WorldWideScience

Sample records for zirconium carbonitride films

  1. Synthesis of zirconium guanidinate complexes and the formation of zirconium carbonitride via low pressure CVD

    NARCIS (Netherlands)

    Potts, S.E.; Carmalt, C.J.; Blackman, C.S.; Abou-Chabine, F.; Pugh, D.; Davies, H.O.

    2009-01-01

    Thin films of zirconium carbonitride have been deposited on glass at 600 °C from two novel guanidinate precursors: [ZrCp'{¿2-(iPrN)2CNMe2}2Cl] (1) and [ZrCp'2{¿2-(iPrN)2CNMe2}Cl] (2) (Cp' ) monomethylcyclopentadienyl). Both compounds 1 and 2 were structurally characterized by X-ray crystallography.

  2. 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

  3. The structure study of boron carbonitride films obtained by use of trimethylamine borane complex

    CERN Document Server

    Kosinova, M L; Fainer, N I; Maximovski, E A; Kuznetsov, F A

    2001-01-01

    Diffraction of synchrotron radiation (SR) was used to investigate crystalline structure and phase composition of thin films (1500-5000 A) of boron carbonitride. These films were synthesized by plasma-enhanced chemical vapor deposition using nontraditional volatile single source precursor trimethylamine borane complex (CH sub 3) sub 3 N centre dot BH sub 3 and its mixture with ammonia. The effect of the gas ratio and substrate temperature on chemical and phase composition as well as the structure of the films were investigated. The XRD peculiarities of texture films and ways of increasing sensibility of measurements were considered. A possibility of the information density rise of the thin film XRD was shown due to application of different methods for recording diffraction patterns.

  4. Composition and optical properties tunability of hydrogenated silicon carbonitride thin films deposited by reactive magnetron sputtering

    Science.gov (United States)

    Bachar, A.; Bousquet, A.; Mehdi, H.; Monier, G.; Robert-Goumet, C.; Thomas, L.; Belmahi, M.; Goullet, A.; Sauvage, T.; Tomasella, E.

    2018-06-01

    Radiofrequency reactive magnetron sputtering was used to deposit hydrogenated amorphous silicon carbonitride (a-SiCxNy:H) at 400 °C by sputtering a silicon target under CH4 and N2 reactive gas mixture. Rutherford backscattering spectrometry revealed that the change of reactive gases flow rate (the ratio R = FN2/(FN2+FCH4)) induced a smooth chemical composition tunability from a silicon carbide-like film for R = 0 to a silicon nitride-like one at R = 1 with a large area of silicon carbonitrides between the two regions. The deconvolution of Fourier Transform InfraRed and X-ray photoelectron spectroscopy spectrum highlighted a shift of the chemical environment of the deposited films corresponding to the changes seen by RBS. The consequence of these observations is that a control of refractive index in the range of [1.9-2.5] at λ = 633 nm and optical bandgap in the range [2 eV-3.8 eV] have been obtained which induces that these coatings can be used as antireflective coatings in silicon photovoltaic cells.

  5. Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite

    Directory of Open Access Journals (Sweden)

    Thampi VV

    2015-10-01

    Full Text Available VV Anusha Thampi,1 P Dhandapani,2 Geetha Manivasagam, B Subramanian11Electrochemical Materials Science Division, Central Electrochemical Research Institute, Karaikudi, 2Corrosion and Materials Protection Division, Central Electrochemical Reserach Institute, Karaikudi, 3Centre for Bio-Materials Science and Technology, VIT University, Vellore, IndiaAbstract: Thin films of titanium carbonitride (TiCN were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating.Keywords: titanium carbonitride thin films, magnetron sputtering, ureolytic bacteria, biocompatibility

  6. Enhancement of bioactivity of titanium carbonitride nanocomposite thin films on steels with biosynthesized hydroxyapatite.

    Science.gov (United States)

    Thampi, V V Anusha; Dhandapani, P; Manivasagam, Geetha; Subramanian, B

    2015-01-01

    Thin films of titanium carbonitride (TiCN) were fabricated by DC magnetron sputtering on medical grade steel. The biocompatibility of the coating was further enhanced by growing hydroxyapatite crystals over the TiCN-coated substrates using biologically activated ammonia from synthetic urine. The coatings were characterized using X-ray diffraction, X-ray photoelectron spectroscopy, scanning electron microscopy (SEM)-energy dispersive spectroscopy, and Raman spectroscopy. The electrochemical behavior of the coatings was determined in simulated body fluid. In addition, hemocompatibility was assessed by monitoring the attachment of platelets on the coating using SEM. The wettability of the coatings was measured in order to correlate with biocompatibility results. Formation of a coating with granular morphology and the preferred orientation was confirmed by SEM and X-ray diffraction results. The hydroxyapatite coating led to a decrease in thrombogenicity, resulting in controlled blood clot formation, hence demonstrating the hemocompatibility of the coating.

  7. 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)

  8. 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.

  9. 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

  10. 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

  11. 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

  12. 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

  13. Plastic flow and preferred orientation in molybdenum and zirconium films

    International Nuclear Information System (INIS)

    Window, B.

    1989-01-01

    X-ray diffraction measurements on samples of molybdenum and zirconium growth with ion assistance at low temperatures support the occurrence of plastic flow during growth, provided the level of bombardment is high enough. As the energy of the argon ions was increased, the lattice strain in the growth direction increased to a maximum before decreasing slowly. That this is a plastic flow transition is shown by the independence of the maximum strain on preparation conditions and by the changes in microstructure. In particular, the grain size in the growth direction decreased and the preferred orientation favored the usual wire drawing textures of these metals. For the zirconium films this involved a change in preferred orientation from a (00.2) to a (10.0) texture. A reduction in strain is observed at high bombardment levels

  14. 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.

  15. 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.

  16. Effect of ageing in the electrolyte and water on porous anodic films on zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Muratore, F.; Hashimoto, T.; Skeldon, P., E-mail: peter.skeldon@manchester.ac.uk; Thompson, G.E.

    2011-06-15

    Highlights: Porous anodic films are formed on zirconium consisting of nanotubes embedded in a fluoride-rich matrix. {yields}Ageing in the formation electrolyte transforms the films from porous to nanotubular. Ageing causes losses of zirconium and fluorine, due to dissolution of the matrix. Ageing in water has negligible influence on the film composition and the film morphology. - Abstract: The present study demonstrates the significant influence of ageing in the formation electrolyte on the morphology and composition of anodic films grown on zirconium in 0.35 M ammonium fluoride in glycerol. Ageing after anodizing, by immersion in the electrolyte for 1 h, is shown to promote a transition from a porous to a nanotubular morphology, due to the dissolution of the fluoride-rich intratubular material in which the nanotubes are embedded. The morphological change is accompanied by a significant loss of zirconium and fluorine from the film. In contrast, ageing in deionized water has little influence on the films.

  17. Properties of zirconium ceramics and film stabilized by yttrium

    International Nuclear Information System (INIS)

    Korobova, N.

    2004-01-01

    Full text: Unstable zirconium dioxide phase transformation can be eliminated by stabilization of the cubic phase with an addition of a selected alkaline earth or rare-earth oxide. Stabilized ZrO 2 has been widely utilized in various high-temperature refractory applications. These stabilized ZrO 2 -base solid solutions also possess rather unique electrical properties, and as a result have considerable potential as solid electrolytes in galvanic and fuel cells and, possibly, as heating elements in high-temperature furnaces. The complex study of synthesis processes, structure and properties of metal alkoxide organic sols have been developed. These have allowed to create main principles of their formation and to show the practical realization of obtained theoretical and experimental results. The correlation between hydrolysis conditions of (Zr+Y) metal alkoxide sols and synthesis of stable colloid multi-component systems has been established. Systematic research of zirconium and yttrium bi-alkoxide electrophoretic deposition was conducted for the first time. The formation mechanism of electrophoretic deposits has been offered and general scientific principles of the electrophoretic process have been formulated. The model of gel deposits structure was proposed. It has enabled to analyze the main (for example, cluster) effects, which have been exhibited in technological procedure for thin film preparation. The structure investigation of stabilized zirconium dioxide thin films and ceramics has been studied. The researches were based on the comparative analysis of the initial gel microstructure and dried gel by the various drying methods. The new approach for drying of gel electrophoretic deposits was formulated theoretically and experimentally has been proved. The modeling of the aggregate kinetics as a type of 'cluster-cluster' has been proposed like a qualitative description of the process. The data of fractal dimensions of aggregates which have been formed at the

  18. 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

  19. 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.

  20. 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

  1. Niobium and zirconium telluride thin films prepared by sputtering

    International Nuclear Information System (INIS)

    Kassem, M.; Pailharey, D.; Mathey, Y.

    2000-01-01

    A versatile procedure of sputter deposition, well adapted for getting a large of Te/M ratios (with M = Zr or Nb), has led to the synthesis of several highly anisotropic zirconium and niobium poly tellurides in thin film form. Upon tuning the two key parameters of the process, i.e., the Te percentage in the target and the substrate temperature during the deposition, preparation of systems ranging from ZrTe 0 .72 to ZrTe 6 .7, on the one hand, and from NbTe 1 .28 to NbTe 7 .84, on the other, has been achieved. Besides their amorphous or crystalline (with or without preferential orientations) behavior and their relationship to known structural types, the most striking feature of these films is their large departure from the stoichiometry of the bulk Mte x reference compounds. This peculiarity, together with the possible changes of composition under annealing, are described and interpreted in terms of variable of Te and M atoms trapped or intercalated within the parent structures. (author)

  2. Optical and electrical characteristics of plasma enhanced chemical vapor deposition boron carbonitride thin films derived from N-trimethylborazine precursor

    Energy Technology Data Exchange (ETDEWEB)

    Sulyaeva, Veronica S., E-mail: veronica@niic.nsc.ru [Department of Functional Materials Chemistry, Nikolaev Institute of Inorganic Chemistry SB RAS, Novosibirsk 630090 (Russian Federation); Kosinova, Marina L.; Rumyantsev, Yurii M.; Kuznetsov, Fedor A. [Department of Functional Materials Chemistry, Nikolaev Institute of Inorganic Chemistry SB RAS, Novosibirsk 630090 (Russian Federation); Kesler, Valerii G. [Laboratory of Physical Principles for Integrated Microelectronics, Rzhanov Institute of Semiconductor Physics SB RAS, Novosibirsk 630090 (Russian Federation); Kirienko, Viktor V. [Laboratory of Nonequilibrium Semiconductors Systems, Rzhanov Institute of Semiconductor Physics SB RAS, Novosibirsk 630090 (Russian Federation)

    2014-05-02

    Thin BC{sub x}N{sub y} films have been obtained by plasma enhanced chemical vapor deposition using N-trimethylborazine as a precursor. The films were deposited on Si(100) and fused silica substrates. The grown films were characterized by ellipsometry, Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray energy dispersive spectroscopy, X-ray photoelectron spectroscopy, spectrophotometry, capacitance–voltage and current–voltage measurements. The deposition parameters, such as substrate temperature (373–973 K) and gas phase composition were varied. Low temperature BC{sub x}N{sub y} films were found to be high optical transparent layers in the range of 300–2000 nm, the transmittance as high as 93% has been achieved. BC{sub x}N{sub y} layers are dielectrics with dielectric constant k = 2.2–8.9 depending on the synthesis conditions. - Highlights: • Thin BC{sub x}N{sub y} films have been obtained by plasma enhanced chemical vapor deposition. • N-trimethylborazine was used as a precursor. • Low temperature BC{sub x}N{sub y} films were found to be high optical transparent layers (93%). • BC{sub x}N{sub y} layers are dielectrics with dielectric constant k = 2.2–8.9.

  3. Optical and electrical characteristics of plasma enhanced chemical vapor deposition boron carbonitride thin films derived from N-trimethylborazine precursor

    International Nuclear Information System (INIS)

    Sulyaeva, Veronica S.; Kosinova, Marina L.; Rumyantsev, Yurii M.; Kuznetsov, Fedor A.; Kesler, Valerii G.; Kirienko, Viktor V.

    2014-01-01

    Thin BC x N y films have been obtained by plasma enhanced chemical vapor deposition using N-trimethylborazine as a precursor. The films were deposited on Si(100) and fused silica substrates. The grown films were characterized by ellipsometry, Fourier transform infrared spectroscopy, scanning electron microscopy, X-ray energy dispersive spectroscopy, X-ray photoelectron spectroscopy, spectrophotometry, capacitance–voltage and current–voltage measurements. The deposition parameters, such as substrate temperature (373–973 K) and gas phase composition were varied. Low temperature BC x N y films were found to be high optical transparent layers in the range of 300–2000 nm, the transmittance as high as 93% has been achieved. BC x N y layers are dielectrics with dielectric constant k = 2.2–8.9 depending on the synthesis conditions. - Highlights: • Thin BC x N y films have been obtained by plasma enhanced chemical vapor deposition. • N-trimethylborazine was used as a precursor. • Low temperature BC x N y films were found to be high optical transparent layers (93%). • BC x N y layers are dielectrics with dielectric constant k = 2.2–8.9

  4. Improvement of the Surface Hardness of Stainless Steel with the TitaniumCarbonitride Ti(CN) Thin Films

    International Nuclear Information System (INIS)

    Agus-Purwadi; Tri-Mardji Atmono; Widdi-Usada; Lely-Susita; Yunanto

    2000-01-01

    Fabrication of the T i (CN) thin films with methods of implantation and RFsputtering for improving the surfaces hardness of stainless steel (SS) hasbeen done. Some kinds of T i C thin films which made individually by varyingof RF sputtering power from 0 up to 160 watt are implanted by the nitrogenion beams on the doses and energy ion optimum of 6.107 x 10 17 ion/cm 2 and100 keV, also fabrication of T i (CN) thin films use RF sputtering method withT i target and reaction gases as argon, silene and nitrogen on the optimum ofsputtering parameter condition. The thin films yields are characterized byusing Microhardness Tester MX 170, obtained SS hardness which layered T i (CN)as 402.5 KHN from its initial of 215.54 KHN and 371.74 KHN (layered T i C), itmeans that the SS surface hardness improve 1.867 times cumulatively. From theX-Ray Diffraction (XRD) analysis yield showed that the microstructure ofT i (CN) films on the SS substrates are dominated by characteristic cubiccrystal structure with Miller plane orientation (111) on the scattering angleof 2 θ = 44 o . Morphology visualization of T i (CN) thin films crosssection on the SS substrate is realized by Spectroscopy Electron Microscope(SEM). (author)

  5. 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.

  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. 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

  8. 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.)

  9. 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.)

  10. 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)

  11. 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.

  12. 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

  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. Method of producing thermally stable uranium carbonitrides

    International Nuclear Information System (INIS)

    Ugajin, M.; Takahashi, I.

    1975-01-01

    A thermally stable uranium carbonitride can be produced by adding tungsten and/or molybdenum in the amount of 0.2 wt percent or more, preferably 0.5 wt percent or more, to a pure uranium carbonitride. (U.S.)

  15. Tests for depositing thin films of metallic zirconium; Essais de depot de zirconium metallique en couches minces

    Energy Technology Data Exchange (ETDEWEB)

    Bentolila, J.; Pattoret, A.; Platzer, R.

    1957-01-15

    The authors report a study which aimed at obtaining a thin, adhesive and non porous coating of metallic zirconium on a uranium substrate by means of chemical process. The main required condition was not to go beyond the uranium phase change temperature (650 C). Two kinds of tests have been performed: on the one hand, tests of reduction of zirconium tetrachloride in non aqueous solvent medium, and on the other hand, tests of vacuum decomposition of zirconium hydride. As far as the first tests are concerned, the authors studied organic solvent media (reduction by aluminium and lithium hydride, action of organic-magnesium compounds), and liquid ammoniac. For the second test type, they describe the apparatus, the preparation of the zirconium hydride, preparation of the substrate surfaces, coating preparation, and decomposition process. Results are discussed in terms of temperature, of presence of copper powder in the coating, of early surface hydriding of uranium, surface polishing.

  16. Ion scattering spectroscopy studies of zirconium dioxide thin films prepared in situ

    International Nuclear Information System (INIS)

    Martin, P.J.; Netterfield, R.P.

    1987-01-01

    Low energy Ion Scattering Spectroscopy has been used to investigate, in situ, thin films of zirconium dioxide deposited by evaporation and ion-assisted deposition. It is shown that when a film is deposited to an average thickness of 0.3 nm +- 0.03, as measured by in situ ellipsometry, complete coverage of the substrate occurs. 'Ion-assisted films have detectably higher Zr surface concentrations and reduced low-energy sputter peaks. Inelastic tailing effects in the Zr scattering peak for 2 keV 4 He + are found to come from particles scattered from approximately the first 7 nm of the oxide surface. The influence of primary ion energy on the Zr/O ratio is also examined. (author)

  17. Physical properties evolution of sputtered zirconium oxynitride films: effects of the growth temperature

    International Nuclear Information System (INIS)

    Rizzo, A; Signore, M A; Mirenghi, L; Piscopiello, E; Tapfer, L

    2009-01-01

    Zirconium oxynitride (ZrNO) films were deposited by RF reactive magnetron sputtering in water vapour-nitrogen atmosphere varying the deposition temperature from RT to 600 0 C. Optical analysis, x-ray diffraction, x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) are the employed characterization techniques to investigate the influence of the substrate temperature on the films physical properties. It was found that the variation of the substrate temperature from RT to 600 0 C caused a structural transition from cubic phase of Zr 2 ON 2 to ZrN one, as confirmed by TEM observations too. In particular, Forouhi-Bloomer dispersion equations for optical parameters (n and k) and deconvolution of XPS spectra allowed further chemical properties be elucidated. They also permitted identification of two oxynitride phases, γ phase (E g = 1.94 eV) and β phase (E g = 1.7 eV), and an over-stoichiometric nitride one. The use of [E c - E v ] values helped to confirm further the distinction between (γ, β)-phases and N-rich zirconium nitride compound, which is unachievable by using only E g values.

  18. Physical properties evolution of sputtered zirconium oxynitride films: effects of the growth temperature

    Energy Technology Data Exchange (ETDEWEB)

    Rizzo, A; Signore, M A; Mirenghi, L; Piscopiello, E; Tapfer, L [ENEA, Department of Physical Technologies and New Materials, SS7, Appia, km 706, 72100 Brindisi (Italy)

    2009-12-07

    Zirconium oxynitride (ZrNO) films were deposited by RF reactive magnetron sputtering in water vapour-nitrogen atmosphere varying the deposition temperature from RT to 600 {sup 0}C. Optical analysis, x-ray diffraction, x-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM) are the employed characterization techniques to investigate the influence of the substrate temperature on the films physical properties. It was found that the variation of the substrate temperature from RT to 600 {sup 0}C caused a structural transition from cubic phase of Zr{sub 2}ON{sub 2} to ZrN one, as confirmed by TEM observations too. In particular, Forouhi-Bloomer dispersion equations for optical parameters (n and k) and deconvolution of XPS spectra allowed further chemical properties be elucidated. They also permitted identification of two oxynitride phases, {gamma} phase (E{sub g} = 1.94 eV) and {beta} phase (E{sub g} = 1.7 eV), and an over-stoichiometric nitride one. The use of [E{sub c} - E{sub v}] values helped to confirm further the distinction between ({gamma}, {beta})-phases and N-rich zirconium nitride compound, which is unachievable by using only E{sub g} values.

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

    Science.gov (United States)

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

    2013-01-01

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

  20. 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.

  1. Synthesis of Zr-Si-O-N phases by carbonitriding reaction. Characterization of crystalline phases using the Rietveld method

    Directory of Open Access Journals (Sweden)

    Mazzoni A.D.

    2001-01-01

    Full Text Available Zirconium compounds are of great interest for ceramic application due to their excellent thermal and mechanical properties. Zirconium phases of the system Zr-O-C-N were obtained using carbonitriding reactions of zircon mineral (ZrO2.SiO2, under different reaction conditions. The reaction products were studied by X-ray diffraction (XRD using the Rietveld method. Silicon was employed as internal standard. Zirconium compounds formed were m-ZrO2 (monoclinic, beta"-zirconium oxynitride and a cubic Zr(C,N,O phase whose lattice parameter a o depends on the composition. The crystallite sizes of the three zirconium phases were determined also by XRD. The minority phases present are the ones of the Si-O-N-C system. The reaction conditions employed allows to obtain reaction products with low or without silicon content.

  2. Gas-phase mechanisms in the growth of ZrCyN1-y thin films by pulsed reactive crossed-beam laser ablation

    International Nuclear Information System (INIS)

    Spillmann, H.; Clerc, C.; Doebeli, M.; Willmott, P.R.

    2002-01-01

    Superhard zirconium carbonitride films have been grown via pulsed reactive crossed-beam laser ablation (PRCLA) using zirconium metal and a nitrogen- and carbon-containing gas pulse mixture. The control of stoichiometry was much simplified by using the thermally stable gas-phase species N 2 and CH 4 . The gas-phase processes are investigated using quadrupole mass spectroscopy and optical emission spectroscopy. The excitation of the ablation plume depends intimately on the collision partner of the gas pulse, in particular on its density of states and the probability of energy transfer to internal degrees of freedom

  3. Investigation of in-pile grown corrosion films on zirconium-based alloys

    International Nuclear Information System (INIS)

    Gebhardt, O.; Hermann, A.; Bart, G.; Blank, H.; Ray, I.L.F.

    1996-01-01

    In-pile grown corrosion films on different fuel rod claddings (standard Zircaloy-4, extra low tin Zircaloy (ELS), and Zr2.5Nb) have been studied using a variety of experimental techniques. The aim of the investigations was to find out common features and differences between the corrosion layers grown on zirconium alloys having different composition. Methods applied were scanning and transmission electron microscopy (SEM, TEM), electrochemical impedance spectroscopy (EIS), and electrochemical anodization. The morphological differences have been observed between the specimens that could explain the irradiation enhancement of corrosion of Zircaloy-4. The features of the compact oxide close to the oxide/metal interface have been characterized by electrochemical methods. The relationship between the thickness of this protective oxide and the overall oxide thickness has been investigated by EIS. It was found that this relation is dependent on the location of the oxide along the fuel rod and on the corrosion rate

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

    Directory of Open Access Journals (Sweden)

    Mozafari M

    2013-04-01

    Full Text Available Masoud Mozafari,1,2 Erfan Salahinejad,1,3 Vahid Shabafrooz,1 Mostafa Yazdimamaghani,1 Daryoosh Vashaee,4 Lobat Tayebi1,5 1Helmerich Advanced Technology Research Center, School of Materials Science and Engineering, Oklahoma State University, Tulsa, OK, USA; 2Biomaterials Group, Faculty of Biomedical Engineering (Center of Excellence, Amirkabir University of Technology, Tehran, Iran; 3Department of Materials Science and Engineering, School of Engineering, Shiraz University, Shiraz, Iran; 4Helmerich Advanced Technology Research Center, School of Electrical and Computer Engineering, Oklahoma State University, Tulsa, OK, USA; 5School of Chemical Engineering, Oklahoma State University, Tulsa, OK, USA Abstract: Surface modification, particularly coatings deposition, is beneficial to tissue-engineering applications. In this work, bioactive glass/zirconium titanate composite thin films were prepared by a sol-gel spin-coating method. The surface features of the coatings were studied by scanning electron microscopy, atomic force microscopy, and spectroscopic reflection analyses. The results show that uniform and sound multilayer thin films were successfully prepared through the optimization of the process variables and the application of carboxymethyl cellulose as a dispersing agent. Also, it was found that the thickness and roughness of the multilayer coatings increase nonlinearly with increasing the number of the layers. This new class of nanocomposite coatings, comprising the bioactive and inert components, is expected not only to enhance bioactivity and biocompatibility, but also to protect the surface of metallic implants against wear and corrosion. Keywords: bioactive glass, zirconium titanate, spin-coating, microstructural properties, bone/dental applications, tissue engineering

  5. Zirconium doped TiO{sub 2} thin films deposited by chemical spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Juma, A. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Department of Physics and Astronomy, Botswana International University of Science and Technology, Private bag 16, Palapye (Botswana); Oja Acik, I., E-mail: ilona.oja@ttu.ee [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Oluwabi, A.T.; Mere, A. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Mikli, V.; Danilson, M. [Chair of Semiconductor Materials Technology, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Krunks, M. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia)

    2016-11-30

    Highlights: • Mean crystallite size of TiO{sub 2}:Zr film decreases with increasing [Zr] in the solution. • Zr doping supresses the anatase to rutile transformation process in TiO{sub 2} films. • Band gap of TiO{sub 2}:Zr film is 3.4 eV irrespective of the annealing temperature. - Abstract: Chemical spray pyrolysis (CSP) is a flexible deposition technique that allows for mixing of the precursor solutions in different proportions suitable for doping thin films. The CSP method was used to dope TiO{sub 2} thin films with Zr by adding zirconium(IV) acetylacetonate into a solution of titanium(IV) isopropoxide in ethanol stabilized by acetylacetone at [Zr]/[Ti] of 0, 5, 10 and 20 at%. The Zr-doped TiO{sub 2} thin films were uniform and homogeneous showing much smaller grains than the undoped TiO{sub 2} films. Zr stabilized the anatase phase to temperatures above 800 °C depending on Zr concentration in the spray solution. The concentration of Zr determined by XPS was 6.4 at% for the thin film deposited from the 20 at% solution. According to AFM studies, Zr doping decreased the root mean square roughness of TiO{sub 2} film from 5.9 to 1.1 nm. An XRD study of samples with the highest Zr amount showed the ZrTiO{sub 4} phase started forming after annealing at 800 °C. The optical band gap for TiO{sub 2} decreased from 3.3 eV to 3.0 eV after annealing at 800 °C but for the TiO{sub 2}:Zr(20) film it remained at 3.4 eV. The dielectric constant increased by more than four times with Zr-doping and this was associated with the change in the bond formations caused by substitution of Ti by Zr in the lattice.

