phases under extreme conditions

  4. SIMS study of oxygen diffusion in monoclinic HfO2

    Science.gov (United States)

    Mueller, Michael P.; De Souza, Roger A.

    2018-01-01

    The diffusion of oxygen in dense ceramics of monoclinic HfO2 was studied by means of (18O/16O) isotope exchange annealing and subsequent determination of isotope depth profiles by Secondary Ion Mass Spectrometry. Anneals were performed in the temperature range of 573 ≤T /K ≤ 973 at an oxygen partial pressure of p O2=200 mbar . All measured isotope profiles exhibited two features: the first feature, closer to the surface, was attributed mainly to slow oxygen diffusion in an impurity silicate phase; the second feature, deeper in the sample, was attributed to oxygen diffusion in bulk monoclinic HfO2 . The activation enthalpy of oxygen tracer diffusion in bulk HfO2 was found to be ΔHD∗≈0.5 eV .

  5. Evidence for photo-induced monoclinic metallic VO{sub 2} under high pressure

    Energy Technology Data Exchange (ETDEWEB)

    Hsieh, Wen-Pin, E-mail: wphsieh@stanford.edu; Mao, Wendy L. [Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Department of Geological and Environmental Sciences, Stanford University, Stanford, California 94305 (United States); Trigo, Mariano [Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Stanford PULSE Institute, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Reis, David A. [Stanford Institute for Materials and Energy Sciences, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Stanford PULSE Institute, SLAC National Accelerator Laboratory, Menlo Park, California 94025 (United States); Department of Photon Science and Applied Physics, Stanford University, Stanford, California 94305 (United States); Andrea Artioli, Gianluca; Malavasi, Lorenzo [Dipartimento di Chimica, Sezione di Chimica Fisica, INSTM (UdR Pavia), Università di Pavia, Viale Taramelli 16, 27100 Pavia (Italy)

    2014-01-13

    We combine ultrafast pump-probe spectroscopy with a diamond-anvil cell to decouple the insulator-metal electronic transition from the lattice symmetry changing structural transition in the archetypal strongly correlated material vanadium dioxide. Coherent phonon spectroscopy enables tracking of the photo-excited phonon vibrational frequencies of the low temperature, monoclinic (M{sub 1})-insulating phase that transforms into the metallic, tetragonal rutile structured phase at high temperature or via non-thermal photo-excitations. We find that in contrast with ambient pressure experiments where strong photo-excitation promptly induces the electronic transition along with changes in the lattice symmetry, at high pressure, the coherent phonons of the monoclinic (M{sub 1}) phase are still clearly observed upon the photo-driven phase transition to a metallic state. These results demonstrate the possibility of synthesizing and studying transient phases under extreme conditions.

  6. Calculation of magnetization curves and probability distribution for monoclinic and uniaxial systems

    International Nuclear Information System (INIS)

    Sobh, Hala A.; Aly, Samy H.; Yehia, Sherif

    2013-01-01

    We present the application of a simple classical statistical mechanics-based model to selected monoclinic and hexagonal model systems. In this model, we treat the magnetization as a classical vector whose angular orientation is dictated by the laws of equilibrium classical statistical mechanics. We calculate for these anisotropic systems, the magnetization curves, energy landscapes and probability distribution for different sets of relevant parameters and magnetic fields of different strengths and directions. Our results demonstrate a correlation between the most probable orientation of the magnetization vector, the system's parameters, and the external magnetic field. -- Highlights: ► We calculate magnetization curves and probability angular distribution of the magnetization. ► The magnetization curves are consistent with probability results for the studied systems. ► Monoclinic and hexagonal systems behave differently due to their different anisotropies

  7. Identification of monoclinic calcium pyrophosphate dihydrate and hydroxyapatite in human sclera using Raman microspectroscopy.