  6. 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

  7. Nanostructure and bonding of zirconium diboride thin films studied by X-ray spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Stewart, David M., E-mail: david.stewart@maine.edu; Meulenberg, Robert W.; Lad, Robert J., E-mail: rjlad@maine.edu

    2015-12-01

    Zirconium diboride (ZrB{sub 2}) is an important ceramic due to its extremely high melting temperature of 3245 °C and metallic electrical conductivity, properties that make it an ideal candidate thin film electrode material for high temperature electronics. In this report, thin films of varying B:Zr ratio ranging from 3–0.67 have been grown by e-beam evaporation from elemental sources. X-ray absorption spectra at the Zr K-edge were measured before and after annealing in ultra-high vacuum for 9 h at 1000 °C. Films with compositions near ZrB{sub 2} stoichiometry show X-ray absorption fine structure that can be well modeled by crystalline ZrB{sub 2} with a small portion of a coexisting tetragonal zirconia (t-ZrO{sub 2}) phase. Films far from stoichiometry show substantial disorder beyond the nearest-neighbor distances, and after vacuum annealing exhibit high levels of oxidation. Contributions to the X-ray absorption fine structure from a pure Zr phase are very small compared to ZrB{sub 2} and t-ZrO{sub 2} phases. The fact that nearly stoichiometric (3 < B:Zr < 1.6) as-deposited amorphous films form the same crystalline ZrB{sub 2} nanostructure after annealing is particularly encouraging for high temperature thin film electronics applications, because it would allow the production of highly stable electrodes with e-beam evaporation without the need of any high temperature heating during film growth. - Highlights: • Zr–B thin films of different compositions were grown at low substrate temperatures. • EXAFS analysis indicates a ZrB{sub 2} crystal structure after vacuum annealing. • The coexistence of crystalline and amorphous Zr–B phases is also observed. • Films with excess Zr readily form t-ZrO{sub 2} during deposition, which coexists with ZrB{sub 2}. • Low temperature synthesis routes are important for technological applications.

  8. 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)

  9. 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.

  10. 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.

  11. Zircon Carburation Studies as Intermediate Stage in the Zirconium Fabrication

    International Nuclear Information System (INIS)

    Almagro Huertas, V.; Saenz de Tejada Gonzalez, L.; Lopez Rodriguez, M.

    1963-01-01

    Zirconium carbide and carbonitride mixtures were obtained by Kroll's method.Reaction products have been identified by micrography and X-ray diffraction analysis. The optimum graphite content in the initial charge for the carburation reaction has been studied. zirconium, silicon and carbon content in the final product has been controlled as a function of current in the furnace and reaction time.Further chlorination of the final product was performed successfully. (Author) 16 refs

  12. 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

  13. Preparation and properties of molybdenum-tungsten-carbonitrides

    International Nuclear Information System (INIS)

    Schreiner, M.; Ettmayer, P.; Kieffer, R.

    1982-01-01

    Molybdenum-tungsten-carbonitrides can be prepared by reacting prealloyed powders of Mo and W with carbon in the presence of nitrogen or ammonia. Single phase carbonitrides (Mo,W) (C,N) with the WC-type structure can be obtained. The nitrogen content of these carbonitrides increases with increasing molybdenum content. Flowing ammonia has a decarburizing effect, which has to be counterbalanced by an addition of a carbonaceous gas such as methane. Nitrogen instead of ammonia is equally effective and gives carbonitrides which have a nitrogen content only insignificantly lower than the carbonitrides obtained in flowing ammonia. The lattice parameters of the carbonitrides are found to slightly smaller than the lattice parameters of the corresponding carbides. (Author)

  14. 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.

  15. 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.

  16. Synthesis of nano-crystalline zirconium aluminium oxynitride (ZrAlON) composite films by dense plasma Focus device

    Energy Technology Data Exchange (ETDEWEB)

    Khan, I.A.; Hassan, M.; Hussain, T. [Department of Physics, GC University, 54000 Lahore (Pakistan); Ahmad, R., E-mail: ahriaz@gmail.com [Department of Physics, GC University, 54000 Lahore (Pakistan); Zakaullah, M. [Department of Physics, Quaid-i-Azam University, 45320 Islamabad (Pakistan); Rawat, R.S. [National Institute of Education, Nanyang Technological University, Singapore 637616 (Singapore)

    2009-04-01

    Zirconium aluminium oxynitride multiphase composite film is deposited on zirconium substrate using energetic nitrogen ions delivered from dense plasma Focus device. X-ray diffractometer (XRD) results show that five Focus shots are sufficient to initiate the nucleation of ZrN and Al{sub 2}O{sub 3} whereas 10 Focus shots are sufficient to initiate the nucleation of AlN. XRD results reveal that crystal growth of nitrides/oxides increases by increasing Focus shots (up to 30 Focus shots) and resputtering of the previously deposited film is taken place by further increase in Focus shots (40 Focus shots). Scanning electron microscopic (SEM) results indicate the uniform distribution of spherical grains ({approx}35 nm). A smoother surface is observed for 20 Focus shots at 0 deg. angular position. SEM results also show a net-type microstructure (thread like features) of the sample treated for 30 Focus shots whereas rough surface morphology is observed for 40 Focus shots. Energy dispersive spectroscopic profiles show the distribution of different elements present in the deposited composite films. A typical microhardness value of the deposited composite films is 5255 {+-} 10 MPa for 10 grams imposed load which is 3.3 times than the microhardness values of unexposed sample. The microhardness values of the exposed samples increases with increasing Focus shots (up to 30 Focus shots) and decreases for 40 Focus shots treatment due to resputtering of the previously deposited composite film. The microhardness values of the composite films decreases by increasing the sample's angular position.

  17. In situ crystallized zirconium phenylphosphonate films with crystals vertically to the substrate and their hydrophobic, dielectric, and anticorrosion properties.

    Science.gov (United States)

    Cui, Zhaohui; Zhang, Fazhi; Wang, Lei; Xu, Sailong; Guo, Xiaoxiao

    2010-01-05

    The in situ crystallization technique has been utilized to fabricate zirconium phenylphosphonate (ZrPP) films with their hexagonal crystallite perpendicular to the copper substrate. The micro/nano roughness surface structure, as well as the intrinsic hydrophobic characteristic of the surface functional groups, affords ZrPP films excellent hydrophobicity with water contact angle (CA) ranging from 134 degrees to 151 degrees , without any low-surface-energy modification. Particularly, in the corrosive solutions such as acidic or basic solutions over a wide pH from 2 to 12, no obvious fluctuation in CA was observed for all the ZrPP film. The k values of the hydrophobic ZrPP films are in the low-k range (k feature is proposed to bear ZrPP film a more stable low-k value in an ambient atmosphere. Besides, the polarization current of ZrPP films is reduced by 2 orders of magnitude, compared to that of the untreated copper substrate. Even deposited in a vacuum oven for 30 days at room temperature, ZrPP films also show excellent corrosion resistance, indicating a stable anticorrosion property.

  18. Zirconium titanate thin film prepared by surface sol-gel process and effects of thickness on dielectric property

    CERN Document Server

    Kim, C H

    2002-01-01

    Single phase of multicomponent oxide ZrTiO sub 4 film could be prepared through surface sol-gel route simply by coating the mixture of 100mM zirconium butoxide and titanium butoxide on Pt/Ti/SiO sub 2 /Si(100) substrate, following pyrolysis at 450 .deg. C, and annealing it at 770 .deg. C. The dielectric constant of the film was reduced as the film thickness decreased due to of the interfacial effects caused by layer/electrode and a few voids inside the multilayer. However, the dielectric property was independent of applied dc bias sweeps voltage (-2 to +2 V). The dielectric constant of bulk film, 31.9, estimated using series-connected capacitor model was independent of film thickness and frequency in the measurement range, but theoretical interfacial thickness, t sub i , was dependent on the frequency. It reached a saturated t sub i value, 6.9 A, at high frequency by extraction of some capacitance component formed at low frequency range. The dielectric constant of bulk ZrTiO sub 4 pellet-shaped material was 3...

  19. 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.

  20. Thin polycrystalline diamond films protecting zirconium alloys surfaces: From technology to layer analysis and application in nuclear facilities

    Energy Technology Data Exchange (ETDEWEB)

    Ashcheulov, P. [Institute of Physics, Academy of Sciences Czech Republic v.v.i, Na Slovance 2, CZ-182 21, Prague 8 (Czech Republic); Škoda, R.; Škarohlíd, J. [Czech Technical University in Prague, Faculty of Mechanical Engineering, Technická 4, Prague 6, CZ-160 07 (Czech Republic); Taylor, A.; Fekete, L.; Fendrych, F. [Institute of Physics, Academy of Sciences Czech Republic v.v.i, Na Slovance 2, CZ-182 21, Prague 8 (Czech Republic); Vega, R.; Shao, L. [Texas A& M University, Department of Nuclear Engineering TAMU-3133, College Station, TX TX 77843 (United States); Kalvoda, L.; Vratislav, S. [Faculty of Nuclear Science and Physical Engineering, Czech Technical University in Prague, Brehova 7, CZ-115 19, Prague 1 (Czech Republic); Cháb, V.; Horáková, K.; Kůsová, K.; Klimša, L.; Kopeček, J. [Institute of Physics, Academy of Sciences Czech Republic v.v.i, Na Slovance 2, CZ-182 21, Prague 8 (Czech Republic); Sajdl, P.; Macák, J. [University of Chemistry and Technology, Power Engineering Department, Technická 3, Prague 6, CZ-166 28 (Czech Republic); Johnson, S. [Nuclear Fuel Division, Westinghouse Electric Company, 5801 Bluff Road, Hopkins, SC 29209 (United States); Kratochvílová, I., E-mail: krat@fzu.cz [Institute of Physics, Academy of Sciences Czech Republic v.v.i, Na Slovance 2, CZ-182 21, Prague 8 (Czech Republic); Faculty of Nuclear Science and Physical Engineering, Czech Technical University in Prague, Brehova 7, CZ-115 19, Prague 1 (Czech Republic)

    2015-12-30

    Graphical abstract: - Highlights: • In this work we showed that films prepared by MW-LA-PECVD technology can be used as anticorrosion protective layer for Zircaloy2 nuclear fuel claddings at elevated temperatures (950 °C) when α phase of zirconium changes to β phase (more opened for oxygen/hydrogen diffusion). Quality of PCD films was examined by Raman spectroscopy, XPS, SEM, AFM and SIMS analysis. • The polycrystalline diamond films were of high quality - without defects and contaminations. After hot steam oxidation (950 °C) a high level of structural integrity of PCD layer was observed. Both sp{sup 2} and sp{sup 3} C phases were present in the protective PCD layer. Higher resistance and a lower degree of impedance dispersion was found in the hot steam oxidized PCD coated Zircaloy2 samples, which may suggest better protection of the Zircaloy2 surface. The PCD layer blocks the hydrogen diffusion into the Zircaloy2 surface thus protecting the material from degradation. • Hot steam oxidation tests confirmed that PCD coated Zircaloy2 surfaces were effectively protected against corrosion. Presented results demonstrate that the PCD anticorrosion protection can significantly prolong service life of Zircaloy2 nuclear fuel claddings in nuclear reactors even at elevated temperatures. - Abstract: Zirconium alloys can be effectively protected against corrosion by polycrystalline diamond (PCD) layers grown in microwave plasma enhanced linear antenna chemical vapor deposition apparatus. Standard and hot steam oxidized PCD layers grown on Zircaloy2 surfaces were examined and the specific impact of polycrystalline Zr substrate surface on PCD layer properties was investigated. It was found that the presence of the PCD coating blocks hydrogen diffusion into the Zircaloy2 surface and protects Zircaloy2 material from degradation. PCD anticorrosion protection of Zircaloy2 can significantly prolong life of Zircaloy2 material in nuclear reactors even at temperatures above Zr

  1. Three-dimensional ordered titanium dioxide-zirconium dioxide film-based microfluidic device for efficient on-chip phosphopeptide enrichment.

    Science.gov (United States)

    Zhao, De; He, Zhongyuan; Wang, Gang; Wang, Hongzhi; Zhang, Qinghong; Li, Yaogang

    2016-09-15

    Microfluidic technology plays a significant role in separating biomolecules, because of its miniaturization, integration, and automation. Introducing micro/nanostructured functional materials can improve the properties of microfluidic devices, and extend their application. Inverse opal has a three-dimensional ordered net-like structure. It possesses a large surface area and exhibits good mass transport, making it a good candidate for bio-separation. This study exploits inverse opal titanium dioxide-zirconium dioxide films for on-chip phosphopeptide enrichment. Titanium dioxide-zirconium dioxide inverse opal film-based microfluidic devices were constructed from templates of 270-, 340-, and 370-nm-diameter poly(methylmethacrylate) spheres. The phosphopeptide enrichments of these devices were determined by matrix-assisted laser desorption/ionization time-of-flight (MALDI-TOF) mass spectrometry. The device constructed from the 270-nm-diameter sphere template exhibited good comprehensive phosphopeptide enrichment, and was the best among these three devices. Because the size of opal template used in construction was the smallest, the inverse opal film therefore had the smallest pore sizes and the largest surface area. Enrichment by this device was also better than those of similar devices based on nanoparticle films and single component films. The titanium dioxide-zirconium dioxide inverse opal film-based device provides a promising approach for the efficient separation of various biomolecules. Copyright © 2016 Elsevier Inc. All rights reserved.

  2. Deposition and characterization of zirconium nitride (ZrN) thin films by reactive magnetron sputtering with linear gas ion source and bias voltage

    Energy Technology Data Exchange (ETDEWEB)

    Kavitha, A.; Kannan, R. [Department of Physics, University College of Engineering, Anna University, Dindugal-624622 (India); Subramanian, N. Sankara [Department of Physics, Thiagarajar College of Engineering, Madurai -625015, Tamilnadu (India); Loganathan, S. [Ion Plating, Titan Industries Ltd., Hosur - 635126, Tamilnadu (India)

    2014-04-24

    Zirconium nitride thin films have been prepared on stainless steel substrate (304L grade) by reactive cylindrical magnetron sputtering method with Gas Ion Source (GIS) and bias voltage using optimized coating parameters. The structure and surface morphologies of the ZrN films were characterized using X-ray diffraction, atomic microscopy and scanning electron microscopy. The adhesion property of ZrN thin film has been increased due to the GIS. The coating exhibits better adhesion strength up to 10 N whereas the ZrN thin film with bias voltage exhibits adhesion up to 500 mN.

  3. 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.

  4. Facile Synthesis of Ternary Boron Carbonitride Nanotubes

    Directory of Open Access Journals (Sweden)

    Luo Lijie

    2009-01-01

    Full Text Available Abstract In this study, a novel and facile approach for the synthesis of ternary boron carbonitride (B–C–N nanotubes was reported. Growth occurred by heating simple starting materials of boron powder, zinc oxide powder, and ethanol absolute at 1150 °C under a mixture gas flow of nitrogen and hydrogen. As substrate, commercial stainless steel foil with a typical thickness of 0.05 mm played an additional role of catalyst during the growth of nanotubes. The nanotubes were characterized by SEM, TEM, EDX, and EELS. The results indicate that the synthesized B–C–N nanotubes exhibit a bamboo-like morphology and B, C, and N elements are homogeneously distributed in the nanotubes. A catalyzed vapor–liquid–solid (VLS mechanism was proposed for the growth of the nanotubes.

  5. 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.

  6. Theoretical Investigations of the Hexagonal Germanium Carbonitride

    Directory of Open Access Journals (Sweden)

    Xinhai Yu

    2018-04-01

    Full Text Available The structural, mechanical, elastic anisotropic, and electronic properties of hexagonal germanium carbonitride (h-GeCN are systematically investigated using the first-principle calculations method with the ultrasoft pseudopotential scheme in the frame of generalized gradient approximation in the present work. The h-GeCN are mechanically and dynamically stable, as proved by the elastic constants and phonon spectra, respectively. The h-GeCN is brittle because the ratio B/G and Poisson’s ratio v of the h-GeCN are less than 1.75 and 0.26, respectively. For h-GeCN, from brittleness to ductility, the transformation pressures are 5.56 GPa and 5.63 GPa for B/G and Poisson’s ratio v, respectively. The h-GeCN exhibits the greater elastic anisotropy in Young’s modulus and the sound velocities. In addition, the calculated band structure of h-GeCN reveals that there is no band gap for h-GeCN with the HSE06 hybrid functional, so the h-GeCN is metallic.

  7. 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

  8. 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

  9. 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

  10. High-Transparency Sputtered In2O3 and ITO Films Containing Zirconium (Presentation)

    International Nuclear Information System (INIS)

    Gessert, T. A.; Yoshida, Y.; Fesenmaier, C. C.; Coutts, T. J.

    2007-01-01

    Our recent investigations have identified a method to produce ITO-like films that are less sensitive to variations in the oxygen-containing deposition ambient. Specifically, we are studying the effect of adding small amounts of Zr to both In2O3 and ITO ceramic sputtering targets

  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. 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.

  13. 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

  14. Zircon Carburation Studies as Intermediate Stage in the Zirconium Fabrication; Estudios encaminados a la carburacion del circon como etapa intermedia en la obtencion de circonio

    Energy Technology Data Exchange (ETDEWEB)

    Almagro Huertas, V; Saenz de Tejada Gonzalez, L.; Lopez Rodriguez, M

    1963-07-01

    Zirconium carbide and carbonitride mixtures were obtained by Kroll's method.Reaction products have been identified by micrography and X-ray diffraction analysis. The optimum graphite content in the initial charge for the carburation reaction has been studied. zirconium, silicon and carbon content in the final product has been controlled as a function of current in the furnace and reaction time.Further chlorination of the final product was performed successfully. (Author) 16 refs.

  15. Zircon Carburation Studies as Intermediate Stage in the Zirconium Fabrication; Estudios encaminados a la carburacion del circon como etapa intermedia en la obtencion de circonio

    Energy Technology Data Exchange (ETDEWEB)

    Almagro Huertas, V.; Saenz de Tejada Gonzalez, L.; Lopez Rodriguez, M.

    1963-07-01

    Zirconium carbide and carbonitride mixtures were obtained by Kroll's method.Reaction products have been identified by micrography and X-ray diffraction analysis. The optimum graphite content in the initial charge for the carburation reaction has been studied. zirconium, silicon and carbon content in the final product has been controlled as a function of current in the furnace and reaction time.Further chlorination of the final product was performed successfully. (Author) 16 refs.

  16. Fabrication and characterization of polyvinyl alcohol/metal (Ca, Mg, Ti) doped zirconium phosphate nanocomposite films for scaffold-guided tissue engineering application.

    Science.gov (United States)

    Kalita, Himani; Pal, Pallabi; Dhara, Santanu; Pathak, Amita

    2017-02-01

    Nanocomposite films of polyvinyl alcohol (PVA) and zirconium phosphate (ZrP)/doped ZrP (doped with Ca, Mg, Ti) nanoparticles have been developed by solvent casting method to assess their potential as matrix material in scaffold-guided tissue engineering application. The prepared ZrP and doped ZrP nanoparticles as well as the nanocomposite films were characterized by various spectroscopic and microscopic techniques. Nanoindentation studies revealed improved nanomechanical properties in the PVA/doped ZrP nanocomposite films (highest for PVA/Ti doped ZrP: hardness=262.4MPa; elastic modulus=5800MPa) as compared to the PVA/ZrP and neat PVA films. In-vitro cell culture experiments carried out to access the cellular viability, attachment, proliferation, and migration on the substrates, using mouse fibroblast (3T3) cell lines, inferred enhanced bioactivity in the PVA/doped ZrP nanocomposite films (highest for PVA/Ca doped ZrP) in contrast to PVA/ZrP and neat PVA films. Controlled biodegradability as well as swelling behavior, superior bioactivity and improved mechanical properties of the PVA/doped ZrP nanocomposite films make them promising matrix materials for scaffold-guided tissue engineering application. Copyright © 2016 Elsevier B.V. All rights reserved.

  17. X-Ray fluorescence of microquantities of hafnium in zirconium by precipitation as thin film

    International Nuclear Information System (INIS)

    Vigoda de Leyt, Dora; Caridi, A.F.; Deibe, Jorge

    1988-01-01

    The importance of Zr and Hf in the nuclear industry represents and increasing need for the development of reliable chemical methods to determine Hf traces in Zr matrix. A precipitation method in amoniacal medium was developed. A thin film is obtained where matrix effects are absent or minimized. Hf in the range of 5-70.10 -9 Kg in a 5.10 -6 Kg Zr matrix was studied. Fluorescence Hf Lα and Hf Lβ X-rays are excited by a W-anode tube 17 kV-25mA and 50kV-25mA. Radiation scattered by the tube was used as internal standard. Bartlett criterion was used for the regression analysis. Determination limit was fixed in 5±4. 10 -9 Kg Hf at a 95 % probability. (Author) [es

  18. 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

  19. Fabrication and characterization of polyvinyl alcohol/metal (Ca, Mg, Ti) doped zirconium phosphate nanocomposite films for scaffold-guided tissue engineering application

    International Nuclear Information System (INIS)

    Kalita, Himani; Pal, Pallabi; Dhara, Santanu; Pathak, Amita

    2017-01-01

    Nanocomposite films of polyvinyl alcohol (PVA) and zirconium phosphate (ZrP)/doped ZrP (doped with Ca, Mg, Ti) nanoparticles have been developed by solvent casting method to assess their potential as matrix material in scaffold-guided tissue engineering application. The prepared ZrP and doped ZrP nanoparticles as well as the nanocomposite films were characterized by various spectroscopic and microscopic techniques. Nanoindentation studies revealed improved nanomechanical properties in the PVA/doped ZrP nanocomposite films (highest for PVA/Ti doped ZrP: hardness = 262.4 MPa; elastic modulus = 5800 MPa) as compared to the PVA/ZrP and neat PVA films. In-vitro cell culture experiments carried out to access the cellular viability, attachment, proliferation, and migration on the substrates, using mouse fibroblast (3T3) cell lines, inferred enhanced bioactivity in the PVA/doped ZrP nanocomposite films (highest for PVA/Ca doped ZrP) in contrast to PVA/ZrP and neat PVA films. Controlled biodegradability as well as swelling behavior, superior bioactivity and improved mechanical properties of the PVA/doped ZrP nanocomposite films make them promising matrix materials for scaffold-guided tissue engineering application. - Highlights: • PVA/ZrP (undoped/doped with Ca, Mg and Ti) nanocomposite scaffolds were developed. • The nanocomposites were prepared via solvent casting method. • PVA/doped ZrP films exhibited enhanced mechanical properties than PVA/undoped ZrP. • Excellent bioactivity was observed in the PVA/doped ZrP films than PVA/undoped ZrP.

  20. Fabrication and characterization of polyvinyl alcohol/metal (Ca, Mg, Ti) doped zirconium phosphate nanocomposite films for scaffold-guided tissue engineering application

    Energy Technology Data Exchange (ETDEWEB)

    Kalita, Himani [Department of Chemistry, Indian Institute of Technology Kharagpur, West Bengal 721302 (India); Pal, Pallabi; Dhara, Santanu [School of Medical Science and Technology, Indian Institute of Technology Kharagpur, West Bengal 721302 (India); Pathak, Amita, E-mail: ami@chem.iitkgp.ernet.in [Department of Chemistry, Indian Institute of Technology Kharagpur, West Bengal 721302 (India)

    2017-02-01

    Nanocomposite films of polyvinyl alcohol (PVA) and zirconium phosphate (ZrP)/doped ZrP (doped with Ca, Mg, Ti) nanoparticles have been developed by solvent casting method to assess their potential as matrix material in scaffold-guided tissue engineering application. The prepared ZrP and doped ZrP nanoparticles as well as the nanocomposite films were characterized by various spectroscopic and microscopic techniques. Nanoindentation studies revealed improved nanomechanical properties in the PVA/doped ZrP nanocomposite films (highest for PVA/Ti doped ZrP: hardness = 262.4 MPa; elastic modulus = 5800 MPa) as compared to the PVA/ZrP and neat PVA films. In-vitro cell culture experiments carried out to access the cellular viability, attachment, proliferation, and migration on the substrates, using mouse fibroblast (3T3) cell lines, inferred enhanced bioactivity in the PVA/doped ZrP nanocomposite films (highest for PVA/Ca doped ZrP) in contrast to PVA/ZrP and neat PVA films. Controlled biodegradability as well as swelling behavior, superior bioactivity and improved mechanical properties of the PVA/doped ZrP nanocomposite films make them promising matrix materials for scaffold-guided tissue engineering application. - Highlights: • PVA/ZrP (undoped/doped with Ca, Mg and Ti) nanocomposite scaffolds were developed. • The nanocomposites were prepared via solvent casting method. • PVA/doped ZrP films exhibited enhanced mechanical properties than PVA/undoped ZrP. • Excellent bioactivity was observed in the PVA/doped ZrP films than PVA/undoped ZrP.

  1. Synthesis, sintering properties and thermal conductivity of uranium carbonitrides

    International Nuclear Information System (INIS)

    Wolters, R.A.M.

    1978-01-01

    An introduction to the applications and chemistry of uranium carbonitrides is given including the potential use as a nuclear fuel. The powder synthesis of UC, UN and mixtures of UC and UN by a cyclic process is described. The correlation between the composition ratio UN/(UC+UN) in the final product and the parameters of the process is only determined qualitatively. Batch synthesis of a powder does not lead to an increase of the content of metallic impurities and oxygen. The impurity level is determined by that of the starting uranium metal and the thermal conductivity of the sintered compacts of uranium carbonitrides are determined via the measurement of the thermal diffusivity at 1100-1700 K. (Auth.)

  2. Method of preparing uranium nitride or uranium carbonitride bodies

    International Nuclear Information System (INIS)

    Wilhelm, H.A.; McClusky, J.K.

    1976-01-01

    Sintered uranium nitride or uranium carbonitride bodies having a controlled final carbon-to-uranium ratio are prepared, in an essentially continuous process, from U 3 O 8 and carbon by varying the weight ratio of carbon to U 3 O 8 in the feed mixture, which is compressed into a green body and sintered in a continuous heating process under various controlled atmospheric conditions to prepare the sintered bodies. 6 claims, no drawings

  3. Carbonitrides in the system Ta-TaC-TaN

    International Nuclear Information System (INIS)

    Ritzhaupt-Kleissl, H.J.

    1975-04-01

    Specimens have been prepared in the binary section TaC-TaN and the carbon-rich region of the Ta-TaC-TaN system by hot pressing and subsequent homogenisation. It was possible to prepare nitrogen-rich carbonitrides by homogenizing them at 1,800 0 C under a nitrogen-pressure of 50 at up to the composition of 70 mol% TaN/30 mol% TaC. Those carbonitrides containing less than 25 at% nitrogen could be prepared by homogenisation at 2,000 0 C under a nitrogen-pressure of 600 Torr. Subsequent ageing at temperatures of 1,200, 1,300 and 1,400 0 C in high vacuum as well as at 1 at nitrogen resulted in the appearance of precipitations of epsilon-TaN, β-Ta 2 (C,N) and of the zeta-phase. The type amount and shape of the precipitated phases are dependent on the ageing conditions and on the composition the specimens. Single phase specimens with compositions close to the non-metal deficient phase boundary as well as multi-phase carbonitrides with high nitrogen contents and very fine precipitates showed values of the Vickers-hardness up to 3,000 kp/mm 2 at room temperature. With regard to the hot hardness up to a temperature of 1,300 0 C specimens aged in high vacuum were superior to those which were only homogenized as well as to those aged under a nitrogen-pressure of 1 at. On an average the best hardness-values have been found at room temperature as well as at temperatures up to 1,300 0 C for carbonitrides consisting of 50 mol% TaC/50 mol% TaN after homogenisation and subsequent ageing for 40 h at 1,300 0 C. (orig.) [de

  4. Flame retardancy and thermal properties of epoxy acrylate resin/alpha-zirconium phosphate nanocomposites used for UV-curing flame retardant films

    International Nuclear Information System (INIS)

    Xing Weiyi; Jie Ganxin; Song Lei; Wang Xin; Lv Xiaoqi; Hu Yuan

    2011-01-01

    This paper reported the UV-curing flame retardant film, which consisted of epoxy acrylate resin (EA) used as an oligomer, tri(acryloyloxyethyl) phosphate (TAEP) and triglycidyl isocyanurate acrylate (TGICA) used as flame retardant (FR). The flame retardancy and thermal properties of films were reinforced by using alpha-zirconium phosphate (α-Zr (HPO 4 ) 2 H 2 O, α-ZrP). The morphology of nanocomposite film was characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The results showed that the organophilic α-ZrP (OZrP) layers were dispersed well in epoxy acrylate resin. Microscale Combustion Calorimeter (MCC), thermogravimetric analysis (TGA) and thermogravimetric analysis/infrared spectrometry (TGA-IR) were used to characterize the flame retardant property and thermal stability. It was found that the incorporation of TAEP and TGICA can reduce the flammability of EA. Moreover, further reductions were observed due to the addition of OZrP. The char residue for systems with or without OZrP was also explored by scanning electron microscopy (SEM).

  5. 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)

  6. Green Synthesis of Boron Carbonitride with High Capacitance

    Directory of Open Access Journals (Sweden)

    Dongping Chen

    2018-03-01

    Full Text Available Boron carbonitrides (BCN have attracted great interest in superhard or energy storage materials. In this work, thin BCN sheets were synthesized at 250 °C by a facile and green solvothermal method. The structure and morphology were characterized by X-ray diffraction (XRD, Raman spectroscopy, X-ray photoelectron spectroscopy (XPS, scanning electron microscopy (SEM, and transmission electron microscopy (TEM. Based on the results of electrochemical experiments, the thin BCN sheet exhibited excellent capacitance performance (343.1 F/g at a current density of 0.5 A/g and cycling stability (90%, which showed high potential applications in supercapacitors.

  7. 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)

  8. Dissolving of Nb and Ti carbonitride precipitates in microalloyed steels

    Institute of Scientific and Technical Information of China (English)

    Wenjin Nie; Shanwu Yang; Shaoqiang Yuan; Xinlai He

    2003-01-01

    The dissolving behaviour of Nb and Ti carbonitride precipitates in microalloyed steels during isothermal holding at 1300℃ was investigated by Transmission electron microscopy (TEM) and energy dispersion x-ray spectrum (EDX). It was found that all precipitates in Nb-Ti microalloyed steel are (Nb, Ti)(C,N). With holding time increasing, the atomic ratio of Nb/Ti in precipitates decrease gradually. These precipitates still existe even after holding for 48 h at 1300℃ while Nb(C,N) precipitates dissolve away in Nb microalloyed steel only after 4 h at the same temperature. These results show that formation and thermostability of precipitates are considerably influenced by interaction between Nb and Ti.

  9. Effects of annealing on the compositional heterogeneity and structure in zirconium-based bulk metallic glass thin films

    International Nuclear Information System (INIS)

    He, L.; Chu, J.P.; Li, C.-L.; Lee, C.-M.; Chen, Y.-C.; Liaw, P.K.; Voyles, P.M.

    2014-01-01

    In-situ heating fluctuation electron microscopy and scanning transmission electron microscopy have been utilized to study compositional and structural heterogeneities in Zr 51 Cu 32 Al 9 Ni 8 thin films upon annealing. Composition fluctuations are present in the as-deposited thin films. Well below the glass transition temperature, the composition fluctuations increase with annealing time. Short- and medium-range order also change with annealing temperature. The observed heterogeneities in the glass structure persist until annealing causes crystallization. The 20 nm thick Zr 51 Cu 32 Al 9 Ni 8 films contain oxide layers both at the surface and the film/substrate interface with the total thickness of 7–8 nm. In-situ annealing increased the oxygen content of the whole films to about 24 wt.% after 2 h at 400 °C. - Highlights: • Zr 51 Cu 32 Al 9 Ni 8 thin films were studied with in-situ heating electron microscopy. • Annealing at 400 °C increases the Zr and Cu compositional fluctuations. • Short-range order in Zr 51 Cu 32 Al 9 Ni 8 becomes less homogeneous above 350 °C. • Medium-range order changes in degree and types at 400 °C, well below T g . • Annealing increases composition and structure heterogeneities until crystallization

  10. Oxidation Behavior of Titanium Carbonitride Coating Deposited by Atmospheric Plasma Spray Synthesis

    Science.gov (United States)

    Zhu, Lin; He, Jining; Yan, Dianran; Liao, Hanlin; Zhang, Nannan

    2017-10-01

    As a high-hardness and anti-frictional material, titanium carbonitride (TiCN) thick coatings or thin films are increasingly being used in many industrial fields. In the present study, TiCN coatings were obtained by atmospheric plasma spray synthesis or reactive plasma spray. In order to promote the reaction between the Ti particles and reactive gases, a home-made gas tunnel was mounted on a conventional plasma gun to perform the spray process. The oxidation behavior of the TiCN coatings under different temperatures in static air was carefully investigated. As a result, when the temperature was over 700 °C, the coatings suffered from serious oxidation, and finally they were entirely oxidized to the TiO2 phase at 1100 °C. The principal oxidation mechanism was clarified, indicating that the oxygen can permeate into the defects and react with TiCN at high temperatures. In addition, concerning the use of a TiCN coating in high-temperature conditions, the microhardness of the oxidized coatings at different treatment temperatures was also evaluated.

  11. 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.

  12. 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

  13. 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}.

  14. Thin polycrystalline diamond films protecting zirconium alloys surfaces: from technology to layer analysis and application in nuclear facilities

    Czech Academy of Sciences Publication Activity Database

    Ashcheulov, Petr; Škoda, R.; Škarohlíd, J.; Taylor, Andrew; Fekete, Ladislav; Fendrych, František; Vega, R.; Shao, L.; Kalvoda, L.; Vratislav, S.; Cháb, Vladimír; Horáková, K.; Kůsová, Kateřina; Klimša, Ladislav; Kopeček, Jaromír; Sajdl, P.; Macák, J.; Johnson, S.; Kratochvílová, Irena

    2015-01-01

    Roč. 359, Dec (2015), s. 621-628 ISSN 0169-4332 R&D Projects: GA ČR(CZ) GA15-05095S; GA TA ČR TA04020156; GA MŠk LO1409; GA MŠk(CZ) LM2011029 Grant - others:SAFMAT(XE) CZ.2.16/3.1.00/22132 Institutional support: RVO:68378271 Keywords : metal coatings * thin polycrystalline diamond film * impedance spectroscopy * Raman spectroscopy * XPS Subject RIV: JI - Composite Materials Impact factor: 3.150, year: 2015

  15. 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

  16. 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.

  17. Internal carbonitriding behavior of Ni-V, Ni-Cr, and Ni-3Nb alloys

    International Nuclear Information System (INIS)

    Allen, A.T.; Douglass, D.L.

    1999-01-01

    Ni-2V, Ni-5V, Ni-12V, Ni-10Cr, Ni-20Cr, and Ni-3Nb alloys were carbonitrided in C 3 H 6 and NH 3 gas mixtures (bal H 2 ) over the range 700--1,000 C. Carbonitridation of Ni-12V and Ni-20Cr in C 3 H 6 /NH 3 /H 2 (1.5/1.5/97 v/o) and (1.5/10/88.5 v/o) produced duplex subscales consisting of near-surface nitrides with underlying carbides. Growth of each zone obeyed the parabolic rate law under most conditions. The presence of carbon generally did not effect the depth of the nitride zones compared to nitriding the alloys in NH 3 /H 2 (10/90 v/o). However, at 700 C, the nitride zones were deeper in the carbonitrided Ni-V alloys and Ni-20Cr. The presence of nitrogen generally increased the depth of the carbide zones in Ni-12V and Ni-20Cr compared to carburizing these alloys in C 3 H 6 /H 2 (1.5/98.5 v/o). VN, CrN, and NbN formed in Ni-V, Ni-Cr, and Ni-Nb alloys, respectively, whereas the underlying carbide layers contained V 4 C 3 in Ni-12V, Cr 3 C 2 above a zone of Cr 7 C 3 in Ni-20Cr, and NbC in Ni-3Nb. The solubilities and diffusivities of nitrogen and carbon in nickel were determined. Nitrogen and carbon each exhibited retrograde solubility with temperature in pure Ni in both carbonitriding environments. Nitrogen diffusion in nickel was generally lower in each carbonitriding mixture compared to nitrogen diffusion in a nitriding environment, except at 700 C when nitrogen diffusion was higher. Carbon diffusion in nickel was generally higher in the carbonitriding environments compared to carbon diffusion in a carburizing environment

  18. Carbonitriding of low alloy steels: Mechanical and metallurgical responses

    Energy Technology Data Exchange (ETDEWEB)

    Dal' Maz Silva, W., E-mail: waltermateriais@me.com [Institut Jean Lamour – UMR CNRS–Université de Lorraine, 7198, Parc de Saurupt, Nancy 54011 (France); Institut de Recherche Technologique M2P, Metz 57070 (France); Dulcy, J., E-mail: jacky.dulcy@univ-lorraine.fr [Institut Jean Lamour – UMR CNRS–Université de Lorraine, 7198, Parc de Saurupt, Nancy 54011 (France); Ghanbaja, J., E-mail: jaafar.ghanbaja@univ-lorraine.fr [Institut Jean Lamour – UMR CNRS–Université de Lorraine, 7198, Parc de Saurupt, Nancy 54011 (France); Redjaïmia, A., E-mail: abdelkrim.redjaimia@univ-lorraine.fr [Institut Jean Lamour – UMR CNRS–Université de Lorraine, 7198, Parc de Saurupt, Nancy 54011 (France); Michel, G., E-mail: gregory.michel@irt-m2p.fr [Institut de Recherche Technologique M2P, Metz 57070 (France); Thibault, S., E-mail: simon.thibault@safran.fr [Safran Tech, Magny les Hameaux (France); Belmonte, T., E-mail: thierry.belmonte@univ-lorraine.fr [Institut Jean Lamour – UMR CNRS–Université de Lorraine, 7198, Parc de Saurupt, Nancy 54011 (France)

    2017-05-02

    Metallurgical and mechanical responses of alloys 16NiCrMo13 and 23MnCrMo5 to the addition of carbon and/or nitrogen were investigated. Diffusion profiles of these interstitial elements were established by atmospheric pressure carburizing, austenitic nitriding, and a sequence of carburizing and nitriding – the carbonitriding. All treatments were performed at 1173 K under CO-H{sub 2} and/or NH{sub 3} based atmospheres. After enrichment, each sample was (i) room-temperature oil-quenched and (ii) immersed in boiling nitrogen prior to (iii) the stress relief treatment. Cross-section hardness profiles were evaluated after each of these steps. Electron probe microanalysis (EPMA) allowed for the determination of both carbon and nitrogen diffusion profiles after quenching. In order to estimate the fraction of nitrides formed during the enrichment of the alloys, these measured profiles were employed in the simulation of local equilibrium at each evaluated position. This allowed for the computation of total solid solution interstitial content, which was expressed in atomic fraction. Plots of as-quenched hardness against the square root of the computed interstitial content, i.e. the sum of solution carbon and the remaining nitrogen, show the complementary character of these elements in determining the mechanical properties of the materials prior to stress relief treatment. Tempering of carbon-nitrogen martensite resulted in hardness drop to a lesser degree than the one measured on carbon martensite with equivalent interstitial content. In order to investigate this behavior, transmission electron microscopy (TEM) analyses were performed. Results showed the precipitation of two morphologies of Fe{sub 16}N{sub 2} in the nitrogen-rich case and image analysis confirmed the simulated fraction of nitrides.

  19. Mathematical Modelling of Carbonitride Precipitation during Hot Working in Nb Microalloyed Steels

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    Based on thermodynamics and kinetics, precipitation behavior of microalloyed steels was analyzed. Deformation greatly promotes isothermal carbonitride precipitation and makes C-curve shift leftwards. The position and shape of C-curve also depend on the content of Nb and N. C-curve shifts leftwards a little when N content increases and the nose temperature is raised with increasing Nb content. Deformation shortened precipitation start time during continuous cooling, raised precipitation start temperature, accelerated precipitation kinetics of carbonitrides. With decreasing the finishing temperature and coiling temperature, the precipitates volume fraction increases and strength increment is raised during hot rolling. The simulated results are in agreementwith experiment results.

  20. 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)

  1. 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.

  2. Effect of nitrogen flow ratio on structure and properties of zirconium ...

    Indian Academy of Sciences (India)

    Abstract. In this study, zirconium nitride thin films were deposited on Si substrates by ion beam sputtering (IBS). Influence of N2/(N2+Ar) on the structural and physical properties of the films has been investigated with respect to the atomic ratio between nitrogen and zirconium. It was found that the thickness of layers ...

  3. Microwave - Assisted Intercatation of 1-Alkanols and 1, omega-Alkanediols into alpha-Zirconium Phosphate. Evidence of Conformational Phase Transitions in the Bimolecular Film of Alkyl Chains

    Czech Academy of Sciences Publication Activity Database

    Costantino, U.; Vivani, R.; Zima, Vítězslav; Beneš, Ludvík; Melánová, Klára

    xx, č. 18 (2002), s. 1211-1217 ISSN 0743-7463 R&D Projects: GA ČR GA202/01/0520 Keywords : zirconium phosphate * intercalation * alkanols Subject RIV: CA - Inorganic Chemistry Impact factor: 3.248, year: 2002

  4. Thermophysical and elastic properties of titanium carbonitrides containing molybdenum and tungsten

    International Nuclear Information System (INIS)

    Matsuda, Tetsushi; Matsubara, Hideaki

    2013-01-01

    Highlights: ► (Ti,Me)(C,N) sintered bodies were prepared by hot-pressing. ► The thermophysical and elastic properties of the carbonitrides were evaluated. ► The porosities of the specimens were less than 1%. ► The Young’s modulus decreases with increasing Mo content. ► The Debye temperatures decrease with increasing Mo/W content. -- Abstract: Titanium carbonitride has good mechanical properties such as high hardness and high Young’s modulus. It is a major raw material for Ti(C,N)-based cermets, and their properties are strongly dependent on the properties of titanium carbonitrides. The thermophysical and elastic properties of the carbonitride need to be systematically investigated, so as to be used for designing cutting tools and wear-resistant tools. The thermophysical and elastic properties of (Ti,Me)(C,N) (Me = Mo. W) sintered bodies prepared by hot-pressing at 2200 °C were evaluated. The porosities of the specimens were less than 1%. The Young’s modulus decreased with increasing Mo, which seems to be the result of vacancy formation. The thermal expansion coefficient, the thermal conductivity and the Debye temperatures of (Ti,Me)(C,N) sintered bodies decreased with increasing Mo/W content

  5. 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)

  6. 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

  7. 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

  8. 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.

  9. Electrochemical study of lithium insertion into carbon-rich polymer-derived silicon carbonitride ceramics

    International Nuclear Information System (INIS)

    Kaspar, Jan; Mera, Gabriela; Nowak, Andrzej P.; Graczyk-Zajac, Magdalena; Riedel, Ralf

    2010-01-01

    This paper presents the lithium insertion into carbon-rich polymer-derived silicon carbonitride (SiCN) ceramic synthesized by the thermal treatment of poly(diphenylsilylcarbodiimide) at three temperatures, namely 1100, 1300, and 1700 o C under 0.1 MPa Ar atmosphere. At lower synthesis temperatures, the material is X-ray amorphous, while at 1700 o C, the SiCN ceramic partially crystallizes. Anode materials prepared from these carbon-rich SiCN ceramics without any fillers and conducting additives were characterized using cyclic voltammetry and chronopotentiometric charging/discharging. We found that the studied silicon carbonitride ceramics demonstrate a promising electrochemical behavior during lithium insertion/extraction in terms of capacity and cycling stability. The sample synthesized at 1300 o C exhibits a reversible capacity of 392 mAh g -1 . Our study confirms that carbon-rich SiCN phases are electrochemically active materials in terms of Li inter- and deintercalation.

  10. Fundamentals of liquid phase for modern cermets and functionally graded cemented carbonitrides (FGCC)

    International Nuclear Information System (INIS)

    Chen, L.; Lengauer, W.; Ettmayer, P.; Dreyer, K.; Daub, H.W.; Kassel, D.

    2001-01-01

    Metallurgical reactions and microstructure developments during sintering of modern cermets and functionally graded cemented carbonitrides (FGCC) were investigated by modern thermal and analytical methods such as mass spectrometer (MS), differential thermal analysis (DTA), differential scanning calorimeter (DSC), dilatometer (DIL), microscopy and analytical electronic microscopy with energy dispersive spectrometer (EDS). The complex phase reactions and phase equilibrium in the multi-component system Ti/Mo/W/Ta/Nb/C,N-Co/Ni were studied. The melting behaviors in the systems of TiC-WC/MoC-Ni/Co, TiC-TiN-WC-Co and TiCN-TaC-WC-Co have been established. By better understanding of the mechanisms that govern the sintering processing and metallurgical reactions, new cermets and different types of functionally graded cemented carbonitrides (FGCC) with desired microstructures and properties were developed and fabricated. (author)

  11. Tribological studies of nitrogen ion implantation induced overlayer coatings of amorphous carbon and carbonitride phase

    International Nuclear Information System (INIS)

    Kumar, N.; Srivastava, S.K.; Pandian, R.; Bahuguna, Ashok; Dhara, S.; Nair, K.G.M.; Dash, S.; Tyagi, A.K.

    2013-01-01

    Highlights: ► Composite phase of amorphous carbon and carbonitride phase is observed on the N + ion implanted surface of steel. ► Advanced properties of implanted surface shows low friction coefficient of ∼0.05. ► High wear resistance 4.3 × 10 −8 mm 3 /Nm of N + implanted surface is obtained. -- Abstract: Morphology and microstructure of N + ion implanted 316 LN steel are found to modify with irradiated substrate temperature. At low temperature of 100 °C, self-similar micro-ripples are formed but at high temperature of 200 and 300 °C, micro-pores and blisters are observed on the implanted surface. Chemically modified surface is found to consist of amorphous carbon and carbonitride phase. Such composite characteristic of implanted steel surface at irradiated substrate temperature of 300 °C shows improved tribological properties with low friction coefficient and high wear resistance

  12. 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.