    Science.gov (United States)

    Chen, Ko-Hua; Li, Mei-Jane; Cheng, Wen-Ting; Balic-Zunic, Tonci; Lin, Shan-Yang

    2009-02-01

    Raman microspectroscopy was first used to determine the composition of a calcified plaque located at the pterygium-excision site of a 51-year-old female patient's left nasal sclera after surgery. It was unexpectedly found that the Raman spectrum of the calcified sample at 1149, 1108, 1049, 756, 517, 376 and 352/cm was similar to the Raman spectrum of monoclinic form of calcium pyrophosphate dihydrate (CPPD) crystal, but differed from the Raman spectrum of triclinic form of CPPD. An additional peak at 958/cm was also observed in the Raman spectrum of the calcified plaque, which was identical to the characteristic peak at 958/cm of hydroxyapatite (HA). This is the first study to report the spectral biodiagnosis of both monoclinic CPPD and HA co-deposited in the calcified plaque of a patient with sclera dystrophic calcification using Raman microspectroscopy.

  8. Determination of zirconium by fluoride ion selective electrode

    International Nuclear Information System (INIS)

    Mahanty, B.N.; Sonar, V.R.; Gaikwad, R.; Raul, S.; Das, D.K.; Prakash, A.; Afzal, Md.; Panakkal, J.P.

    2010-01-01

    Full text: Zirconium is used in a wide range of applications including nuclear clad, catalytic converters, surgical appliances, metallurgical furnaces, superconductors, ceramics, lamp filaments, anti corrosive alloys and photographical purposes. Irradiation testing of U-Zr and U-Pu-Zr fuel pins has also demonstrated their feasibility as fuel in liquid metal reactors. Different methods that are employed for the determination of zirconium are spectrophotometry, potentiometry, neutron activation analysis and mass spectrometry. Ion-selective electrode (ISE), selective to zirconium ion has been studied for the direct potentiometric measurements of zirconium ions in various samples. In the present work, an indirect method has been employed for the determination of zirconium in zirconium nitrate sample using fluoride ion selective electrode. This method is based on the addition of known excess amount of fluoride ion to react with the zirconium ion to produce zirconium tetra fluoride at about pH 2-3, followed by determination of residual fluoride ion selective electrode. The residual fluoride ion concentrations were determined from the electrode potential data using calibration plot. Subsequently, zirconium ion concentrations were determined from the concentration of consumed fluoride ions. A precision of about 2% (RSD) with the mean recovery of more than 94% has been achieved for the determination of zirconium at the concentration of 4.40 X 10 -3 moles lit -1

  9. Process for surface treatment of zirconium-containing cladding materials for fuel element or other components for nuclear reactors

    International Nuclear Information System (INIS)

    Videm, K.G.; Lunde, L.R.; Kooyman, H.H.

    1975-01-01

    A process for the surface treatment of zirconium-base cladding materials for fuel elements or other components for nuclear reactors is described. The treatment includes pickling the cladding material in a fluoride-containing bath, and then applying a protective coating through oxidation to the pickled cladding material. The fluoride-containing contaminants which remain on the surface of the cladding material during pickling are removed or rendered harmless by anodic oxidation

  10. Nucleation in stress-induced tetragonal-monoclinic transformation of constrained zirconia

    International Nuclear Information System (INIS)

    Chan, S.K.

    1992-08-01

    A theory for stress-induced tetragonal→monoclinic transformation of constrained zirconia is presented based on the assumption that when forcibly strained to a regime of absolute instability where the free energy density of the tetragonal phase has a negative curvature, the constrained tetragonal zirconia becomes unstable with respect to the development of a modulated strain pattern that will evolve into a band of twin monoclinic domains. The temperature range for such an instability, the critical size of the inclusion, the corresponding critical strain, and the periodicity of the modulation are derived in terms of parameters that can be related to the elastic stiffness coefficients of various orders of the inclusion and the shear modulus of the host matrix. An entirely different mechanism is suggested for the reverse monoclinic→tetragonal transformation because the monoclinic phase is metastable when the extrinsic stress is removed. Estimates for the parameters are inferred from a variety of experimental data for pure zirconia and the numerical values for the predicted physical quantities are obtained

  11. Critical Role of Monoclinic Polarization Rotation in High-Performance Perovskite Piezoelectric Materials.

    Science.gov (United States)

    Liu, Hui; Chen, Jun; Fan, Longlong; Ren, Yang; Pan, Zhao; Lalitha, K V; Rödel, Jürgen; Xing, Xianran