  13. Anti-corrosion layer prepared by plasma electrolytic carbonitriding on pure aluminum

    International Nuclear Information System (INIS)

    Wu, Jie; Zhang, Yifan; Liu, Run; Wang, Bin; Hua, Ming; Xue, Wenbin

    2015-01-01

    Highlights: • PEC/N can be applied to low melting point metal. • The spectroscopic characterization of plasma discharge is investigated. • Electron concentration and electron temperature are evaluated for PEC/N. • Phase composition of the carbonitrided layer is determined. • PEC/N improves the corrosion resistance of aluminum greatly. - Abstract: In this paper, plasma electrolytic carbonitriding (PEC/N) method was applied to pure aluminum for the first time. The spectroscopic characterization of plasma discharge during PEC/N process was analyzed and the electron temperature was calculated in terms of optical emission spectroscopy. The results showed the discharge plasma was in local thermal equilibrium (LTE) state. Electron concentration and electron temperature were about 6 × 10 21 m −3 and 4000 K, respectively. The carbonitrided layer contained Al 4 C 3 , AlN and Al 7 C 3 N 3 phases. After PEC/N treatment, the corrosion resistance of pure aluminum was significantly improved, which was related to the formation of nitride phases. This work expands the application of plasma electrolysis technology on the surface modification of low melting point metal

  14. Anti-corrosion layer prepared by plasma electrolytic carbonitriding on pure aluminum

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Jie; Zhang, Yifan; Liu, Run; Wang, Bin; Hua, Ming [Key Laboratory for Beam Technology and Materials Modification of Ministry of Education, College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China); Xue, Wenbin, E-mail: xuewb@bnu.edu.cn [Key Laboratory for Beam Technology and Materials Modification of Ministry of Education, College of Nuclear Science and Technology, Beijing Normal University, Beijing 100875 (China); Beijing Radiation Center, Beijing 100875 (China)

    2015-08-30

    Highlights: • PEC/N can be applied to low melting point metal. • The spectroscopic characterization of plasma discharge is investigated. • Electron concentration and electron temperature are evaluated for PEC/N. • Phase composition of the carbonitrided layer is determined. • PEC/N improves the corrosion resistance of aluminum greatly. - Abstract: In this paper, plasma electrolytic carbonitriding (PEC/N) method was applied to pure aluminum for the first time. The spectroscopic characterization of plasma discharge during PEC/N process was analyzed and the electron temperature was calculated in terms of optical emission spectroscopy. The results showed the discharge plasma was in local thermal equilibrium (LTE) state. Electron concentration and electron temperature were about 6 × 10{sup 21} m{sup −3} and 4000 K, respectively. The carbonitrided layer contained Al{sub 4}C{sub 3}, AlN and Al{sub 7}C{sub 3}N{sub 3} phases. After PEC/N treatment, the corrosion resistance of pure aluminum was significantly improved, which was related to the formation of nitride phases. This work expands the application of plasma electrolysis technology on the surface modification of low melting point metal.

  15. 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.

  16. 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

  17. 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)

  18. 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

  19. 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

  20. 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)

  1. 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

  2. Mean-square displacement of atomic complex in titanium carbonitrides TiCxNy

    International Nuclear Information System (INIS)

    Khidirov, I.; Sultanova, S.Kh.; Mukhtarova, N.N.; Tokhtashev, B.

    2004-01-01

    Full text: The atomic mean-square displacement (MSD) is one of important characteristics of solids, and one can use it for determination of a number of other characteristics of substances. In this work the MSD of atomic complex were determined for a number of compositions of the cubic titanium carbonitrides TiC x N y using the neutron powder diffraction data. The error of MSD determination was less than 3 %. When determining intensity of diffraction maximum a correction for the thermal diffusion dispersion (TDD) was included in the neutron diffraction patterns. The contribution of TDD in the intensity of diffraction maxima was found to be less than the experiment error (no more than 1,5 %). Such small value of the TDD correction is explained by refractory of materials. The values of MSD in titanium carbonitrides for a number of compositions, determined by the neutron powder diffraction measurements, are given. It is shown, that the dependence of MSD on the concentration (C+N)/Ti has a complex character. With decrease of the total content of metalloids MSD decreases at first, reaching a minimum about concentration (C+N)/Ti≅0.80, and then increases. MSD consists of dynamic and static distortions, where the static distortions in the compounds with variable composition increase with increasing of deviation from stoichiometry. The above anomaly in the dependence of MSD on the total concentration of metalloids, apparently, point to prevalence of dynamic distortions over static ones and to complex character of concentration dependence of interatomic interactions in the titanium carbonitrides. This work was supported by the Supporting Fund for Fundamental Researches of Uzbekistan Academy of Sciences (Grant No. 6-04)

  3. Peculiarities of Production of Chromium Carbonitride Nanopowder and Its Physical-Chemical Certification

    International Nuclear Information System (INIS)

    Shiryaeva, L S; Nozdrin, I V; Galevsky, G V

    2015-01-01

    Scientific and technological basics of plasma synthesis of chromium carbonitride have been developed, including analysis of the current production state and application of chromium carbon compounds, defining characteristics of three-jet plasma reactor, modeling- mathematical study of interaction of raw materials and plasma streams, prediction of technological parameters of plasma stream based on the modeling results, selection of optimal technological option, implementation of plasma-metallurgical technology of chromium nitride production, its physical-chemical certification and defining technical-economical production factors. (paper)

  4. Superconductive transition metal carbonitride fibers and method for the preparation thereof

    International Nuclear Information System (INIS)

    Economy, J.; Mason, J.H.; Smith, W.D.

    1976-01-01

    Fine diameter continuous multifilament superconductor yarns comprising niobium carbonitride may be prepared. The fibers of which the yarn is composed possess a very high transition temperature (T/sub c/ of 17 0 K) combined with a good upper critical field (H/sub c2/ of 125 kG) and critical current density (J/sub c/ of 10 5 amps/cm 2 at 40 kG). This invention provides excellent superconductor materials in the form of continuous fine diameter multifilament yarn. 9 claims

  5. 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.

  6. 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

  7. Quantitative mass spectrometry of decarburization and denitridation of cemented carbonitrides during sintering

    International Nuclear Information System (INIS)

    Garcia, J.; Lengauer, W.

    2001-01-01

    Quantitative quadrupole mass spectrometry of (Ti,W)C-based cemented carbonitrides was carried out in order to monitor the evolution of the gas species as a function of time and temperature during vacuum sintering. Solid standards and gas mixtures as well as precise flow control were employed for calibration. Upon integration of the outgassing rates the carbon and nitrogen evolutions and mass losses during sintering of raw hardmetal powder mixtures (WC, TiC, ...) and cemented carbonitrides could be quantified. Outgassing occurs in the range of temperatures 490-1480 o C. Nitrogen outgassing of (Ti,W)(C,N) was greater than that of Ti(C,N) due to the presence of W which increases the nitrogen activity in the solid causing a higher nitrogen equilibrium pressure. TiN showed a CO (0.2 wt %) and N 2 (0.5 wt %) weight loss only in the presence of the binder phase. For powder mixtures, it was observed that the amount of CO, CO 2 and N 2 liberated during vacuum sintering increased with the addition of cobalt in comparison with the same powders without binder phase. Nitrogen containing cermet alloys showed a greater loss of carbon than (Ti,W)C-based hardmetals. (author)

  8. Application of desirability function for optimizing the performance characteristics of carbonitrided bushes

    Directory of Open Access Journals (Sweden)

    Boby John

    2013-06-01

    Full Text Available The performance of a product is generally characterized by more than one response variable. Hence the management often faces the problem of simultaneous optimization of many response variables. This study was undertaken to simultaneously optimize the surface hardness and case depth of carbonitrided bushes. Even though lots of literature has been published on various methodologies for tackling the multi-response optimization problem, the simultaneous optimization of heat treated properties of carbonitrided bushes are not reported yet. In this research the effect of four factors and two interactions on surface hardness and case depth of carbontirded bushes were studied using design of experiments. Based on the experimental results, the expected values of the heat treated properties of the bushes were estimated for all possible combination of factors. Then the best combination which, simultaneously optimized the response variables, was arrived at using desirability function. The study showed that the optimum combination obtained through desirability function approach not only minimized the variation around the targets of surface hardness and case depth but also was superior to the ones obtained by optimizing the response variables separately. Moreover this study provides a useful and effective approach to design the production process to manufacture bushes with customer specified surface hardness and case depth targets.

  9. 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

  10. 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)

  11. 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

  12. 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

  13. 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

  14. 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

  15. 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.

  16. 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

    The effects of crystal textures and the potentials in the anodic oxidation of zirconium in a boiling nitric acid solution were investigated to study the stress corrosion cracking of zirconium in nitric acid solutions. The test specimen was machined such that the specimen surface was parallel to the rolling surface, arranged with a (0002) crystal texture. The potentials applied for the anodic oxidation of zirconium were set at 1.2, 1.4, and 1.5 V against a saturated KCl–Ag/AgCl electrode (SSE) in boiling 6 M HNO_3. The growth of the zirconium oxide film dramatically changed depending on the applied potential at a closed depassivation potential (1.47 V vs. SSE in this study). At 1.5 V, the zirconium oxide film rapidly grows, and its growth exhibits cyclic oxidation kinetics in accordance with a nearly cubic rate law. The zirconium oxide film grows according to the quantity of electric charge and the growth rate does not depend on the crystal texture in the pretransition region before the cyclic oxidation kinetics. However, the growth and cracking under the thick oxide film depend on the crystal texture in the transition region. On the normal direction side, the oxide film thickness decreases on average since some areas of the thick oxide film are separated from the specimen surface owing to the cracks in the thick oxide. On the rolling direction (RD) side, no cracks in the thick oxide film are observed, but cracks are found under the thick oxide film, which deeply propagate in metal matrix along the RD without an external stress. The cracks under the thick oxide film propagate to the center of the oxide layer. The crystal orientation relationship between the oxide layer and the zirconium matrix is (0002)_Z_r//(111)_Z_r_O_2, and the cracks in the oxide layer propagate in the (0002)_Z_r plane in the zirconium matrix. The oxide layer consists of string-like zirconium oxide and zirconium hydride. The string-like zirconium oxide contains orthorhombic ZrO_2 in addition

  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. 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/ .

  19. Large-scale aligned silicon carbonitride nanotube arrays: Synthesis, characterization, and field emission property

    International Nuclear Information System (INIS)

    Liao, L.; Xu, Z.; Liu, K. H.; Wang, W. L.; Liu, S.; Bai, X. D.; Wang, E. G.; Li, J. C.; Liu, C.

    2007-01-01

    Large-scale aligned silicon carbonitride (SiCN) nanotube arrays have been synthesized by microwave-plasma-assisted chemical vapor deposition using SiH 4 , CH 4 , and N 2 as precursors. The three elements of Si, C, and N are chemically bonded with each other and the nanotube composition can be adjusted by varying the SiH 4 concentration, as revealed by electron energy loss spectroscopy and x-ray photoelectron spectroscopy. The evolution of microstructure of the SiCN nanotubes with different Si concentrations was characterized by high-resolution transmission electron microscopy and Raman spectroscopy. The dependence of field emission characteristics of the SiCN nanotubes on the composition has been investigated. With the increasing Si concentration, the SiCN nanotube exhibits more favorable oxidation resistance, which suggests that SiCN nanotube is a promising candidate as stable field emitter

  20. Thermal behaviour of nitrogen implanted into zirconium

    International Nuclear Information System (INIS)

    Miyagawa, S.; Ikeyama, M.; Saitoh, K.; Nakao, S.; Niwa, H.; Tanemura, S.; Miyagawa, Y.

    1994-01-01

    Zirconium films were implanted with 15 N ions of energy 50keV to a total fluence of 1x10 18 ionscm -2 in an attempt to study the formation process and thermal stability of ZrN layers produced by high fluence implantation of nitrogen. Subsequent to the implantation at room temperature, samples were annealed at temperatures of 300 C-900 C. The depth profiles of the implanted nitrogen were measured by nuclear reaction analysis using the 15 N(p,αγ) 12 C at E R =429keV, and the surfaces were examined by thin film X-ray diffraction (XRD) and scanning electron microscopy. There were many blisters 0.2-0.4μm in diameter on the surface of the as-implanted samples and double peaks were observed in the nitrogen depth profiles; they were in both sides of the mean projected range. It was found that most of the blisters became extinct after annealing above 400 C, and the XRD peak (111) intensity was increased with the increase in the annealing temperature. Moreover, 14 N and 15 N implantations were superimposed on Zr samples in order to study the atomic migration of nitrogen at each stage of high fluence implantation. It was found that the decrease in the peak at the deeper layers was related to blister extinction and nitrogen diffusion into underling zirconium which could be correlated with radiation damage induced by post-implanted ions. ((orig.))

  1. 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.

  2. 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

  3. 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

  4. Effects of working gas pressure on zirconium dioxide thin film prepared by pulsed plasma deposition: roughness, wettability, friction and wear characteristics.

    Science.gov (United States)

    Berni, M; Marchiori, G; Gambardella, A; Boi, M; Bianchi, M; Russo, A; Visani, A; Marcacci, M; Pavan, P G; Lopomo, N F

    2017-08-01

    In joint arthroplasty one of the main issues related to the failure of prosthetic implants is due to the wear of the ultra-high molecular weight polyethylene (UHMWPE) component. Surface treatments and coatings have been recognized as enhancing methods, able to improve the tribological properties of the implants. Therefore, the main objective of this work was to investigate the possibility to fabricate yttria-stabilized zirconia (YSZ) coatings on a metal (AISI 316-L) substrate by means of Pulsed Electron Deposition, in order to improve the tribological behavior of the polymer-metal coupling, by reducing the initial wear of the UHMWPE component. In order to optimize the coating characteristics, the effects of working gas pressure on both its morphological and tribological properties were analyzed. Morphological characterization of the films was evaluated by Atomic Force Microscopy (AFM). Coating wettability was also estimated by contact angle (CA) measurement. Tribological performance (coupling friction and wear of UHMWPE) was evaluated by using a ball-on-disc tribometer during highly-stressing tests in dry and lubricated (i.e. NaCl and serum) conditions; friction and wear were specifically evaluated at the initial sliding distances - to highlight the main effect of coating morphology - and after 100m - where the influence of the intrinsic materials properties prevails. AFM analysis highlighted that the working pressure heavily affected the morphological characteristics of the realized films. The wettability of the coating at the highest and lowest deposition pressures (CA ~ 60°, closed to substrate value) decreased for intermediate pressures, reaching a maximum CA of ~ 90°. Regarding tribological tests, a strong correlation was found in the initial steps between friction coefficient and wettability, which decreased as the distance increased. Concerning UHMWPE wear associated to coated counterpart, at 100m a reduction rate of about 7% in dry, 12% in NaCl and 5% in

  5. 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)

  6. Electrochemical stripping determination of traces of copper, lead, cadmium and zinc in zirconium metal and zirconium dioxide

    International Nuclear Information System (INIS)

    Stulik, K.; Beran, P.; Dolezal, J.; Opekar, F.

    1978-01-01

    Procedures have been developed for the determination of copper, lead, cadmium and zinc in zirconium metal and zirconium dioxide, at concentrations of 1ppm or less. Zirconium metal was dissolved in sulphuric acid, and zirconium dioxide decomposed under pressure with hydrofluoric acid. Sample solutions were prepared in dilute sulphuric acid. For the stripping determination, the sample solution was either mixed with a complexing tartrate base electrolyte or the pre-electrolysis was carried out in acid solution, with the acid solution being exchanged for a pure base electrolyte (e.g. an acetate buffer) for the stripping step. The stripping step was monitored by d.c., differential pulse and Kalousek commutator voltammetry and the three methods were compared. A stationary mercury-drop electrode can generally be used for all the methods, whereas a mercury-film electrode is suitable only for the d.c. voltammetric determination of copper, lead and cadmium, as pulse measurements with films are poorly reproducible and the electrodes are easily damaged. The relative standard deviation does not exceed 20%. Some samples contained relatively large amounts of copper, which is best separated by electrodeposition on a platinum electrode. (author)

  7. Possibilities of application of perfect solution model to calculation of equilibrium composition of complex carbonitrides and their solubility in steels

    International Nuclear Information System (INIS)

    Gol'dshtejn, M.I.; Popov, V.V.; Cheremnykh, V.G.

    1980-01-01

    Using the Fe-Nb-V-C-N and Fe-Ti-V-C-N systems' low carbon steels, the earlier suggested model of perfect solid solutions has been experimentally researched. Also studied has been the feasibility to calculate the composition of carbonitrides in steels by the derived equations, that comprise, as parameters, products of respective compounds' solubility and coefficients of components interaction in iron-based solid solutions. A conclusion is drawn that perfect solutions models may be used adequately for complex carbonitrides like Nbsub(p)Vsub(1-p)Csub(q)Nsub(1-q) and Tisub(p)Vsub(1-p)Csub(q)Nsub(1-q) during the calculations of their equilibrium composition and solubility in steels

  8. 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.

  9. Method to electrolytically precipitate metals onto zirconium objects

    International Nuclear Information System (INIS)

    Donaghy, R.E.

    1978-01-01

    Tubes and other formed bodies made of zirconium or zirconium alloys which serve to take up nuclear fuels, are plated by electrolytically depositing a metal film onto these in order to improve their mechanical and corrosion properties. The object is activated in a solution of ammonium bifluoride and sulphuric acid, whereby an electrically conducting solid and a loose layer is formed. This loose film is removed by using fluoboric acid or hydrofluoric silicic acid solution, ultrasonics, or strips of organic material (cotton, polyester, nylon). The plating of Cu, Ni, Cr is described in detail. The object is rinsed between the process steps with deionized water and finally degased at a temperature of 150-200 0 C. (IHOE) [de

  10. 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

  11. 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

  12. Nanostructured thin film coatings with different strengthening effects

    Directory of Open Access Journals (Sweden)

    Panfilov Yury

    2017-01-01

    Full Text Available A number of articles on strengthening thin film coatings were analyzed and a lot of unusual strengthening effects, such as super high hardness and plasticity simultaneously, ultra low friction coefficient, high wear-resistance, curve rigidity increasing of drills with small diameter, associated with process formation of nanostructured coatings by the different thin film deposition methods were detected. Vacuum coater with RF magnetron sputtering system and ion-beam source and arc evaporator for nanostructured thin film coating manufacture are represented. Diamond Like Carbon and MoS2 thin film coatings, Ti, Al, Nb, Cr, nitride, carbide, and carbo-nitride thin film materials are described as strengthening coatings.

  13. 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)

  14. Shot-peening of carbonitrided steel: influence of the process on the mechanical state

    Directory of Open Access Journals (Sweden)

    François M.

    2010-06-01

    Full Text Available Residual stresses have a significant role in affecting engineering properties of materials and shot peening process is an effective production technique to ensure required residual stress levels. This paper presents an analysis of an orthogonal design of experiment to establish an empirical relationship between main parameters of shot peening process and residual stress profiles for a carbonitrided steel. The hardening / softening evolution of the material is followed using hardness and diffraction peak width. Four critical peening parameters, i.e. shot size, incident angle, exposure time, airblast pressure, have been chosen and the range of peening conditions are established by using the Taguchi technique. In this study, a shot velocity measurement system is used to obtain the on-line velocity during the peening process and the relationship between the maximum compressive residual stresses and the shot velocity is also developed. Analysis of the experimental data showed that it is possible to optimize the shot peening process by an effective control of process parameters.

  15. Evaluation of activities of carbons in chemical equilibrium with uranium carbonitride

    International Nuclear Information System (INIS)

    Katsura, Masahiro; Hirota, Masayuki; Miyake, Masanobu; Hamada, Kazuo.

    1992-01-01

    A mixture of uranium sesquinitride and carbon was prepared by the reaction of UC of UC 2 with N 2 in the temperature range from 700 to 1400degC. When the mixture of uranium sesquinitride and carbon is kept at temperatures above 1200degC in the atmosphere of N 2 at low pressure, the state where uranium carbonitride (UC 1-x N x ) and carbon are present together in chemical equilibrium will be established. A thermodynamic analysis suggests that, in the equilibrium state, the composition of UC 1-x N x is determined by the chemical activity of carbon, a c , which is related to the chemical potential of the carbon, μ c , by the equation, μ c = μ c deg + RT 1n a c . Here μ c deg refers to graphite, which is usually taken as the standard state of carbon (a c = 1). Mixtures of U 2 N 3 and carbon with several degrees of graphitization were heat-treated at 1400degC, and the composition of UC 1-x N x in the reaction product was determined. From these experimental results and the thermodynamic analysis, values of the activity of the carbon coexisting with UC 1-x N x were estimated. (author)

  16. Process for electrolytic deposition of metals on zirconium materials

    International Nuclear Information System (INIS)

    Donaghy, R.E.

    1981-01-01

    An article made of a zirconium alloy can be electrolytically plated with a layer of a metal such as copper, nickel or chromium when the article is free of any loosely adhering film formed during an activation step. The article is activated in an aged aqueous solution of ammonium bifluoride and sulfuric acid. Next the loosely adhering film formed in the first step is removed by chemical treatment, ultrasonic cleaning, or by swabbing the surface with cotton or an organic material. Finally the article is contacted with an electrolytic plating solution in the presence of an electrode receiving current

  17. 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.)

  18. 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

  19. Comparative study of the tribological behavior under hybrid lubrication of diamond-like carbon films with different adhesion interfaces

    Science.gov (United States)

    Costa, R. P. C.; Lima-Oliveira, D. A.; Marciano, F. R.; Lobo, A. O.; Corat, E. J.; Trava-Airoldi, V. J.

    2013-11-01

    This paper reports the influence of the adhesion interlayer between stainless steel and diamond-like carbon (DLC) films in two different contact conditions: in dry air and deionized water. The water was the liquid used to understand the mechanism and chemical reactions of the tribolayer formation under boundary lubrication. The effect of silicon and carbonitride adhesion interlayer was investigated on uncoated and coated DLC films. The results show that DLC/DLC pairs using carbonitride in air (30% RH) showed 60% less friction coefficient and wear less than three orders of magnitude than DLC/DLC pairs using silicon as interlayer. In deionized water, DLC/DLC pairs using carbonitride as interlayer showed 31% less friction coefficient when compared to DLC/DLC pairs with silicon. Raman related the chemical and structural changes in the DLC films during sliding in air and in the presence of water. Scratch tests showed a critical load of 14 N and 33 N in DLC films with silicon and carbonitride, respectively.

  20. 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.

  1. Precipitation Behaviour of Carbonitrides in Ti-Nb-C-N Microalloyed Steels and an Engineering Application with Homogenously Precipitated Nano-particles

    Directory of Open Access Journals (Sweden)

    Yanlin WANG

    2015-11-01

    Full Text Available A thermodynamic model enabling calculation of equilibrium carbonitride composition and relative amounts as a function of steel composition and temperature has been developed previously based on the chemical equilibrium method. In the present work, actual carbonitride precipitation behaviour has been verified in the Ti-Nb-C-N microalloyed steels. The Ti microalloyed steel after refining with 0.012 % Nb exhibited highly improved tensile strength without sacrificing ductility. According to further detailed SEM and TEM analysis, the improved mechanical properties of Ti/Nb microalloyed steel could be attributed to the larger solubility of Nb and Ti, inducing fine dispersion of the carbonitrides with particle size of 2 – 10 nm in the ferrite matrix.DOI: http://dx.doi.org/10.5755/j01.ms.21.4.9622

  2. 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)

  3. 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

  4. 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...

  5. 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)

  6. 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)

  7. 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

  8. Determination of zirconium

    International Nuclear Information System (INIS)

    Iha, C.; Sood, S.P.; Sato, I.M.

    1985-01-01

    The analysis of Zr and Hf by X-ray fluorescence was studied. The thin film technique for sample preparation by deposition of precipitate on the filter paper was used. The K sub(α) line of Zr and L sub(β) 1 line of Hf were considered for the analysis. The behaviour of fluorescence intensity ratio with the corresponding mass ratio was also studied. The direct determination of Hf in concentrations between 2 and 95% in samples without any separation was investigated. For Hf concentrations lower than 2%, a method for its enrichment was standardized. (Author) [pt

  9. 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)

  10. 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)

  11. 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

  12. 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

  13. Protection of zirconium and its alloys by metallic coatings

    International Nuclear Information System (INIS)

    Loriers, H.; Lafon, A.; Darras, R.; Baque, P.

    1968-01-01

    At 600 deg. C in an atmosphere of carbon dioxide, zirconium and its alloys undergo corrosion which presents two aspects simultaneously: - formation of a surface layer of zirconia, - dissolution of oxygen in the alloy sub-layer leading to brittleness. The two phenomena greatly restrict the possibilities of using zirconium alloys as a canning material for fuel elements in CO 2 cooled nuclear reactors. An attempt has thus been made to limit, and perhaps to suppress, the corrosion effects in zirconium under these conditions by protecting it with metallic coatings. A first attempt to obtain a protection using copper-based coatings did not produce the result hoped for. Aluminium coatings produced by vacuum evaporation, followed by a consolidating thermal treatment make it possible to prevent the formation of the zirconia layer, but they do not eliminate the hardening effect produced by oxygen diffusion. On the other hand, electrolytically produced chromium deposits whose adherence is improved by a thermal vacuum treatment, counteract both these phenomena simultaneously. A similar result has been obtained with coatings of molybdenum produced by the technique of high-frequency inductive plasma sputtering. The particular effectiveness of the last two types of coatings is due to their structures characterized by the existence of an adherent film of chromium or molybdenum in the free state. (authors) [fr

  14. 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

  15. 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

  16. 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)

  17. 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

  18. 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)

  19. 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)

  20. 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

  1. 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

  2. Method to precipitate metals on zirconium articles without using current

    International Nuclear Information System (INIS)

    Donaghy, R.E.