    2017-07-07

    High-performance piezoelectric materials constantly attract interest for both technological applications and fundamental research. The understanding of the origin of the high-performance piezoelectric property remains a challenge mainly due to the lack of direct experimental evidence. We perform in situ high-energy x-ray diffraction combined with 2D geometry scattering technology to reveal the underlying mechanism for the perovskite-type lead-based high-performance piezoelectric materials. The direct structural evidence reveals that the electric-field-driven continuous polarization rotation within the monoclinic plane plays a critical role to achieve the giant piezoelectric response. An intrinsic relationship between the crystal structure and piezoelectric performance in perovskite ferroelectrics has been established: A strong tendency of electric-field-driven polarization rotation generates peak piezoelectric performance and vice versa. Furthermore, the monoclinic M_{A} structure is the key feature to superior piezoelectric properties as compared to other structures such as monoclinic M_{B}, rhombohedral, and tetragonal. A high piezoelectric response originates from intrinsic lattice strain, but little from extrinsic domain switching. The present results will facilitate designing high-performance perovskite piezoelectric materials by enhancing the intrinsic lattice contribution with easy and continuous polarization rotation.

  12. Molten salt extractive distillation process for zirconium-hafnium separation

    International Nuclear Information System (INIS)

    McLaughlin, D.F.; Stoltz, R.A.

    1989-01-01

    This patent describes an improvement in a process for zirconium-hafnium separation. It utilizes an extractive distillation column with a mixture of zirconium and hafnium tetrachlorides introduced into a distillation column having a top and bottom with hafnium enriched overheads taken from the top of the column and a molten salt solvent circulated through the column to provide a liquid phase, and with molten salt solvent containing zirconium chloride being taken from the bottom of the distillation column. The improvements comprising: utilizing a molten salt solvent consisting principally of lithium chloride and at least one of sodium, potassium, magnesium and calcium chlorides; stripping of the zirconium chloride taken from the bottom of the distillation column by electrochemically reducing zirconium from the molten salt solvent; and utilizing a pressurized reflux condenser on the top of the column to add the hafnium chloride enriched overheads to the molten salt solvent previously stripped of zirconium chloride

  13. Advances in zirconium technology for nuclear reactor application

    International Nuclear Information System (INIS)

    Ganguly, C.

    2002-01-01

    Zirconium alloys are extensively used as a material for cladding nuclear fuels and for making core structurals of water-cooled nuclear power reactors all over the world for generation of nearly 16 percent of the worlds electricity. Only four countries in the world, namely France, USA, Russia and India, have large zirconium industry and capability to manufacture reactor grade zirconium sponge, a number of zirconium alloys and a wide variety of structural components for water cooled nuclear reactor. The present paper summarises the status of zirconium technology and highlights the achievement of Nuclear Fuel Complex during the last ten years in developing a wide variety of zirconium alloys and components for water-cooled nuclear power programme

  14. Alumina-zirconium ceramics synthesis by selective laser sintering/melting

    International Nuclear Information System (INIS)

    Shishkovsky, I.; Yadroitsev, I.; Bertrand, Ph.; Smurov, I.

    2007-01-01

    In the present paper, porous refractory ceramics synthesized by selective laser sintering/melting from a mixture of zirconium dioxide, aluminum and/or alumina powders are subjected to optical metallography and X-ray analysis to study their microstructure and phase composition depending on the laser processing parameters. It is shown that high-speed laser sintering in air yields ceramics with dense structure and a uniform distribution of the stabilizing phases. The obtained ceramic-matrix composites may be used as thermal and electrical insulators and wear resistant coating in solid oxide fuel cells, crucibles, heating elements, medical tools. The possibility to reinforce refractory ceramics by laser synthesis is shown on the example of tetragonal dioxide of zirconium with hardened micro-inclusion of Al 2 O 3 . By applying finely dispersed Y 2 O 3 powder inclusions, the type of the ceramic structure is significantly changed

  15. Immobilization of transition metal ions on zirconium phosphate monolayers

    International Nuclear Information System (INIS)

    Melezhik, A.V.; Brej, V.V.

    1998-01-01

    It is shown that ions of transition metals (copper, iron, vanadyl, titanium) are adsorbed on zirconium phosphate monolayers. The zirconium phosphate threshold capacity corresponds to substitution of all protons of hydroxyphosphate groups by equivalent amounts of copper, iron or vanadyl. Adsorption of polynuclear ions is possible in case of titanium. The layered substance with specific surface up to 300 m 2 /g, wherein ultradispersed titanium dioxide particles are intercalirated between zirconium-phosphate layers, is synthesized

  16. Titanium zirconium and hafnium coordination compounds with vanillin thiosemicarbazone

    International Nuclear Information System (INIS)

    Konunova, Ts.B.; Kudritskaya, S.A.

    1987-01-01

    Coordination compounds of titanium zirconium and hafnium tetrachlorides with vanillin thiosemicarbazone of MCl 4 x nLig composition, where n=1.5, 4 for titanium and 1, 2, 4 for zirconium and hafnium, are synthesized. Molar conductivity of ethanol solutions is measured; IR spectroscopic and thermochemical investigation are carried out. The supposition about ligand coordination via sulfur and azomethine nitrogen atoms is made. In all cases hafnium forms stable compounds than zirconium

  17. Manufacturing process to reduce large grain growth in zirconium alloys

    International Nuclear Information System (INIS)

    Rosecrans, P.M.

    1987-01-01

    A method is described of treating cold worked zirconium alloys to reduce large grain growth during thermal treatment above its recrystallization temperature. The method comprises heating the zirconium alloy at a temperature of about 1300 0 F. to 1350 0 F. for about 1 to 3 hours subsequent to cold working the zirconium alloy and prior to the thermal treatment at a temperature of between 1450 0 -1550 0 F., the thermal treatment temperature being above the recrystallization temperature

  18. Preparation of zirconium molybdate gel generator

    International Nuclear Information System (INIS)

    Charoen, S.; Aungurarat, G.; Laohawilai, S.; Sukontpradit, W.; Jingjit, S.

    1994-01-01

    A procedure for preparation of 99mTc generator based on conversion to zirconium molybdate gel of 99Mo produced by neutron activation was reported. The gel was prepared from zirconium oxychloride solution pH 1.6, ammonium molybdate solution pH 3-5 and mole ratio of Zr:Mo 1:1 which had water content about 7-8%. Small generators containing 1-1.5 g of gel were eluted with average efficiencies of 77% and the activity peak in the first 3 ml of 10 ml of saline solution. The amount of Mo and Zr in eluates were below the acceptance limit. The gel generators of activity about 100 mCi were prepared and had the good performance in elutability and stability

  19. Study of some properties of zirconium phosphate

    International Nuclear Information System (INIS)

    Prospert, J.

    1963-05-01

    Zirconium phosphate has been studied with a view to using it as an ion exchanger: the first objective was to develop a method of preparation easy to apply and also reproducible. To this end, several tests were carried out varying the molar ratios of phosphorus and of zirconium. Some physical properties such as the diffraction of X-rays were examined. The work then involved certain chemical properties, particularly the percentages of free water and structural water given by the loss on calcination, the Karl-Fisher method and the weight losses by thermogravimetry. Finally an attempts was made to apply the exchanger to the separation of alkaline ions. The static tests showed that the order of fixation of these ions was Cs + > Rb + >> K + > Na + . Tests with columns showed that Na + and K + were easily separable, as was the Rb + -Cs + mixture, this last pair being fairly difficult to dissociate. (author) [fr

  20. Separation process of zirconium and hafnium

    International Nuclear Information System (INIS)

    Hure, J.; Saint-James, R.

    1955-01-01

    About the separation different processes of zirconium-hafnium, the extraction by solvent in cross-current is the most easily the process usable on an industrial scale. It uses tributyl phosphate as solvent, diluted with white spirit to facilitate the decanting. Some exploratory tests showed that nitric environment seemed the most favorable for extraction; but a lot of other factors intervene in the separation process. We studied the influence of the acidity successively, the NO 3 - ions concentration, the role of the cation coming with NO 3 - , as well as the influence of the concentration of zirconium in the solution on the separation coefficient β = α Zr / α Hf . (M.B.) [fr