    1978-01-01

    Tubes or other bodies made of zirconium or Zr alloys used for taking up nuclear fuels are coated without current with a metal film to improve the mechanical and corrosion properties. The article is activated in a solution of ammonium bifluoride and sulphuric acid where an electrical conducting fixed and loose layer are fermed. This loose film is removed chemically by reacting with fluoroboric acid or hydrofluorosilica acid by ultrasonic treatment or by stripping from organic material (cotton, polyester, nylon). The current-free plating with Cu and Ni is described. The article is washed with deionized water between the process steps and finally degassed at a temperature of 150-200 0 C. (IHOE) [de

  3. 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)

  4. 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.

  5. 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

  6. 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

  7. Methods for and products of processing nanostructure nitride, carbonitride and oxycarbonitride electrode power materials by utilizing sol gel technology for supercapacitor applications

    Science.gov (United States)

    Huang, Yuhong; Wei, Oiang; Chu, Chung-tse; Zheng, Haixing

    2001-01-01

    Metal nitride, carbonitride, and oxycarbonitride powder with high surface area (up to 150 m.sup.2 /g) is prepared by using sol-gel process. The metal organic precursor, alkoxides or amides, is synthesized firstly. The metal organic precursor is modified by using unhydrolyzable organic ligands or templates. A wet gel is formed then by hydrolysis and condensation process. The solvent in the wet gel is then be removed supercritically to form porous amorphous hydroxide. This porous hydroxide materials is sintered to 725.degree. C. under the ammonia flow and porous nitride powder is formed. The other way to obtain high surface area nitride, carbonitride, and oxycarbonitride powder is to pyrolyze polymerized templated metal amides aerogel in an inert atmosphere. The electrochemical capacitors are prepared by using sol-gel prepared nitride, carbonitride, and oxycarbonitride powder. Two methods are used to assemble the capacitors. Electrode is formed either by pressing the mixture of nitride powder and binder to a foil, or by depositing electrode coating onto metal current collector. The binder or coating is converted into a continuous network of electrode material after thermal treatment to provide enhanced energy and power density. Liquid electrolyte is soaked into porous electrode. The electrochemical capacitor assembly further has a porous separator layer between two electrodes/electrolyte and forming a unit cell.

  8. 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.

  9. 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.

  10. 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)

  11. 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)

  12. 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.

  13. 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)

  14. 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

  15. 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.)

  16. The Influence of Zirconium Acrylate on Curable Palm Oil Resin as Coating Material by Using UV Technique

    International Nuclear Information System (INIS)

    Mohd Sofian Alias; Nik Ghazali Nik Salleh; Mek Zah Salleh; Mohd Hamzah Harun; Rida Tajau; Khairul Azhar Abdul Halim; Nurul Huda Mudri

    2016-01-01

    Epoxidized Palm oil liquid acrylate (EPOLA) was introduced with commercial monomer and oligomer to produce coating film by using radiation technique. The percentage of EPOLA in curable formulation has varied in order to study the influence of EPOLA on coating film properties. Meanwhile Zirconium Acrylate was added and varied as additive into curable formulation to investigate the influence on film coating. FTIR analysis was used to monitor the crosslinking process by observed the disappearance of acrylate group. The performance of coating film were investigated by doing several mechanical analysis such as pencil hardness and adhesion test. Meanwhile, in order to determine gloss properties for cured film at different dose of radiation, gloss meter was used to measure gloss value. According to mechanical analysis result, an increasing of EPOLA compound in coating formulation will reduce film hardness and adhesion properties. However after additional of zirconium acrylate into resin formulation the properties of coating film were improved due to presence of zirconium in crosslinking network (author)

  17. 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

  18. Effects of rapid thermal annealing on structural, chemical, and electrical characteristics of atomic-layer deposited lanthanum doped zirconium dioxide thin film on 4H-SiC substrate

    International Nuclear Information System (INIS)

    Lim, Way Foong; Quah, Hock Jin; Lu, Qifeng; Mu, Yifei; Ismail, Wan Azli Wan; Rahim, Bazura Abdul; Esa, Siti Rahmah; Kee, Yeh Yee; Zhao, Ce Zhou

    2016-01-01

    Graphical abstract: - Highlights: • Studies of RTA temperatures on La doped ZrO2 atomic layer deposited on 4HSiC. • Oxygen vacancies improved insulating and catalytic properties of La doped ZrO2. • 700 °C annealed sample showed the highest EB, k value, and sensitivity on O2. • La doped ZrO2 was proposed as a potential metal reactive oxide on 4H-SiC. - Abstract: Effects of rapid thermal annealing at different temperatures (700–900 °C) on structural, chemical, and electrical characteristics of lanthanum (La) doped zirconium oxide (ZrO_2) atomic layer deposited on 4H-SiC substrates have been investigated. Chemical composition depth profiling analysis using X-ray photoelectron spectroscopy (XPS) and cross-sectional studies using high resolution transmission electron microscopy equipped with energy dispersive X-ray spectroscopy line scan analysis were insufficient to justify the presence of La in the investigated samples. The minute amount of La present in the bulk oxide was confirmed by chemical depth profiles of time-of-flight secondary ion mass spectrometry. The presence of La in the ZrO_2 lattice led to the formation of oxygen vacancies, which was revealed through binding energy shift for XPS O 1s core level spectra of Zr−O. The highest amount of oxygen vacancies in the sample annealed at 700 °C has yielded the acquisition of the highest electric breakdown field (∼ 6.3 MV/cm) and dielectric constant value (k = 23) as well as the highest current–time (I–t) sensor response towards oxygen gas. The attainment of both the insulating and catalytic properties in the La doped ZrO_2 signified the potential of the doped ZrO_2 as a metal reactive oxide on 4H-SiC substrate.

  19. 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.

  20. 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.

  1. 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.

  2. Components made of corrosion-resistent zirconium alloy and method for its production

    International Nuclear Information System (INIS)

    Hanneman, R.E.; Urquhart, A.W.; Vermilyea, D.A.

    1977-01-01

    The invention deals with a method to increase the resistance of zirconium alloys to blister corrosion which mainly occurs in boiling-water nuclear reactors. According to the method described, the surface of the alloy body is coated with a thin film of a suitable electronically conducting material. Gold, silver, platinum, nickel, chromium, iron and niobium are suitable as coating materials. The invention is more closely explained by means of examples. (GSC) [de

  3. 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).

  4. 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

    oxide film matrix which develops at high temperatures. Cold spray and thermal spray deposition of ZrSi2 have been performed by systematically varying deposition parameters. While deposition of coating was achieved, further process optimization is required to improve coating quality deposited using these methods. An optimal zirconium-silicide slurry coating for mechanical properties and corrosion resistance/oxide protection was developed based on a theoretical characterization. The slurry coating was investigated using a range of similar compositional coatings to accurately characterize the best coating with respect its mechanical integrity and environmental protection for zirconium alloy substrates. Distinctive oxide layers of ZrSi2 prepared at 1000°C and 1400°C in ambient air were subjected to a 3.9 MeV Si2+ ions irradiation at 305°C and their radiation responses were characterized and analyzed. Nanocomposite oxides consisting of ZrO2 nanocrystals embedded in amorphous SiO2 matrix formed on ZrSi2 surface after oxidation at 1000°C. Radiation-induced phase mixing of the oxide phases and amorphization of ZrO2 was observed up to ~ 820 nm in depth, about one-third of the total radiation damaged region (2.5 µm in thickness) as estimated by SRIM calculation. Polygonal crystalline ZrSiO4 grains in dual-layered oxide scale on ZrSi2 at 1400°C were completely amorphized under the ion-irradiation. Given the high corrosion resistance of ZrSiO4 and immobilization of Si in aqueous environments conclusively demonstrated in this study, it is anticipated that the irradiated oxide scale would have a superior corrosion resistance compared to unirradiated surface. The results can be applied to not only baseline data for radiation response of the potential neutron deflector in advanced reactors but also development of nanocomposite structural materials in future spacecraft, sensors, detector subjected to high radiation dose. A quench test facility was designed and built to study

  5. 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.

  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. Amorphous and nanocrystalline titanium nitride and carbonitride materials obtained by solution phase ammonolysis of Ti(NMe2)4

    International Nuclear Information System (INIS)

    Jackson, Andrew W.; Shebanova, Olga; Hector, Andrew L.; McMillan, Paul F.

    2006-01-01

    Solution phase reactions between tetrakisdimethylamidotitanium (Ti(NMe 2 ) 4 ) and ammonia yield precipitates with composition TiC 0.5 N 1.1 H 2.3 . Thermogravimetric analysis (TGA) indicates that decomposition of these precursor materials proceeds in two steps to yield rocksalt-structured TiN or Ti(C,N), depending upon the gas atmosphere. Heating to above 700 deg. C in NH 3 yields nearly stoichiometric TiN. However, heating in N 2 atmosphere leads to isostructural carbonitrides, approximately TiC 0.2 N 0.8 in composition. The particle sizes of these materials range between 4-12 nm. Heating to a temperature that corresponds to the intermediate plateau in the TGA curve (450 deg. C) results in a black powder that is X-ray amorphous and is electrically conducting. The bulk chemical composition of this material is found to be TiC 0.22 N 1.01 H 0.07 , or Ti 3 (C 0.17 N 0.78 H 0.05 ) 3.96 , close to Ti 3 (C,N) 4 . Previous workers have suggested that the intermediate compound was an amorphous form of Ti 3 N 4 . TEM investigation of the material indicates the presence of nanocrystalline regions x (C,N) y crystalline phases

  8. Plasma synthesis of titanium nitride, carbide and carbonitride nanoparticles by means of reactive anodic arc evaporation from solid titanium

    International Nuclear Information System (INIS)

    Kiesler, D.; Bastuck, T.; Theissmann, R.; Kruis, F. E.

    2015-01-01

    Plasma methods using the direct evaporation of a transition metal are well suited for the cost-efficient production of ceramic nanoparticles. In this paper, we report on the development of a simple setup for the production of titanium-ceramics by reactive anodic arc evaporation and the characterization of the aerosol as well as the nanopowder. It is the first report on TiC X N 1 − X synthesis in a simple anodic arc plasma. By means of extensive variations of the gas composition, it is shown that the composition of the particles can be tuned from titanium nitride over a titanium carbonitride phase (TiC X N 1 − X ) to titanium carbide as proven by XRD data. The composition of the plasma gas especially a very low concentration of hydrocarbons around 0.2 % of the total plasma gas is crucial to tune the composition and to avoid the formation of free carbon. Examination of the particles by HR-TEM shows that the material consists mostly of cubic single crystalline particles with mean sizes between 8 and 27 nm

  9. The evolution of primary and secondary niobium carbonitrides in AISI 347 stainless steel during manufacturing and long-term ageing

    Energy Technology Data Exchange (ETDEWEB)

    Erneman, J. [Department of Applied Physics, Chalmers University of Technology, SE-41296 Goeteborg (Sweden); Schwind, M. [Outokumpu Stainless AB, PB 74, SE-774 22 Avesta (Sweden); Andren, H.-O. [Department of Applied Physics, Chalmers University of Technology, SE-41296 Goeteborg (Sweden); Nilsson, J.-O. [AB Sandvik Materials Technology, R and D Centre, SE-81181 Sandviken (Sweden)]. E-mail: jan-olof.nilsson@sandvik.com; Wilson, A. [AB Sandvik Materials Technology, R and D Centre, SE-81181 Sandviken (Sweden); Agren, J. [Department of Materials Science and Engineering, Royal Institute of Technology, SE-10044 Stockholm (Sweden)

    2006-01-15

    Nb(C,N) precipitates were studied in a niobium-stabilised stainless steel (AISI 347) statically aged at 700 {sup o}C. Scanning electron microscopy and energy filtered transmission electron microscopy were used to determine the volume fraction and precipitate size of primary and secondary Nb(C,N) after ageing times between 0 and 70,000 h. The experimental data were correlated with simulations of Nb(C,N) formation based on the assumption that the process is controlled by diffusion. These simulations provide a rationale for the existence of two sets of niobium carbonitrides in commercial tubes of AISI 347. Growth of primary Nb(C,N) occurred essentially during manufacturing, with no significant growth at 700 {sup o}C. Rapid dissolution and re-precipitation of secondary Nb(C,N) occurred during manufacturing. Coarsening at 700 {sup o}C of secondary particles was modelled using the Lifshitz-Slyozov-Wagner theory, which overestimated the coarsening rate. These problems were overcome with a model developed by the authors. This model takes both growth and coarsening into account.

  10. The evolution of primary and secondary niobium carbonitrides in AISI 347 stainless steel during manufacturing and long-term ageing

    International Nuclear Information System (INIS)

    Erneman, J.; Schwind, M.; Andren, H.-O.; Nilsson, J.-O.; Wilson, A.; Agren, J.

    2006-01-01

    Nb(C,N) precipitates were studied in a niobium-stabilised stainless steel (AISI 347) statically aged at 700 o C. Scanning electron microscopy and energy filtered transmission electron microscopy were used to determine the volume fraction and precipitate size of primary and secondary Nb(C,N) after ageing times between 0 and 70,000 h. The experimental data were correlated with simulations of Nb(C,N) formation based on the assumption that the process is controlled by diffusion. These simulations provide a rationale for the existence of two sets of niobium carbonitrides in commercial tubes of AISI 347. Growth of primary Nb(C,N) occurred essentially during manufacturing, with no significant growth at 700 o C. Rapid dissolution and re-precipitation of secondary Nb(C,N) occurred during manufacturing. Coarsening at 700 o C of secondary particles was modelled using the Lifshitz-Slyozov-Wagner theory, which overestimated the coarsening rate. These problems were overcome with a model developed by the authors. This model takes both growth and coarsening into account

  11. 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.

  12. 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...

  13. 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.

  14. 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

  15. 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

  16. 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

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. 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...

  2. 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

  3. 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

  4. 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

  5. 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

  6. 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

  7. 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.

  8. Microstructural modelling and lubrication study during zirconium alloy hot extrusion

    International Nuclear Information System (INIS)

    Gaudout, B.

    2009-01-01

    Using torsion tests (with strain rate jumps) and an experimental hot mini-extrusion apparatus, several samples zirconium alloy have been deformed: Zircaloy-4 (high α range) and Zr-1Nb (α + β domain). The fragmentation of the microstructure and post-dynamic grain growth have been examined. The main difference between these two alloys is that Zr-1Nb does not show grain growth during a heat treatment within the α + β domain after hot deformation. The recrystallization volume fraction has been measured on extruded samples with or without heat treatment. These rheological and microstructural data have been used to determine the parameters of a microstructural model including: a work-hardening model (Laaasraoui/Jonas), a continuous dynamic recrystallization model (Gourdet/Montheillet) and a grain growth model. This model leads to a good prediction of recrystallization volume fraction for Zircaloy-4 extrusion. However, the Zr-1Nb model cannot be validated because of the difficulty to observe deformed microstructures. Extrusion process is lubricated with a solid film. Trapping tests show that this lubricant is thermoviscoplastic. Friction along the container and several observations show the lubrication is not realized by a continuous film. Indeed, the heterogeneousness of deformation of these alloys causes a rupture of the lubricant film. Experiments and numerical simulations show that the radial gradient of axial displacement is affected by friction but also by stress softening of the alloys. (author)

  9. Metal-free spin and spin-gapless semiconducting heterobilayers: monolayer boron carbonitrides on hexagonal boron nitride.

    Science.gov (United States)

    Pan, Hongzhe; Zhang, Hongyu; Sun, Yuanyuan; Ding, Yingchun; Chen, Jie; Du, Youwei; Tang, Nujiang

    2017-06-07

    The interfaces between monolayer boron carbonitrides and hexagonal boron nitride (h-BN) play an important role in their practical applications. Herein, we respectively investigate the structural and electronic properties of two metal-free heterobilayers constructed by vertically stacking two-dimensional (2D) spintronic materials (B 4 CN 3 and B 3 CN 4 ) on a h-BN monolayer from the viewpoints of lattice match and lattice mismatch models using density functional calculations. It is found that both B 4 CN 3 and B 3 CN 4 monolayers can be stably adsorbed on the h-BN monolayer due to the van der Waals interactions. Intriguingly, we demonstrate that the bipolar magnetic semiconductor (BMS) behavior of the B 4 CN 3 layer and the spin gapless semiconductor (SGS) property of the B 3 CN 4 layer can be well preserved in the B 4 CN 3 /BN and B 3 CN 4 /BN heterobilayers, respectively. The magnetic moments and spintronic properties of the two systems originate mainly from the 2p z electrons of the carbon atoms in the B 4 CN 3 and B 3 CN 4 layers. Furthermore, the BMS behavior of the B 4 CN 3 /BN bilayer is very robust while the electronic property of the B 3 CN 4 /BN bilayer is sensitive to interlayer couplings. These theoretical results are helpful both in understanding the interlayer coupling between B 4 CN 3 or B 3 CN 4 and h-BN monolayers and in providing a possibility of fabricating 2D composite B 4 CN 3 /BN and B 3 CN 4 /BN metal-free spintronic materials theoretically.

  10. 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.)

  11. 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.

  12. 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

  13. 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)

  14. 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

  15. 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%

  16. Properties of carbides, nitrides and carbonitrides based on Ti and Mo multicomponent layers

    Energy Technology Data Exchange (ETDEWEB)

    Kozlowski, J.; Markowski, J.; Prajzner, A.; Zdanowski, J. [Politechnika Wroclawska (Poland). Inst. Technologii Elektronowej

    1998-01-01

    Coating have been produced by bias activated reactive evaporation method (BARE) [1] on polished HSS steel and Corning glass substrates. Titanium and molybdenum were co-evaporated using a special two-hearth electron gun with separate Ti and Mo evaporation sources. Various chemical compositions were obtained by means of heating time control of respective materials. The working gases were nitrogen, acetylene and a 1:1 mixture of both. The investigation of properties of layers with various chemical compositions covered samples: TiC, TiCN, TiN, (Ti,Mo)C, (Ti,Mo)CN, (Ti,Mo)N, MoC, MoCN, MoN. The chemical film compositions were determined using the energy-dispersive X-ray analysis (EDAX) method. Vickers hardness measurements were made. The structures of the deposited layers were examined by means of X-ray diffraction. The electrical measurements of the deposited layers covered resistivity ({rho}) and temperature coefficient of resistivity (TCR). It has been found that the measurements of electrical properties may be very sensitive indicators of the layer composition and structure. (orig.) 5 refs.

  17. 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

  18. 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)

  19. 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

  20. Linear low density polyethylene (LLDPE) and lamellar zirconium phosphate (Zr P) composites: morphology and mechanical properties

    International Nuclear Information System (INIS)

    Silva, Daniela F.; Mandes, Luis C.; Lino, Adan S.

    2011-01-01

    Composites of linear low density polyethylene (LLDPE) and zirconium phosphate (ZrP) were prepared by extrusion in the molten state, containing 2 (w%) of the lamellar filler. The filler was previously synthesized by direct precipitation method and characterized. After processing, the composite and the pure virgin polymer were molded by compression in order to obtain films of 1 mm thick which were characterized by X-ray diffraction at high angle (WAXD), stress-strain mechanical analysis and scanning electron microscopy (SEM). The WAXD and SEM analysis showed that there was no intercalation of LLDPE in zirconium phosphate, possibly due to the fact that the layers do not have spacing enough to allow the intercalation of polymer chains in the galleries of the filler and thus allow the exfoliation. (author)

  1. 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.)

  2. 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

  3. 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.)

  4. 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.

  5. 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

  6. 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)

  7. 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 ...

  8. 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.)

  9. 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

  10. 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

  11. 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

  12. 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.

  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. 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

  15. 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.

  16. 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

  17. 5A Zirconium Dioxide Ammonia Microsensor Integrated with a Readout Circuit Manufactured Using the 0.18 μm CMOS Process

    Science.gov (United States)

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

    2013-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Ming-Zhi Yang

    2013-03-01

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

  19. 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

  20. 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

  1. 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

  2. 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

  3. 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

  4. 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

  5. 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

  6. 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

  7. 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

  8. Sorption of Europium in zirconium silicate

    International Nuclear Information System (INIS)

    Garcia R, G.

    2004-01-01

    Some minerals have the property of sipping radioactive metals in solution, that it takes advantage to manufacture contention barriers that are placed in the repositories of nuclear wastes. The more recent investigations are focused in the development of new technologies guided to the sorption of alpha emissors on minerals which avoid their dispersion in the environment. In an effort to contribute to the understanding of this type of properties, some studies of sorption of Europium III are presented like homologous of the americium, on the surface of zirconium silicate (ZrSiO 4 ). In this work the results of sorption experiences are presented as well as the interpretation of the phenomena of the formation of species in the surface of the zirconium silicate. (Author)

  9. Preparation and characterization of nanocrystalline composites Mo-C-N hard films

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Q. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, POB 1129, 230031 Hefei (China); Liu, T. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, POB 1129, 230031 Hefei (China); Fang, Q.F. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, POB 1129, 230031 Hefei (China)]. E-mail: qffang@issp.ac.cn; Liang, F.J. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, POB 1129, 230031 Hefei (China); Wang, J.X. [Key Laboratory of Materials Physics, Institute of Solid State Physics, Chinese Academy of Sciences, POB 1129, 230031 Hefei (China)

    2006-05-01

    Molybdenum carbonitride (MoCN) films were deposited on Si (001) and stainless steel substrates by reactive direct-current magnetron sputtering with a molybdenum and graphite composite target. By changing the substrate temperature and the N{sub 2} / Ar ratio in the sputtering gas, it is found that good quality MoCN films can be deposited at substrate temperature of 300-400 deg. C under N{sub 2} partial pressure of 0.25-0.5 Pa with a total working pressure of 1 Pa. The structures of the films deposited at such conditions were determined by X-ray diffraction and X-ray photoelectron spectroscopy analysis as nanocrystalline molybdenum carbonitride with a grain size of several ten nanometers was embedded in the amorphous matrix of C and CN {sub x}. The hardness of the MoCN films can reach 28 GPa, much higher than the value of MoC and MoN films alone.

  10. New solvent extraction process for zirconium and hafnium

    International Nuclear Information System (INIS)

    Takahashi, M.; Katoh, Y.; Miyazaki, H.

    1984-01-01

    The authors' company developed a new solvent extraction process for zirconium and hafnium separation, and started production of zirconium sponge by this new process in September 1979. The process utilizes selective extraction of zirconium oxysulfate using high-molecular alkyl amine, and has the following advantages: 1. This extraction system has a separation factor as high as 10 to 20 for zirconium and hafnium in the range of suitable acid concentration. 2. In the scrubbing section, removal of all the hafnium that coexists with zirconium in the organic solvent can be effectively accomplished by using scrubbing solution containing hafnium-free zirconium sulfate. Consequently, hafnium in the zirconium sponge obtained is reduced to less than 50 ppm. 3. The extractant undergoes no chemical changes but is very stable for a long period. In particular, its solubility in water is small, about 20 ppm maximum, posing no environmental pollution problems such as are often caused by other process raffinates. At the present time, the zirconium and hafnium separation operation is very stable, and zirconium sponge made by this process can be applied satisfactorily to nuclear reactors

  11. Effects of titanium and zirconium on iron aluminide weldments

    Energy Technology Data Exchange (ETDEWEB)

    Mulac, B.L.; Edwards, G.R. [Colorado School of Mines, Golden, CO (United States). Center for Welding, Joining, and Coatings Research; Burt, R.P. [Alumax Technical Center, Golden, CO (United States); David, S.A. [Oak Ridge National Lab., TN (United States). Metals and Ceramics Div.

    1997-12-01

    When gas-tungsten arc welded, iron aluminides form a coarse fusion zone microstructure which is susceptible to hydrogen embrittlement. Titanium inoculation effectively refined the fusion zone microstructure in iron aluminide weldments, but the inoculated weldments had a reduced fracture strength despite the presence of a finer microstructure. The weldments fractured by transgranular cleavage which nucleated at cracked second phase particles. With titanium inoculation, second phase particles in the fusion zone changed shape and also became more concentrated at the grain boundaries, which increased the particle spacing in the fusion zone. The observed decrease in fracture strength with titanium inoculation was attributed to increased spacing of second phase particles in the fusion zone. Current research has focused on the weldability of zirconium- and carbon-alloyed iron aluminides. Preliminary work performed at Oak Ridge National Laboratory has shown that zirconium and carbon additions affect the weldability of the alloy as well as the mechanical properties and fracture behavior of the weldments. A sigmajig hot cracking test apparatus has been constructed and tested at Colorado School of Mines. Preliminary characterization of hot cracking of three zirconium- and carbon-alloyed iron aluminides, each containing a different total concentration of zirconium at a constant zirconium/carbon ratio of ten, is in progress. Future testing will include low zirconium alloys at zirconium/carbon ratios of five and one, as well as high zirconium alloys (1.5 to 2.0 atomic percent) at zirconium/carbon ratios of ten to forty.

  12. Structure of zirconium dioxide based porous glasses

    Czech Academy of Sciences Publication Activity Database

    Gubanova, N. N.; Kopitsa, G. P.; Ezdakova, K. V.; Baranchikov, A. Y.; Angelov, Borislav; Feoktystov, A.; Pipich, V.; Ryukhtin, Vasyl; Ivanov, V. K.

    2014-01-01

    Roč. 8, č. 5 (2014), s. 967-975 ISSN 1027-4510 R&D Projects: GA ČR GAP208/10/1600; GA MŠk(XE) LM2011019; GA ČR GB14-36566G Institutional support: RVO:61389013 ; RVO:61389005 Keywords : zirconium dioxide * porous glasse * nanoparticles Subject RIV: CF - Physical ; Theoretical Chemistry; BG - Nuclear, Atomic and Molecular Physics, Colliders (UJF-V) Impact factor: 0.359, year: 2012

  13. Evaluation of a Zirconium Recycle Scrubber System

    Energy Technology Data Exchange (ETDEWEB)

    Spencer, Barry B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Bruffey, Stephanie H. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2017-04-01

    A hot-cell demonstration of the zirconium recycle process is planned as part of the Materials Recovery and Waste Forms Development (MRWFD) campaign. The process treats Zircaloy® cladding recovered from used nuclear fuel with chlorine gas to recover the zirconium as volatile ZrCl4. This releases radioactive tritium trapped in the alloy, converting it to volatile tritium chloride (TCl). To meet regulatory requirements governing radioactive emissions from nuclear fuel treatment operations, the capture and retention of a portion of this TCl may be required prior to discharge of the off-gas stream to the environment. In addition to demonstrating tritium removal from a synthetic zirconium recycle off-gas stream, the recovery and quantification of tritium may refine estimates of the amount of tritium present in the Zircaloy cladding of used nuclear fuel. To support these objectives, a bubbler-type scrubber was fabricated to remove the TCl from the zirconium recycle off-gas stream. The scrubber was fabricated from glass and polymer components that are resistant to chlorine and hydrochloric acid solutions. Because of concerns that the scrubber efficiency is not quantitative, tests were performed using DCl as a stand-in to experimentally measure the scrubbing efficiency of this unit. Scrubbing efficiency was ~108% ± 3% with water as the scrubber solution. Variations were noted when 1 M NaOH scrub solution was used, values ranged from 64% to 130%. The reason for the variations is not known. It is recommended that the equipment be operated with water as the scrubbing solution. Scrubbing efficiency is estimated at 100%.

  14. 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)

  15. 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.

  16. Study of zirconium-addition binary systems

    International Nuclear Information System (INIS)

    Wozniakova, B.; Kuchar, L.

    1975-01-01

    The curves are given of the solid and the liquid of binary zirconium-addition systems. Most additions reduce the melting temperature of zirconium. The only known additions to increase the melting temperature are nitrogen, oxygen and hafnium. Also given are the transformation curves of the systems and the elements are given which reduce or raise the temperature of α-β transformation. From the Mendeleev table into which are plotted the curves of the solid and the liquid of binary systems it is possible to predict the properties of unknown binary systems. For the calculations of the curves of the solid and the liquid, 1860 degC was taken as the temperature of zirconium melting. For the calculations of transformation curves, 865 degC was taken as the temperature of α-β transformation. The equations are given of the curves of the solid and the liquid and of the transformation curves of some Zr-addition systems. Also given are the calculated equilibrium distribution coefficients and the equilibrium distribution coefficients of the transformation of additions in Zr and their limit values for temperatures approximating the melting point or the temperature of the transformation of pure Zr, and the values pertaining to eutectic and peritectic or eutectoid and peritectoid temperatures. (J.B.)

  17. Development of zirconium alloy tube manufacturing technology

    International Nuclear Information System (INIS)

    Kim, In Kyu; Park, Chan Hyun; Lee, Seung Hwan; Chung, Sun Kyo

    2009-01-01

    In late 2004, Korea Nuclear Fuel Company (KNF) launched a government funded joint development program with Westinghouse Electric Co. (WEC) to establish zirconium alloy tube manufacturing technology in Korea. Through this program, KNF and WEC have developed a state of the art facility to manufacture high quality nuclear tubes. KNF performed equipment qualification tests for each manufacturing machine with the support of WEC, and independently carried out product qualification tests for each tube product to be commercially produced. Apart from those tests, characterization test program consisting of specification test and characterization test was developed by KNF and WEC to demonstrate to customers of KNF the quality equivalency of products manufactured by KNF and WEC plants respectively. As part of establishment of performance evaluation technology for zirconium alloy tube in Korea, KNF carried out analyses of materials produced for the characterization test program using the most advanced techniques. Thanks to the accomplishment of the development of zirconium alloy tube manufacturing technology, KNF is expected to acquire positive spin off benefits in terms of technology and economy in the near future

  18. Neutronographic Texture Analysis of Zirconium Based Alloys

    International Nuclear Information System (INIS)

    Kruz'elová, M; Vratislav, S; Kalvoda, L; Dlouhá, M

    2012-01-01

    Neutron diffraction is a very powerful tool in texture analysis of zirconium based alloys used in nuclear technique. Textures of five samples (two rolled sheets and three tubes) were investigated by using basal pole figures, inversion pole figures, and ODF distribution function. The texture measurement was performed at diffractometer KSN2 on the Laboratory of Neutron Diffraction, Department of Solid State Engineering, Faculty of Nuclear Sciences and Physical Engineering, CTU in Prague. Procedures for studying textures with thermal neutrons and procedures for obtaining texture parameters (direct and inverse pole figures, three dimensional orientation distribution function) are also described. Observed data were processed by software packages HEXAL and GSAS. Our results can be summarized as follows: i) All samples of zirconium alloys show the distribution of middle area into two maxima in basal pole figures. This is caused by alloying elements. A characteristic split of the basal pole maxima tilted from the normal direction toward the transverse direction can be observed for all samples, ii) Sheet samples prefer orientation of planes (100) and (110) perpendicular to rolling direction and orientation of planes (002) perpendicular to normal direction, iii) Basal planes of tubes are oriented parallel to tube axis, meanwhile (100) planes are oriented perpendicular to tube axis. Level of resulting texture and maxima position is different for tubes and for sheets. The obtained results are characteristic for zirconium based alloys.

  19. low dose irradiation growth in zirconium

    International Nuclear Information System (INIS)

    Fortis, A.M.

    1987-01-01

    Low dose neutron irradiation growth in textured and recrystallized zirconium, is studied, at the Candu Reactors Calandria temperature (340 K) and at 77 K. It was necessary to design and build 1: A facility to irradiate at high temperatures, which was installed in the Argentine Atomic Energy Commission's RA1 Reactor; 2: Devices to carry out thermal recoveries, and 3: Devices for 'in situ' measurements of dimensional changes. The first growth kinetics curves were obtained at 365 K and at 77 K in a cryostat under neutron fluxes of similar spectra. Irradiation growth experiments were made in zirconium doped with fissionable material (0,1 at % 235 U). In this way an equivalent dose two orders of magnitude greater than the reactor's fast neutrons dose was obtained, significantly reducing the irradiation time. The specimens used were bimetallic couples, thus obtaining a great accuracy in the measurements. The results allow to determine that the dislocation loops are the main cause of irradiation growth in recrystallized zirconium. Furthermore, it is shown the importance of 'in situ' measurements as a way to avoid the effect that temperature changes have in the final growth measurement; since they can modify the residual stresses and the overconcentrations of defects. (M.E.L.) [es

  20. Development of Zirconium alloys (for pressure tubes)

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Young Suk; Kwon, Sang Chul; Choo, Ki Nam; Jung, Chung Hwan; Yim, Kyong Soo; Kim, Sung Soo; Baek, Jong Hyuk; Jeong, Yong Hwan; Kim, Kyong Ho; Cho, Hae Dong [Korea Atomic Energy Research Inst., Daeduk (Korea, Republic of); Hwang, S. K.; Kim, M. H. [Inha Univ., Incheon (Korea, Republic of); Kwon, S. I [Korea Univ., Seoul (Korea, Republic of); Kim, I. S. [Korea Advanced Inst. of Science and Technology, Taejon (Korea, Republic of)

    1997-09-01

    The objective of this research is to set up the basic technologies for the evaluation of pressure tube integrity and to develop improved zirconium alloys to prevent pressure tube failures due to DHC and hydride blister caused by excessive creep-down of pressure tubes. The experimental procedure and facilities for characterization of pressure tubes were developed. The basic research related to a better understanding of the in-reactor performances of pressure tubes leads to noticeable findings for the first time : the microstructural effect on corrosion and hydrogen pick-up behavior of Zr-2.5Nb pressure tubes, texture effect on strength and DHC resistance and enhanced recrystallization by Fe in zirconium alloys and etc. Analytical methodology for the assessment of pressure tubes with surface flaws was set up. A joint research is being under way with AECL to determine the fracture toughness of O-8 at the EOL (End of Life) that had been quadruple melted and was taken out of the Wolsung Unit-1 after 10 year operation. In addition, pressure tube with texture controlled is being made along with VNINM in Russia as a joint project between KAERI and Russia. Finally, we succeeded in developing 4 different kinds of zirconium alloys with better corrosion resistance, low hydrogen pickup fraction and higher creep strength. (author). 121 refs., 65 tabs., 260 figs

  1. Low stress creep behaviour of zirconium

    International Nuclear Information System (INIS)

    Prasad, N.

    1989-01-01

    Creep behaviour of alpha zirconium of grain size varying between 16 and 55 μm has been investigated in the temperature range 813 to 1003K at stresses upto 5.5 MNm -2 using high sensitive spring specimen geometry. Creep experiments on specimens of 50 μm grain size revealed a transition from lattice diffusion controlled viscous creep at temperatures greater than 940K to grain boundary diffusion controlled viscous creep at lower temperatures. Tests conducted on either side of the transition suggest the dominance of Nabarro-Herring and Coble creep processes respectively. Evidence for power-law creep has been observed in practically all the creep tests. Based on the experimental data obtained in the present study and those recently reported by Novotny et al (1985), Langdon creep mechanism maps have bee n constructed at 873 and 973K. With the help of these maps for zirconium and those published for titanium the low stress creep behaviour of zirconium and titanium are compared. (author). 22 refs., 11 figs., 3 tabs

  2. 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

  3. Quantitative analysis of nickel in zirconium and zircaloy; Dosage du nickel dans le zirconium et dans le zircaloy

    Energy Technology Data Exchange (ETDEWEB)

    Rastoix, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1957-07-01

    A rapid spectrophotometric has been developed for determination of 10 to 1000 ppm of Ni in zirconium and zircaloy using dimethylglyoxime. Iron, copper, tin and chromium, do not interfere at the concentration usually present in zirconium and its alloys. (author) [French] On determine colorimetriquenent 10 a 1000 ppm de Ni dans le zirconium et le zircaloy par photo colorimetrie a 440 m{mu} de la dimethylglyoxime nickelique. Le dosage est rapide. Le fer, le cuivre, l'etain, le chrome ne genent pas aux concentrations habituellement rencontrees dans le zirconium et ses alliages. (auteur)

  4. Study of carbonitriding thermochemical treatment by plasma screen in active with pressures main austenitic stainless steels AISI 409 and AISI 316L

    International Nuclear Information System (INIS)

    Melo, M.S.; Oliveira, A.M.; Leal, V.S.; Sousa, R.R.M. de; Alves Junior, C.; Centro Federal de Educacao Tecnologica do Piaui; Universidade Federal do Rio Grande do Norte

    2010-01-01

    The technique called Active Screen Plasma Nitriding (ASPN) is being used as an alternative once it offers several advantages with respect to conventional DC plasma. In this method, the plasma does not form directly in the sample's surface but on a screen, in such a way that undesired effects such as the edge effect is minimized. Stainless steels present not very satisfactory wearing characteristics. However, plasma carbonitriding has been used as to improve its resistance to wearing due to the formation of a fine surface layer with good properties. In this work, samples of stainless steel AISI 316L and AISI 409 were treated at pressures of 2.5 and 5 mbar. After the treatments they were characterized by microhardness, microscopy and Xray diffraction. Microscopy and hardness analysis showed satisfactory layers and toughness in those steels. (author)

  5. [The clinical application of zirconium-dioxide-ceramics. Case report].

    Science.gov (United States)

    Somfai, Dóra; Zsigmond, Ágnes; Károlyházy, Katalin; Kispély, Barbara; Hermann, Péter

    2015-12-01

    Due to its outstanding physical, mechanical and esthetic properties, zirconium-dioxide is one of the most popular non-metal denture, capable of surpassing PFM in most cases. The recent advances of CAD/CAM technology makes it a good alternitve. Here we show the usefulness of zirconium-dioxide in everyday dental practice through three case reports.

  6. Thermotransport of nitrogen and oxygen in β-zirconium

    NARCIS (Netherlands)

    Vogel, D.L.; Rieck, G.D.

    1971-01-01

    An investigation of thermotransport of nitrogen in ß-zirconium is reported. Using a method previously described, the heat of transport turned out to be 25.1 kcal/mole with a standard deviation of 2.5 kcal/mole. The formerly published value of the heat of transport of oxygen in ß-zirconium, viz. 20

  7. Quantitative analysis of nickel in zirconium and zircaloy

    International Nuclear Information System (INIS)

    Rastoix, M.

    1957-01-01

    A rapid spectrophotometric has been developed for determination of 10 to 1000 ppm of Ni in zirconium and zircaloy using dimethylglyoxime. Iron, copper, tin and chromium, do not interfere at the concentration usually present in zirconium and its alloys. (author) [fr

  8. Effect of zirconium addition on the recrystallization behaviour of a ...

    Indian Academy of Sciences (India)

    In the present work, zirconium was added to a commercial Al–Cu–Mg alloy and by heat treatment Al3Zr particles were precipitated and after forging, the grain size was an order of magnitude lower than the alloy without zirconium. Transmission electron microscopy was employed to characterize the second phase particles, ...

  9. Molten salt scrubbing of zirconium or hafnium tetrachloride

    International Nuclear Information System (INIS)

    Lee, E.D.; McLaughlin, D.F.

    1990-01-01

    This patent describes a continuous process for removing impurities of iron or aluminum chloride or both from vaporous zirconium or hafnium chloride or both. It comprises: introducing impure zirconium or hafnium chloride vapor or both into a middle portion of an absorbing column containing a molten salt phase, the molten salt phase absorbing the impurities of iron or aluminum chloride or both to produce chloride vapor stripped of zirconium or hafnium chloride; introducing sodium or potassium chloride or both into a top portion of the column; controlling the top portion of the column to between 300--375 degrees C.; heating a bottom portion of the column to 450--550 degrees C. To vaporize zirconium chloride or hafnium chloride or hafnium and zirconium chloride from the molten salt; withdrawing molten salt substantially free of zirconium and hafnium chloride from the bottom portion of the column; and withdrawing zirconium chloride or hafnium chloride or hafnium and zirconium chloride vapor substantially free of impurities of iron and aluminum chloride from the top of the column

  10. Formation of zirconium dioxide layers on microelectrode of zirconium. Inhibition of the hydrogen evolution reaction

    Czech Academy of Sciences Publication Activity Database

    Pospíšil, Lubomír; Fanelli, N.; Hromadová, Magdaléna

    2017-01-01

    Roč. 49, C (2017), s. 128-133 ISSN 0324-1130 R&D Projects: GA ČR(CZ) GA16-03085S Institutional support: RVO:61388955 Keywords : zirconium * ZrO2 * corrosion Subject RIV: CG - Electrochemistry OBOR OECD: Electrochemistry (dry cells, batteries, fuel cells, corrosion metals, electrolysis) Impact factor: 0.238, year: 2016

  11. PROCESS FOR DISSOLVING BINARY URANIUM-ZIRCONIUM OR ZIRCONIUM-BASE ALLOYS

    Science.gov (United States)

    Jonke, A.A.; Barghusen, J.J.; Levitz, N.M.

    1962-08-14

    A process of dissolving uranium-- zirconium and zircaloy alloys, e.g. jackets of fuel elements, with an anhydrous hydrogen fluoride containing from 10 to 32% by weight of hydrogen chloride at between 400 and 450 deg C., preferably while in contact with a fluidized inert powder, such as calcium fluoride is described. (AEC)

  12. Phase Transformations in a Uranium-Zirconium Alloy containing 2 weight per cent Zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Lagerberg, G

    1961-04-15

    The phase transformations in a uranium-zirconium alloy containing 2 weight percent zirconium have been examined metallographically after heat treatments involving isothermal transformation of y and cooling from the -y-range at different rates. Transformations on heating and cooling have also been studied in uranium-zirconium alloys with 0.5, 2 and 5 weight per cent zirconium by means of differential thermal analysis. The results are compatible with the phase diagram given by Howlett and Knapton. On quenching from the {gamma}-range the {gamma} phase transforms martensitically to supersaturated a the M{sub S} temperature being about 490 C. During isothermal transformation of {gamma} in the temperature range 735 to 700 C {beta}-phase is precipitated as Widmanstaetten plates and the equilibrium structure consists of {beta} and {gamma}{sub 1}. Below 700 C {gamma} transforms completely to Widmanstaetten plates which consist of {beta} above 660 C and of a at lower temperatures. Secondary phases, {gamma}{sub 2} above 610 C and {delta} below this temperature, are precipitated from the initially supersaturated Widmanstaetten plates during the isothermal treatments. At and slightly below 700 C the cooperative growth of |3 and {gamma}{sub 2} is observed. The results of isothermal transformation are summarized in a TTTdiagram.

  13. 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)

  14. 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

  15. Zirconium alloy fuel cladding resistant to PCI crack propagation

    International Nuclear Information System (INIS)

    Boyle, R.F.; Foster, J.P.

    1987-01-01

    A nuclear fuel element is described cladding tube comprising: concentric tubular layers of zirconium base alloys; the concentric tubular layers including an inner layer and outer layer; the outer layer metallurgically bonded to the inner layer; the outer layer composed of a first zirconium base alloy characterized by excellent resistance to corrosion caused by exposure to high temperature and pressure aqueous environments; the inner layer composed of a second zirconium base alloy consisting of: about 0.2 to 0.6 wt.% tin, about 0.03 to 0.11 wt.% iron, less than about 0.02 wt.% chromium, up to about 350 ppm oxygen and the remainder being zirconium and incidental impurities, and the inner layer characterized by improved resistance to crack propagation under reactor operating conditions compared to the first zirconium alloy

  16. Antimony removal from aqueous solutions using Zirconium hydroxide

    International Nuclear Information System (INIS)

    Petrescu, D.; Velciu, L.; Bucur, C.

    2016-01-01

    In this paper it is presented an experimental test for non-radioactive antimony removal from aqueous solutions using zirconium hydroxide powder. Also, it was studied how the temperature and pH influences antimony adsorption onto zirconium hydroxide surface. After the adsorption, solutions were filtered on Cellulose Mixed Ester Membrane with 0.2 μm pore size to remove the zirconium powder and then the aqueous solutions were sent to Inductively Coupled Plasma Optic Emission Spectrometry (ICP-OES) for quantitative analysis of Sb. Zirconium hydroxide powders were examined by optical microscopy. For the solutions that were tested at pH 4.5 and 10.2 the antimony concentration dropped below the detection limit of ICP-OES device, proof of antimony adsorption on zirconium hydroxide. Also, for the other tested solutions which had pH=12 the antimony concentration reduced with 77% and 80%. The temperature had no influence upon adsorption mechanism. (authors)

  17. 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.)

  18. Adherent zirconia films by reactive ion implantation

    International Nuclear Information System (INIS)

    Bunker, S.N.; Armini, A.J.

    1993-01-01

    Conventional methods of forming ceramic coatings on metal substrates, such as CVD or plasma spray, typically retain a sharp interface and may have adhesion problems. In order to produce a completely mixed interface for better adhesion, a method using reactive ion implantation was used which can grow a thick stoichiometric film of an oxide ceramic starting from inside the substrate. Zirconium oxide ceramic films have been produced by this technique using a high-energy zirconium ion beam in an oxygen gas ambient. Compositional data are shown based on Auger electron spectroscopy of the film. Tribological properties of the layer were determined from wear and friction measurements using a pin-on-disk test apparatus. The adhesion was measured both by a scratch technique as well as by thermal shock. Results show an extremely adherent ZrO 2 film with good tribological properties

  19. 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

  20. 21 CFR 700.16 - Use of aerosol cosmetic products containing zirconium.

    Science.gov (United States)

    2010-04-01

    ... zirconium. 700.16 Section 700.16 Food and Drugs FOOD AND DRUG ADMINISTRATION, DEPARTMENT OF HEALTH AND HUMAN... cosmetic products containing zirconium. (a) Zirconium-containing complexes have been used as an ingredient... indicates that certain zirconium compounds have caused human skin granulomas and toxic effects in the lungs...

  1. ZIRCONIUM-TITANIUM-BERYLLIUM BRAZING ALLOY

    Science.gov (United States)

    Gilliland, R.G.; Patriarca, P.; Slaughter, G.M.; Williams, L.C.

    1962-06-12

    A new and improved ternary alloy is described which is of particular utility in braze-bonding parts made of a refractory metal selected from Group IV, V, and VI of the periodic table and alloys containing said metal as a predominating alloying ingredient. The brazing alloy contains, by weight, 40 to 50 per cent zirconium, 40 to 50 per cent titanium, and the balance beryllium in amounts ranging from 1 to 20 per cent, said alloy having a melting point in the range 950 to 1400 deg C. (AEC)

  2. Irradiation induced effects in zirconium (A review)

    International Nuclear Information System (INIS)

    Madden, P.K.

    1975-06-01

    Irradiation creep in zirconium and its alloys is comprehensively discussed. The main theories are outlined and the gaps between them and the observed creep behaviour, indicated. Although irradiation induced point defects play an important role, effects due to irradiation induced dislocation loops seem insignificant. The experimental results suggest that microstructural variations due to prior cold-working or hydrogen injection perturb the irradiation growth and the irradiation creep of zircaloy. Further investigations into these areas are required. One disadvantage of creep experiments lies in their duration. The possibility of accelerated experiments using ion implantation or electron irradiation is examined in the final section, and its possible advantages and disadvantages are outlined. (author)

  3. Minimizing hydride cracking in zirconium alloys

    International Nuclear Information System (INIS)

    Coleman, C.E.; Cheadle, B.A.; Ambler, J.F.R.; Eadie, R.L.

    1985-01-01

    Zirconium alloy components can fail by hydride cracking if they contain large flaws and are highly stressed. If cracking in such components is suspected, crack growth can be minimized by following two simple operating rules: components should be heated up from at least 30K below any operating temperature above 450K, and when the component requires cooling to room temperature from a high temperature, any tensile stress should be reduced as much and as quickly as is practical during cooling. This paper describes the physical basis for these rules

  4. Quantitative spectrographic determination of zirconium minerals

    International Nuclear Information System (INIS)

    Rocal Adell, M.; Alvarez Gonzalez, F.; Fernandez Cellini, R.

    1958-01-01

    The method described in the following report permits the quantitative determination of zirconium in minerals and rocks in a 0,02-100% of ZrO 2 concentration rate. The excitation is carried out by a 10 ampere continuous current arc among carbon electrodes, and placing the sample in a crater of 2 mm depth. For low concentrations a dilution of the sample with the same weight as its own in carbon powder and with 1/25 of its weight of Co 3 O 4 (internal patron) is carried out. Line Zr 2571,4, Co 2585,3 and Co 2587,2 are used. (Author) 6 refs

  5. Phase equilibria at the Zirconium metal purification

    International Nuclear Information System (INIS)

    Dwiretnani-Sudjoko; Busron-Masduki; Sunardjo; Budi-Sulistyo

    1996-01-01

    It was investigated the research in the purification of zirconium metal, which was results from the reduction process, by adding heat in the vacuum environment. The process was done in batch in the stainless steel reactor, equiped with vacuum pump and electric heater. The investigated variable were process temperature and pressure. From this research it was obtained that equilibrium constant for MgCl 2 and Mg were expressed in the equation K M g C l 2 = 0.9011 P 1 .3779 1.06552 T and K M g = 6.0115P + 1.35256T - 6.93912

  6. Zirconium coatings doped with nanoparticles for the protection of stainless steel

    International Nuclear Information System (INIS)

    Pineda, F; Vargas, E; Martinez, C; Sancy, M; Rabagliati, F.M; Pavez, J; Paez, M.A

    2008-01-01

    The anticorrosive protection of metal alloys, like stainless steel, is usually carried out with chrome-based coatings, but the toxic wastes associated with the process minimizes its applicability. The above has motivated the search for alternative protection methodologies, among which are the inorganic polymers prepared by the sol-gel method, which are a viable protection alternative because of their outstanding chemical and physical properties in aggressive environments. Despite the method's benefits, the application of sol-gel coatings to metals exposed to highly corrosive materials is restricted due to the substantial porosity of the films. Recent studies report that this limiting factor can be diminished by adding inorganic nanoparticles to the polymeric matrices, significantly improving the anticorrosive properties of the coatings. Considering the above, this work evaluated the inclusion of iron oxide nanoparticles (III) in zirconium polymeric matrices for the protection of 316 and 316L stainless steel. Electrochemical techniques, such as polarization curves and electrochemical impedance spectroscopy and morphological analysis with atomic force microscopy were used for this purpose. The responses obtained showed improvements in the anticorrosive properties of the zirconium films when doped with nanoparticles, and the best protective response was obtained with the minimum amount of the nanomaterial, aided by a significant increase in the metallic material's passivity. A critical content of nanoparticles was also identified in the polymeric matrix, above which the coating suffers serious deterioration, caused by the apparent formation of percolation channels leading to the oversaturation of the polymeric matrix

  7. The development of zirconium alloy and its manufacturing

    International Nuclear Information System (INIS)

    Yuan Gaihuan; Yue Qiang

    2015-01-01

    Nuclear power which acts as one of low-carbon energy resources is the most realistic in large-scale application. It is also the preferred choice for many countries to develop energy resources and optimize its structure. Zirconium alloy is a key structural material for nuclear power plant fuel assemblies and cladding tubes of zirconium alloy are often referred as the first safeguard to nuclear power safety. With the development of nuclear power, three kinds of zirconium alloys Zr-Sn, Zr-Nb, Zr-Sn-Nb and with the representative products of Zr-4, M5, Zirlo respectively are developed and widely applied. Because of its severe operating environment and influence to nuclear safety, the requirements to zirconium alloys for physical and chemical properties, nuclear capability, tolerance and surface quality are very strict. The in-depth research and its manufacture capability become one of the main barriers for many countries who are developing the nuclear energy. In recent years, a stated-owned company, State Nuclear Bao Ti Zirconium Industry Company ('SNZ' for short) as well as National R and D Center for Nuclear Grade Zirconium material, is founded to meet the requirement of the rapid development of China's nuclear power industry. SNZ is dedicated for the fabrication and the research of nuclear grade zirconium products. After the successful completion of technology transfer of manufacturing for production chain and fully grasped of the manufacturing technology for the nuclear grade zirconium sponge through zirconium alloy tube, rod and strip products. National R and D Center for Nuclear Grade Zirconium material is cooperating with universities, nuclear energy research and design institutes and the owners of nuclear power plant to develop new zirconium alloy of self-owned brand. Through the selection of components, in-process testing and product inspection, four kinds of new zirconium alloys owns better performance than currently commercialized M5, Zirlo etc

  8. 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

  9. Recrystallization resistance in aluminum alloys containing zirconium

    International Nuclear Information System (INIS)

    Ranganathan, K.

    1991-01-01

    Zirconium forms a fine dispersion of the metastable β' (Al 3 Zr) phase that controls recrystallization by retarding the motion of high-angle boundaries. The primary material chosen for this research was aluminum alloy 7150 containing zinc, magnesium, and copper as the major solute elements and zirconium as the dispersoid-forming element. The size, distribution, and the volume fraction of β' was controlled by varying the alloy composition and preheat practices. Preheated ingots were subjected to a specific sequence of hot-rolling operations to evaluate the resistance to recrystallization of the different microstructures. Optical and transmission electron microscopy (TEM) techniques were used to investigate the influence of dispersoid morphology resulting from the thermal treatments and deformation processing on the recrystallization behavior of the alloy. Studies were conducted to determine the influence of the individual solute elements present in 7150 on the precipitation of β' and consequently on the recrystallization behavior of the material. These studies were done on compositional variants of commercial 7150

  10. 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.

  11. 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.

  12. 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)

  13. Irradiation growth in zirconium alloys: a review

    International Nuclear Information System (INIS)

    Fidleris, V.

    1980-09-01

    The change in shape during irradiation without external stress, irradiation growth, was first discovered in uranium and later in graphite, zirconium and other core materials which exhibit anisotropic physical properties. The direction of maximum growth of metals invariably corresponds with the direction of minimum thermal expansion. In polycrystalline zirconium alloys growth is positive in the direction of maximum deformation during fabrication and in other directions it can be either positive or negative depending on the preferred orientation of grains (crystallographic texture). Growth increases gradually with temperature between 300 K and 620 K and rapidly with fluence up to about 1 x 10 25 n.m. -2 (Eμ1 MeV). At higher fluences the growth appears to saturate in annealed materials and reach a steady rate approximately proportional to dislocation density in cold-worked materials. Above 600 K both annealed and cold-worked materials have similar steady growth rates. Irradiation growth is caused by the segregation to different sinks of the vacancies and interstitials generated by irradiation, but the dominant types of sinks for each type of point defect and the mode of transport of the point defects to sinks cannot therefore be predicted theoretically. For the purpose of designing reactor core components empirical equations have been derived that can satisfactorily predict the steady state growth behaviour from texture and microstructure. (auth)

  14. 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

  15. 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)

  16. Research and development of zirconium industry in China

    International Nuclear Information System (INIS)

    Liu Jianzhang; Tian Zhenye

    2001-01-01

    The development of uranium material for nuclear power and silicon material for information industry represents two revolutionary changes in the material field in 20-th century. The development of these kinds of materials not only brings about great revolution of technology in the material field, but also promotes the great advancement of the world economy. Zirconium or its alloy, as one of the most important material in atomic age, just as the same as foreign countries has been developed under promotion of nuclear submarine project in China, and building of civil nuclear power reactor then has been laid a solid foundation for zirconium industry and provide a broad market for zirconium material

  17. RECOVERY OF URANIUM FROM ZIRCONIUM-URANIUM NUCLEAR FUELS

    Science.gov (United States)

    Gens, T.A.

    1962-07-10

    An improvement was made in a process of recovering uranium from a uranium-zirconium composition which was hydrochlorinated with gsseous hydrogen chloride at a temperature of from 350 to 800 deg C resulting in volatilization of the zirconium, as zirconium tetrachloride, and the formation of a uranium containing nitric acid insoluble residue. The improvement consists of reacting the nitric acid insoluble hydrochlorination residue with gaseous carbon tetrachloride at a temperature in the range 550 to 600 deg C, and thereafter recovering the resulting uranium chloride vapors. (AEC)

  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. Study of the uranium-zirconium diffusion; Etude de la diffusion uranium-zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Adda, Y; Mairy, C; Bouchet, P [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1957-07-01

    The intermetallic diffusion of uranium fuel and zirconium used as cladding is studied. Intermetallic diffusion can occur during the cladding of uranium rods and uranium can penetrate the zirconium cladding. Different parameters are involved in this mechanism as structure and mechanical properties of the diffusion area as well as presence of impurities in the metal. The uses of different analysis techniques (micrography, Castaing electronic microprobe, microhardness and autoradiography) have permitted to determine with great accuracy the diffusion coefficient in gamma phase (body centered cubic system) and the results have given important information on the intermetallic diffusion mechanisms. The existence of the Kirkendall effect in the U-Zr diffusion is also an argument in favor of the generality of the diffusion mechanism by vacancies in body centered cubic system. (M.P.)

  20. Separation process of zirconium and hafnium; Procede de separation du zirconium et du hafnium

    Energy Technology Data Exchange (ETDEWEB)

    Hure, J; Saint-James, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-07-01

    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{sub 3}{sup -} ions concentration, the role of the cation coming with NO{sub 3}{sup -}, as well as the influence of the concentration of zirconium in the solution on the separation coefficient {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (M.B.) [French] Des differents procedes de separation zirconium-hafnium, l'extraction par solvant en contre-courant est le procede le plus facilement utilisable a l'echelle industrielle. On utilise comme solvant le phosphate de tributyle, dilue avec du white spirit pour faciliter les decantations. Des essais preliminaires ont montre que le milieu nitrique semblait le plus favorable a l'extraction; mais beaucoup d'autres facteurs interviennent dans le processus de separation. Nous avons etudie successivement l'influence de l'acidite, celle de la concentration en ions NO{sub 3}{sup -}, le role du cation accompagnant NO{sub 3}{sup -}, ainsi que l'influence de la concentration en zirconium de la solution sur le coefficient de separation {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (MB)

  1. 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

  2. A computer model for hydride blister growth in zirconium alloys

    International Nuclear Information System (INIS)

    White, A.J.; Sawatzky, A.; Woo, C.H.

    1985-06-01

    The failure of a Zircaloy-2 pressure tube in the Pickering unit 2 reactor started at a series of zirconium hydride blisters on the outside of the pressure tube. These blisters resulted from the thermal diffusion of hydrogen to the cooler regions of the pressure tube. In this report the physics of thermal diffusion of hydrogen in zirconium is reviewed and a computer model for blister growth in two-dimensional Cartesian geometry is described. The model is used to show that the blister-growth rate in a two-phase zirconium/zirconium-hydride region does not depend on the initial hydrogen concentration nor on the hydrogen pick-up rate, and that for a fixed far-field temperature there is an optimum pressure-type/calandria-tube contact temperature for growing blisters. The model described here can also be used to study large-scale effects, such as hydrogen-depletion zones around hydride blisters

  3. Ductile zirconium powder by hydride-dehydride process

    Energy Technology Data Exchange (ETDEWEB)

    Krishnan, T S [BHABHA ATOMIC RESEARCH CENTRE, BOMBAY (INDIA); CHAUDHARY, S [NUCLEAR FUEL COMPLEX, HYDERABAD (INDIA)

    1976-09-01

    The preparation of ductile zirconium powder by the hydride-dehydride process has been described. In this process massive zirconium obtained from Kroll reduction of ZrCl/sub 4/ is first rendered brittle by hydrogenation and the hydride crushed and ground in a ball mill to the required particle size. Hydrogen is then hot vacuum extracted to yield the metal powder. The process has been successfully employed for the production of zirconium powders with low oxygen content and having hardness values in the range of 115-130 BHN, starting from a zirconium sponge of 100-120 BHN hardness. Influence of surface characteristics of the starting metal on its hydriding behaviour has been studied and the optimum hydriding-dehydriding conditions established.

  4. 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.)

  5. Spectrophotometric titration of sulfates in the presence of zirconium

    International Nuclear Information System (INIS)

    Kuznetsov, V.V.; Kotova, S.S.; Molokanova, L.G.; Chekmarev, A.M.; Yagodin, G.A.

    1978-01-01

    The procedure has been proposed for express determination of sulphate ions in the presence of zirconium by spectrophotometric titration with the use of barium chloride and nitrochromazo as an indicator. The procedure is based on bonding zirconium into a more stable complex with EDTA (ethylenediaminotetraacetic acid). The presence of excess of EDTA and zirconium (4) complexonate in the solution being titrated does not affect the titration curve shape and the character of break on the curve in the equivalence point. A complete demasking of SO 4 2- is observed in the case of 1O-fold excess of EDTA with respect to zirconium (4). Statistic evaluation of the method has shown that the results of titration can be distorted by chance errors only

  6. Development of zirconium hydride highly effective moderator materials

    International Nuclear Information System (INIS)

    Yin Changgeng

    2005-10-01

    The zirconium hydride with highly content of hydrogen and low density is new efficient moderator material for space nuclear power reactor. Russia has researched it to use as new highly moderator and radiation protection materials. Japanese has located it between the top of pressure vessel and the main protection as a shelter, the work temperature is rach to 220 degree C. The zirconium hydride moderator blocks are main parts of space nuclear power reactor. Development of zirconium hydride moderator materials have strength research and apply value. Nuclear Power Research and Design Instituteoh China (NPIC) has sep up the hydrogenation device and inspect systems, and accumurate a large of experience about zirconium hydride, also set up a strict system of QA and QC. (authors)

  7. Investigation of colourless complexes of thorium, hafnium and zirconium

    International Nuclear Information System (INIS)

    Kiciak, S.; Stefanowicz, T.; Gontarz, H.; Swit, Z.

    1980-01-01

    The investigations conducted in the Institute of General Chemistry of Poznan Technical University in partial cooperation with Kharkhof Technical University related with thorium, hafnium and zirconium complexes are reviewed. (author)

  8. Uranium (Vi) sorption onto zirconium diphosphate chemically modified

    International Nuclear Information System (INIS)

    Garcia G, N.; Ordonez R, E.

    2010-10-01

    This work deals with the uranium (Vi) speciation after sorption onto zirconium diphosphate (ZrP 2 O 7 ) surface, hydrated and in a surface modified with organic acids. Oxalic and citric acids were chosen to modify the ZrP 2 O 7 surface because they have poly carboxylic groups and they mimic the organic matter in nature. Thus the interest of this work is to evaluate the uranium (Vi) sorption edge at different s ph values in natural and modified surfaces. The luminescence technique (fluorescence and phosphorescence, respectively) was used for the quantification and speciation of uranyl sorbed at the zirconium diphosphate interface. The fluorescence experiment, showed that adsorption of uranyl on surface of zirconium diphosphate tends to 100%. The speciation shows that there are different complexes in surface which were formed between zirconium diphosphate and uranyl, since it is produced a displacement of wavelength in fluorescence spectra of each system. (Author)

  9. Zirconium analysis. Impurities determination by spark mass specrometry

    International Nuclear Information System (INIS)

    Anon.

    Determination of impurities in zirconium, suitable for atomic content greater than 10 -8 but particularly adapted for low contents. The method is quantitative only if a reference sample is available (metallic impurities) [fr

  10. Radiation stability of proton irradiated zirconium carbide

    International Nuclear Information System (INIS)

    Yang, Yong; Dickerson, Clayton A.; Allen, Todd R.

    2009-01-01

    The use of zirconium carbide (ZrC) is being considered for the deep burn (DB)-TRISO fuel as a replacement for the silicon carbide coating. The radiation stability of ZrC was studied using 2.6 MeV protons, across the irradiation temperature range from 600 to 900degC and to doses up to 1.75 dpa. The microstructural characterization shows that the irradiated microstructure is comprised of a high density of nanometer-sized dislocation loops, while no irradiation induced amorphization or voids are observed. The lattice expansion induced by point defects is found to increase as the dose increases for the samples irradiated at 600 and 800degC, while for the 900degC irradiation, a slight lattice contraction is observed. The radiation hardening is also quantified using a micro indentation technique for the temperature and doses studies. (author)

  11. In situ hydrogen loading on zirconium powder

    Energy Technology Data Exchange (ETDEWEB)

    Maimaitiyili, Tuerdi, E-mail: tuerdi.maimaitiyili@mah.se; Blomqvist, Jakob [Malmö University, Östra Varvsgatan 11 A, Malmö, Skane 20506 (Sweden); Steuwer, Axel [Lund University, Ole Römers väg, Lund, Skane 22100 (Sweden); Nelson Mandela Metropolitan University, Gardham Avenue, Port Elizabeth 6031 (South Africa); Bjerkén, Christina [Malmö University, Östra Varvsgatan 11 A, Malmö, Skane 20506 (Sweden); Zanellato, Olivier [Ensam - Cnam - CNRS, 151 Boulevard de l’Hôpital, Paris 75013 (France); Blackmur, Matthew S. [Materials Performance Centre, School of Materials, The University of Manchester, Manchester M1 7HS (United Kingdom); Andrieux, Jérôme [European Synchrotron Radiation Facility, 6 rue J Horowitz, Grenoble 38043 (France); Université de Lyon, 43 Bd du 11 novembre 1918, Lyon 69100 (France); Ribeiro, Fabienne [Institut de Radioprotection et Sûreté Nucléaire, IRSN, BP 3, 13115 Saint-Paul Lez Durance (France)

    2015-06-26

    Commercial-grade Zr powder loaded with hydrogen in situ and phase transformations between various Zr and ZrH{sub x} phases have been monitored in real time. For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studied in situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement.

  12. 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.

  13. Irradiation effects in hydrated zirconium molybdate

    Energy Technology Data Exchange (ETDEWEB)

    Fourdrin, C., E-mail: chloe.fourdrin@polytechnique.edu [CEA Saclay, DEN/DANS/DPC/SECR/LSRM, 91 191 Gif-sur-Yvette (France); CEA Saclay, DSM/IRAMIS/SIS2M-UMR 3299/Lrad, 91 191 Gif-sur-Yvette (France); Esnouf, S. [CEA Saclay, DSM/IRAMIS/SIS2M-UMR 3299/Lrad, 91 191 Gif-sur-Yvette (France); Dauvois, V. [CEA Saclay, DEN/DANS/DPC/SECR/LSRM, 91 191 Gif-sur-Yvette (France); Renault, J.-P. [CEA Saclay, DSM/IRAMIS/SIS2M-UMR 3299/Lrad, 91 191 Gif-sur-Yvette (France); Venault, L. [CEN Valrho, DEN/DRCP/SCPS/LC2A, 30 207 Bagnols-sur-Ceze (France); Tabarant, M. [CEA Saclay, DEN/DANS/DPC/LRSI, 91 191 Gif-sur-Yvette (France); Durand, D. [CEA Saclay, DEN/DANS/DPC/SECR/LSRM, 91 191 Gif-sur-Yvette (France); Cheniere, A. [CEA Saclay, DEN/DANS/DPC/LRSI, 91 191 Gif-sur-Yvette (France); Lamouroux-Lucas, C. [CEA Saclay, DEN/DANS/DPC/SECR/LSRM, 91 191 Gif-sur-Yvette (France); Cochin, F. [AREVA NC Tour, AREVA, 92 084 Paris La Defense cedex (France)

    2012-07-15

    Hydrated zirconium molybdate is a precipitate formed during the process of spent nuclear fuel dissolution. In order to study the radiation stability of this material, we performed gamma and electron irradiation in a dose range of 10-100 kGy. XRD patterns showed that the crystalline structure is not affected by irradiation. However, the yellow original sample exhibits a blue-grey color after exposure. The resulting samples were analyzed by means of EPR and diffuse reflectance spectroscopy. Two sites for trapped electrons were evidenced leading to a d{sup 1} configuration responsible for the observed coloration. Moreover, a third defect corresponding to a hole trapped on oxygen was observed after electron irradiation at low temperature.

  14. Progress in zirconium resonance ionization spectroscopy

    International Nuclear Information System (INIS)

    Page, R.H.; Dropinski, S.C.; Worden, E.F.; Stockdale, J.A.D.

    1993-01-01

    The authors have examined the stepwise-resonant three-photon-ionization spectrum of neutral zirconium atoms using three separately-tunable pulsed visible dye lasers. The ground-level (first-step) transitions were chosen on the basis of demonstrated 91 Zr selectivity. Lifetimes of even-parity levels around 36,000 cm -1 , measured with the delayed-photoionization technique, range from 10 to 100 nsec. Direct ionization cross sections appear to be less than 10 -17 cm 2 ; newly-detected autoionizing levels give peak ionization cross sections (inferred from saturation fluences) up to 10 -15 cm 2 . Portions of Rydberg series converging to the 315 and 763 cm -1 levels of Zr + were identified. Clumps of autoionizing levels are thought to be due to Rydberg-valence mixing

  15. In situ hydrogen loading on zirconium powder

    International Nuclear Information System (INIS)

    Maimaitiyili, Tuerdi; Blomqvist, Jakob; Steuwer, Axel; Bjerkén, Christina; Zanellato, Olivier; Blackmur, Matthew S.; Andrieux, Jérôme; Ribeiro, Fabienne

    2015-01-01

    Commercial-grade Zr powder loaded with hydrogen in situ and phase transformations between various Zr and ZrH x phases have been monitored in real time. For the first time, various hydride phases in a zirconium–hydrogen system have been prepared in a high-energy synchrotron X-ray radiation beamline and their transformation behaviour has been studied in situ. First, the formation and dissolution of hydrides in commercially pure zirconium powder were monitored in real time during hydrogenation and dehydrogenation, then whole pattern crystal structure analysis such as Rietveld and Pawley refinements were performed. All commonly reported low-pressure phases presented in the Zr–H phase diagram are obtained from a single experimental arrangement

  16. Fluorimetric determination of uranium in zirconium and zircaloy alloys

    International Nuclear Information System (INIS)

    Acosta L, E.

    1991-05-01

    The objective of this procedure is to determine microquantities of uranium in zirconium and zircaloy alloys. The report also covers the determination of uranium in zirconium alloys and zircaloy in the range from 0.25 to 20 ppm on 1 g of base sample of radioactive material. These limit its can be variable if the size of the used aliquot one is changed for the final determination of uranium. (Author)

  17. Arc melting in inert gas atmosphere of zirconium sponge

    International Nuclear Information System (INIS)

    Julio Junior, O.; Andrade, A.H.P. de

    1991-01-01

    The obtainment of metallic zirconium in laboratory scale with commercial and nuclear quality is the objective of the Metallurgy Department of IEN/CNEN - Brazil, so a melting procedure of zirconium sponge in laboratory scale using an arc furnace in inert atmosphere is developed. The effects of atmosphere operation, and the use of gas absorber and the sponge characteristics over the quality of button in as-cast reporting with hardness measures are described. (C.G.C.)

  18. 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

  19. Modelling of Zirconium and Hafnium separation using continuous annular chromatography

    International Nuclear Information System (INIS)

    Moch-Setyadji; Endang Susiantini

    2014-01-01

    Nuclear degrees of zirconium in the form of a metal alloy is the main material for fuel cladding of NPP. Zirconium is also used as sheathing UO 2 kernel in the form of ZrC as a substitute of SiC in the fuel elements of High Temperature Reactor (HTR). Difficulty separating hafnium from zirconium because it has a lot of similarities in the chemical properties of Zr and Hf. Annular chromatography is a device that can be used for separating of zirconium and hafnium to obtain zirconium nuclear grade. Therefore, it is necessary to construct the mathematical modelling that can describe the separation of zirconium and hafnium in the annular chromatography containing anion resin dowex-1X8. The aim of research is to perform separation simulation by using the equilibrium model and mass transfer coefficient resulted from research. Zr and Hf feed used in this research were 26 and 1 g/l, respectively. Height of resin (L), angular velocity (ω) and the superficial flow rate (uz) was varied to determine the effect of each parameter on the separation of Zr and Hf. By using Kd and Dv values resulted previous research. Simulation results showed that zirconium and hafnium can be separated using a continuous annular chromatography with high resin (long bed) 50 cm, superficial flow rate of 0.001 cm/s, the rotation speed of 0.006 rad/min and 20 cm diameter annular. In these conditions the results obtained zirconium concentration of 10,303.226 g/m 3 and hafnium concentration of 12.324 g/m 3 (ppm). (author)

  20. Identification and characterization of a new Zirconium hydride

    International Nuclear Information System (INIS)

    Zhao, Z.

    2007-01-01

    In order to control the integrity of the fuel clad, alloy of zirconium, it is necessary to predict the behavior of zirconium hydrides in the environment (temperature, stress...), at a microscopic scale. A characterization study by TEM of hydrides has been realized. It shows little hydrides about 500 nm, in hydride Zircaloy 4. Then a more detailed study identified a new hydride phase presented in this paper. (A.L.B.)

  1. Synthesis of zirconium by zirconium tetrachloride reduction by magnesio-thermia. Experimental study and modelling; Elaboration de zirconium par reduction de tetrachlorure de zirconium par magnesothermie. Etude experimentale et modelisation

    Energy Technology Data Exchange (ETDEWEB)

    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{sub 4} + 2 Mg = 2 MgCl{sub 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.)

  2. 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

  3. Zirconium molybdate hydrate precipitates in spent nuclear fuel reprocessing

    International Nuclear Information System (INIS)

    Magnaldo, A.; Noire, M.H.; Esbelin, E.; Dancausse, J.P.; Picart, S.

    2004-01-01

    This paper presents through 2 posters a general overview studies realised by CEA teams on deposits observed in the La Hague plant dissolution facilities. Their main constituents are metallic debris bound together with zirconium molybdate hydrate. A comprehensive study of zirconium molybdate hydrate formation included nucleation and growth kinetics was developed. Fouling mechanisms were consequently explained as influenced by the operation conditions. Pu insertion was also overviewed. Its behaviour is important when curative and preventive chemical treatments are considered. (authors)

  4. 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

  5. Sorption of cesium on titanium and zirconium phosphates

    International Nuclear Information System (INIS)

    Lebedev, V.N.; Mel'nik, N.A.; Rudenko, A.V.

    2003-01-01

    Titanium and zirconium phosphates were prepared from mineral raw materials of the Kola Peninsula. Their capability to recover cesium cations from the model solutions and liquid radioactive waste (LRW) was studied. Titanium phosphate prepared from solutions formed by titanite breakdown demonstrates greater distribution coefficients of cesium as compared to zirconium phosphate. Titanium phosphate as a cheaper agent featuring greater sorption capacity was recommended for treatment of LRW to remove cesium [ru

  6. An evaluated neutronic data file for elemental zirconium

    International Nuclear Information System (INIS)

    Smith, A.B.; Chiba, S.

    1994-09-01

    A comprehensive evaluated neutronic data file for elemental zirconium is derived and presented in the ENDF/B-VI formats. The derivation is based upon measured microscopic nuclear data, augmented by model calculations as necessary. The primary objective is a quality contemporary file suitable for fission-reactor development extending from conventional thermal to fast and innovative systems. This new file is a significant improvement over previously available evaluated zirconium files, in part, as a consequence of extensive new experimental measurements reported elsewhere

  7. Polymer-Derived Silicoboron Carbonitride Foams for CO2 Capture: From Design to Application as Scaffolds for the in Situ Growth of Metal-Organic Frameworks.

    Science.gov (United States)

    Sandra, Fabien; Depardieu, Martin; Mouline, Zineb; Vignoles, Gérard L; Iwamoto, Yuji; Miele, Philippe; Backov, Rénal; Bernard, Samuel

    2016-06-06

    A template-assisted polymer-derived ceramic route is investigated for preparing a series of silicoboron carbonitride (Si/B/C/N) foams with a hierarchical pore size distribution and tailorable interconnected porosity. A boron-modified polycarbosilazane was selected to impregnate monolithic silica and carbonaceous templates and form after pyrolysis and template removal Si/B/C/N foams. By changing the hard template nature and controlling the quantity of polymer to be impregnated, controlled micropore/macropore distributions with mesoscopic cell windows are generated. Specific surface areas from 29 to 239 m(2)  g(-1) and porosities from 51 to 77 % are achieved. These foams combine a low density with a thermal insulation and a relatively good thermostructural stability. Their particular structure allowed the in situ growth of metal-organic frameworks (MOFs) directly within the open-cell structure. MOFs offered a microporosity feature to the resulting Si/B/C/N@MOF composite foams that allowed increasing the specific surface area to provide CO2 uptake of 2.2 %. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Influence of carbon on structure stability, mechanical and tribological properties of β-Si3(Cx,N1‑x)4 silicon carbonitride

    Science.gov (United States)

    Zhong, Jing; Hua, Guomin; Chen, Linbo; Li, Changsheng; Yang, Jianhong; Cheng, Xiaonong

    2018-05-01

    In this study, β-Si3(Cx,N1‑x)4 Silicon Carbonitride was prepared by Self-Propagation High-Temperature Synthesis (SHS). And the influence of carbon on structure stability, mechanical and tribological properties of β-Si3(Cx,N1‑x)4 were investigated. The results showed that the solubility of carbon in β-Si3(Cx,N1‑x)4 was about 10 wt%, beyond which cubic-SiC segregated out of β-Si3(Cx,N1‑x)4 to form β-Si3N4/cubic-SiC composite. Regarding influences of carbon concentration on mechanical properties, the hardness of β-Si3(Cx,N1‑x)4 decreased from 1400 Hv to 1200 Hv with the increase of carbon concentration. Whereas, the fracture toughness of β-Si3(Cx,N1‑x)4 increased from 6.5 MPa · m0.5 to 7.6 MPa · m0.5 with the increase of carbon concentration. The tribological property studies revealed the anti-wear performance of β-Si3(Cx,N1‑x)4 was enhanced by the increase of carbon concentration. The dominated wear mechanism could be attributed to the abrasive wear by fracture.

  9. Antibacterial and Tribological Performance of Carbonitride Coatings Doped with W, Ti, Zr, or Cr Deposited on AISI 316L Stainless Steel

    Science.gov (United States)

    Yao, Sun-Hui; Su, Yen-Liang; Lai, Yu-Cheng

    2017-01-01

    Carbonitride (CNx) coatings have existed for several decades but are not well understood. Related studies have indicated that CNx coatings exhibit behaviors comparable to diamond-like carbon (DLC) coatings. Metal-doped CNx coatings are expected to show superior performance to single CNx coatings. In this study, a CNx coating and a group of CNx coatings with 6 at. % metal doping (W, Ti, Zr, or Cr) were prepared on biograde AISI 316L stainless steel (SS316L) substrates, and they were then characterized and studied for antibacterial and wear performance. The microstructure, constituent phase, nanohardness, adhesion, surface roughness, and contact angle were evaluated. The antimicrobial test used Staphylococcus aureus and followed the Japanese Industrial Standard JIS Z 2801:2010. Finally, the wear behavior was assessed. The results showed that the CNx coating was a composite of amorphous CNx and amorphous C structures. The metal doping caused crystalline metal carbides/nitrides to form in the CNx coatings, which weakened their overall integrity. All the coatings showed antimicrobial ability for the SS316L samples. The CNx-Zr coating, the surface of which had the highest hydrophilicity, produced the best antibacterial performance. However, the CNx-Zr coating showed lower wear resistance than the CNx-W and CNx-Ti coatings. The CNx-Ti coating with a highly hydrophilic surface exhibited the lowest antibacterial ability. PMID:29039782

  10. Antibacterial and Tribological Performance of Carbonitride Coatings Doped with W, Ti, Zr, or Cr Deposited on AISI 316L Stainless Steel

    Directory of Open Access Journals (Sweden)

    Sun-Hui Yao

    2017-10-01

    Full Text Available Carbonitride (CNx coatings have existed for several decades but are not well understood. Related studies have indicated that CNx coatings exhibit behaviors comparable to diamond-like carbon (DLC coatings. Metal-doped CNx coatings are expected to show superior performance to single CNx coatings. In this study, a CNx coating and a group of CNx coatings with 6 at. % metal doping (W, Ti, Zr, or Cr were prepared on biograde AISI 316L stainless steel (SS316L substrates, and they were then characterized and studied for antibacterial and wear performance. The microstructure, constituent phase, nanohardness, adhesion, surface roughness, and contact angle were evaluated. The antimicrobial test used Staphylococcus aureus and followed the Japanese Industrial Standard JIS Z 2801:2010. Finally, the wear behavior was assessed. The results showed that the CNx coating was a composite of amorphous CNx and amorphous C structures. The metal doping caused crystalline metal carbides/nitrides to form in the CNx coatings, which weakened their overall integrity. All the coatings showed antimicrobial ability for the SS316L samples. The CNx-Zr coating, the surface of which had the highest hydrophilicity, produced the best antibacterial performance. However, the CNx-Zr coating showed lower wear resistance than the CNx-W and CNx-Ti coatings. The CNx-Ti coating with a highly hydrophilic surface exhibited the lowest antibacterial ability.

  11. Quercetin as colorimetric reagent for determination of zirconium

    Science.gov (United States)

    Grimaldi, F.S.; White, C.E.

    1953-01-01

    Methods described in the literature for the determination of zirconium are generally designed for relatively large amounts of this element. A good procedure using colorimetric reagent for the determination of trace amounts is desirable. Quercetin has been found to yield a sensitive color reaction with zirconium suitable for the determination of from 0.1 to 50?? of zirconium dioxide. The procedure developed involves the separation of zirconium from interfering elements by precipitation with p-dimethylaminoazophenylarsonic acid prior to its estimation with quercetin. The quercetin reaction is carried out in 0.5N hydrochloric acid solution. Under the operating conditions it is indicated that quercetin forms a 2 to 1 complex with zirconium; however, a 2 to 1 and a 1 to 1 complex can coexist under special conditions. Approximate values for the equilibrium constants of the complexes are K1 = 0.33 ?? 10-5 and K2 = 1.3 ?? 10-9. Seven Bureau of Standards samples of glass sands and refractories were analyzed with excellent results. The method described should find considerable application in the analysis of minerals and other materials for macro as well as micro amounts of zirconium.

  12. Low cycle fatigue behaviour of zirconium alloys at 3000C

    International Nuclear Information System (INIS)

    Hosbons, R.R.

    1975-01-01

    The low cycle fatigue lives of two zirconium alloys, zirconium-2.5 wt% niobium and zirconium-1.1 wt% chronium-0.1 wt% iron, have been determined at 300 0 C. Both annealed material and cold-worked and stress-relieved material have similar fatigue lives to annealed Zircaloy-2 but β-quenched zirconium-niobium and zirconium-chromium-iron have lower fatigue lives than annealed Zircaloy-2. An atmosphere containing a concentration of iodine lower than that required for stress corrosion cracking still significantly lowers the fatigue life. A mathematical relationship between fatigue life and short-term tensile properties was used to estimate the fatigue life of zirconium alloy fuel sheaths and it was estimated that for a strain cycle of 0.1 per cent a cyclic frequency exceeding 0.116 Hz (10 000 cycles/day) would be required to cause fatigue failure of the sheath before its design life is realized. (author)

  13. Low cycle fatigue behaviour of zirconium alloys at 3000C

    International Nuclear Information System (INIS)

    Hosbons, R.R.

    1975-01-01

    The low cycle fatigue lives of two zirconium alloys, zirconium--2.5 wt percent niobium and zirconium--1.1 wt percent chromium--0.1 wt percent iron, have been determined at 300 0 C. Both annealed material and cold-worked and stress-relieved material have similar fatigue lives to annealed Zircaloy-2 but β-quenched zirconium--niobium and zirconium--chromium--iron have lower fatigue lives than annealed Zircaloy-2. An atmosphere containing a concentration of iodine lower than that required for stress corrosion cracking still significantly lowers the fatigue life. A mathematical relationship between fatigue life and short-term tensile properties was used to estimate the fatigue life of zirconium alloy fuel sheaths and it was estimated that for a strain cycle of 0.1 percent a cyclic frequency exceeding 0.116 Hz (10,000 cycles/ day) would be required to cause fatigue failure of the sheath before its design life is realized

  14. 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

  15. Nanostructured zirconium titanate fibers prepared by particulate sol–gel and cellulose templating techniques

    Energy Technology Data Exchange (ETDEWEB)

    Rouhani, P. [Helmerich Advanced Technology Research Center, School of Electrical and Computer Engineering, Oklahoma State University, OK 74106 (United States); Salahinejad, E. [Helmerich Advanced Technology Research Center, School of Material Science and Engineering, Oklahoma State University, OK 74106 (United States); Department of Materials Science and Engineering, School of Engineering, Shiraz University, Zand Blvd., 7134851154 Shiraz (Iran, Islamic Republic of); Kaul, R. [Department of Biochemistry and Microbiology, Center for Health Sciences, Oklahoma State University, OK 74107 (United States); Vashaee, D. [Helmerich Advanced Technology Research Center, School of Electrical and Computer Engineering, Oklahoma State University, OK 74106 (United States); Tayebi, L., E-mail: lobat.tayebi@okstate.edu [Helmerich Advanced Technology Research Center, School of Material Science and Engineering, Oklahoma State University, OK 74106 (United States); School of Chemical Engineering, Oklahoma State University, Stillwater, OK 74078 (United States)

    2013-08-15

    Highlights: •A method to produce zirconium titanate fibers was introduced. •The resultant structure and photocatalytic activity of the fiber were investigated. •The fiber exhibited higher photocatalytic characteristics, compared with the powders. -- Abstract: In this paper, a method for cost-effective production of nanostructured zirconium titanate (ZrTiO{sub 4}) fibers is introduced. In this method, ZrTiO{sub 4} fibers were synthesized by a sol–gel technique using cellulose fibers as the template. The resultant structures were studied by transmission electron microscopy, X-ray diffraction, scanning electron microscopy, and Brunauer–Emmett–Teller (BET) analyses. The photocatalytic activity of the fiber was compared to that of ZrTiO{sub 4} powders prepared by the same sol–gel method, in dark and under UVA and UVC radiations. According to the results, after calcination accompanied by the template removal, the ZrTiO{sub 4} fiber consists of uniformly-deposited, crystalline nanoparticles. This nanostructured fiber exhibited a higher surface area and a higher porosity compared with the ZrTiO{sub 4} powders, resulting in considerably higher photocatalytic characteristics, as confirmed by the experiment. The large surface area and the enhanced photocatalytic activity of the ZrTiO{sub 4} fibers also offer applications in sensors and bioactive films.

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

    Science.gov (United States)

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

    2014-04-01

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

  17. 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

  18. Understanding the Irradiation Behavior of Zirconium Carbide

    International Nuclear Information System (INIS)

    Motta, Arthur; Sridharan, Kumar; Morgan, Dane; Szlufarska, Izabela

    2013-01-01

    Zirconium carbide (ZrC) is being considered for utilization in high-temperature gas-cooled reactor fuels in deep-burn TRISO fuel. Zirconium carbide possesses a cubic B1-type crystal structure with a high melting point, exceptional hardness, and good thermal and electrical conductivities. The use of ZrC as part of the TRISO fuel requires a thorough understanding of its irradiation response. However, the radiation effects on ZrC are still poorly understood. The majority of the existing research is focused on the radiation damage phenomena at higher temperatures (>450ee)C) where many fundamental aspects of defect production and kinetics cannot be easily distinguished. Little is known about basic defect formation, clustering, and evolution of ZrC under irradiation, although some atomistic simulation and phenomenological studies have been performed. Such detailed information is needed to construct a model describing the microstructural evolution in fast-neutron irradiated materials that will be of great technological importance for the development of ZrC-based fuel. The goal of the proposed project is to gain fundamental understanding of the radiation-induced defect formation in zirconium carbide and irradiation response by using a combination of state-of-the-art experimental methods and atomistic modeling. This project will combine (1) in situ ion irradiation at a specialized facility at a national laboratory, (2) controlled temperature proton irradiation on bulk samples, and (3) atomistic modeling to gain a fundamental understanding of defect formation in ZrC. The proposed project will cover the irradiation temperatures from cryogenic temperature to as high as 800ee)C, and dose ranges from 0.1 to 100 dpa. The examination of this wide range of temperatures and doses allows us to obtain an experimental data set that can be effectively used to exercise and benchmark the computer calculations of defect properties. Combining the examination of radiation

  19. Study of some properties of zirconium phosphate; Etude de quelques proprietes du phosphate de zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Prospert, J [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    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{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Tests with columns showed that Na{sup +} and K{sup +} were easily separable, as was the Rb{sup +}-Cs{sup +} mixture, this last pair being fairly difficult to dissociate. (author) [French] Le phosphate de zirconium a ete etudie en vue de son utilisation comme echangeur d'ions: le premier but a atteindre a ete de mettre au point une preparation pouvant se reveler facilement utilisable ainsi qu'aisement reproductible. A cet effet, plusieurs essais ont ete effectues en faisant varier les rapports molaires du phosphore et du zirconium. Quelques proprietes physiques, telle la diffraction des rayons X, ont ete abordees. Ensuite, l'etude a porte sur certaines proprietes chimiques, particulierement les pourcentages d'eau libre et d'eau de structure par des pertes au feu, utilisation de la methode de Karl-Fisher, ainsi que des pertes de poids a la thenmobalance. Enfin, on a tente d'utiliser l'echangeur a la separation des ions alcalins. Les etudes statiques ont permis de constater que l'ordre de fixation de ces ions etait Cs{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Les essais effectues en colonne ont montre que Na{sup +} et K{sup +} etaient aisement separables entre eux, ainsi que du couple Rb{sup +}-Cs{sup +}, ce

  20. Process and operating device for an apparatus using a running liquid film and application to separation of Zr and Hf tetrachlorides

    International Nuclear Information System (INIS)

    Brun, R.

    1989-01-01

    A process is claimed allowing to maintain a thin film in a running film exchanger, by increasing the flow rate for a short time to establish a film all over the surface. Application is made to continuous condensation of zirconium and hafnium tetrachlorides, from the separation column, by absorption in a liquid solvent made of potassium chloroaluminate [fr

  1. Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

    Directory of Open Access Journals (Sweden)

    R.V. Smotraiev

    2016-05-01

    Full Text Available The actual problem of water supply in the world and in Ukraine, in particular, is a high level of pollution in water resources and an insufficient level of drinking water purification. With industrial wastewater, a significant amount of pollutants falls into water bodies, including suspended particles, sulfates, iron compounds, heavy metals, etc. Aim: The aim of this work is to determine the impact of aluminum and manganese ions additives on surface and sorption properties of zirconium oxyhydroxide based sorbents during their production process. Materials and Methods: The sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were prepared by sol-gel method during the hydrolysis of metal chlorides (zirconium oxychloride ZrOCl2, aluminum chloride AlCl3 and manganese chloride MnCl2 with carbamide. Results: The surface and sorption properties of sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides were investigated. X-ray amorphous structure and evolved hydroxyl-hydrate cover mainly characterize the obtained xerogels. The composite sorbents based on xerogels of zirconium oxyhydroxide doped with aluminum oxyhydroxide (aS = 537 m2/g and manganese oxyhydroxide (aS = 356 m2/g have more developed specific surface area than single-component xerogels of zirconium oxyhydroxide (aS = 236 m2/g and aluminum oxyhydroxide (aS = 327 m2/g. The sorbent based on the xerogel of zirconium and manganese oxyhydroxides have the maximum SO42--ions sorption capacity. It absorbs 1.5 times more SO42–-ions than the industrial anion exchanger AN-221. The sorbents based on xerogels of zirconium oxyhydroxide has the sorption capacity of Fe3+-ions that is 1.5…2 times greater than the capacity of the industrial cation exchanger KU-2-8. The Na+-ions absorption capacity is 1.47…1.56 mmol/g for each sorbent. Conclusions: Based on these data it can be concluded that the proposed method is effective for sorbents production based on

  2. Irradiation creep in zirconium single crystals

    International Nuclear Information System (INIS)

    MacEwen, S.R.; Fidleris, V.

    1976-07-01

    Two identical single crystals of crystal bar zirconium have been creep tested in reactor. Both specimens were preirradiated at low stress to a dose of about 4 x 10 23 n/m 2 (E > 1 MeV), and were then loaded to 25 MPa. The first specimen was loaded with reactor at full power, the second during a shutdown. The loading strain for both crystals was more than an order of magnitude smaller than that observed when an identical unirradiated crystal was loaded to the same stress. Both crystals exhibited periods of primary creep, after which their creep rates reached nearly constant values when the reactor was at power. During shutdowns the creep rates decreased rapidly with time. Electron microscopy revealed that the irradiation damage consisted of prismatic dislocation loops, approximately 13.5 nm in diameter. Cleared channels, identified as lying on (1010) planes, were also observed. The results are discussed in terms of the current theories for flux enhanced creep in the light of the microstructures observed. (author)

  3. 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.

  4. 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.)

  5. Corrosion resistant zirconium alloys prepared by powder metallurgy

    International Nuclear Information System (INIS)

    Wojeik, C.C.

    1984-01-01

    Pure zirconium and zirconium 2.5% niobium were prepared by powder metallurgy. The powders were prepared directly from sponge and consolidated by cold isostatic pressing and sintering. Hot isostatic pressing was also used to obtain full density after sintering. For pure zirconium the effects of particle size, compaction pressure, sintering temperature and purity were investigated. Fully densified zirconium and Zr-2.5%Nb exhibited tensile properties comparable to cast material at room temperature and 300 0 F (149 0 C). Pressed and sintered material having density of 94-99% had slightly lower tensile properties. Corrosion tests were performed in boiling 65% H/sub 2/SO/sub 4/, 70% HNO/sub 3/, 20% HCl and 20% HCl + 500 ppm FeCl/sub 3/ (a known pitting solution). For fully dense material the observed corrosion behavior was nearly equivalent to cast material. A slightly higher rate of attack was observed for samples which were only 94-99% dense. Welding tests were also performed on zirconium and Zr-2.5%Nb alloy. Unlike P/M titanium alloys, these materials had good weldability due to the lower content of volatile impurities in the powder. A slight amount of weld porosity was observed but joint efficiencies were always not 100%, even for 94-99% density samples. Several practical applications of the P/M processed material will be briefly described

  6. Inhibition of Ice Growth and Recrystallization by Zirconium Acetate and Zirconium Acetate Hydroxide

    Science.gov (United States)

    Mizrahy, Ortal; Bar-Dolev, Maya; Guy, Shlomit; Braslavsky, Ido

    2013-01-01

    The control over ice crystal growth, melting, and shaping is important in a variety of fields, including cell and food preservation and ice templating for the production of composite materials. Control over ice growth remains a challenge in industry, and the demand for new cryoprotectants is high. Naturally occurring cryoprotectants, such as antifreeze proteins (AFPs), present one solution for modulating ice crystal growth; however, the production of AFPs is expensive and inefficient. These obstacles can be overcome by identifying synthetic substitutes with similar AFP properties. Zirconium acetate (ZRA) was recently found to induce the formation of hexagonal cavities in materials prepared by ice templating. Here, we continue this line of study and examine the effects of ZRA and a related compound, zirconium acetate hydroxide (ZRAH), on ice growth, shaping, and recrystallization. We found that the growth rate of ice crystals was significantly reduced in the presence of ZRA and ZRAH, and that solutions containing these compounds display a small degree of thermal hysteresis, depending on the solution pH. The compounds were found to inhibit recrystallization in a manner similar to that observed in the presence of AFPs. The favorable properties of ZRA and ZRAH suggest tremendous potential utility in industrial applications. PMID:23555701

  7. Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison

    Science.gov (United States)

    2015-06-05

    of any copyrighted material in the thesis manuscript entitled: Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison Is...Uniformed Services University Date: 02/20/2015 Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison By...the thesis manuscript entitled: Primary Stability of Zirconium vs Titanium Implants: An In Vitro Comparison Is appropriately acknowledged

  8. 40 CFR 721.10089 - Modified salicylic acid, zirconium complex (generic).

    Science.gov (United States)

    2010-07-01

    ... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Modified salicylic acid, zirconium... Specific Chemical Substances § 721.10089 Modified salicylic acid, zirconium complex (generic). (a) Chemical... as modified salicylic acid, zirconium complex (PMN P-00-552) is subject to reporting under this...

  9. 40 CFR 471.90 - Applicability; description of the zirconium-hafnium forming subcategory.

    Science.gov (United States)

    2010-07-01

    ... zirconium-hafnium forming subcategory. 471.90 Section 471.90 Protection of Environment ENVIRONMENTAL... POINT SOURCE CATEGORY Zirconium-Hafnium Forming Subcategory § 471.90 Applicability; description of the zirconium-hafnium forming subcategory. This subpart applies to discharges of pollutants to waters of the...

  10. 40 CFR 421.330 - Applicability: Description of the primary zirconium and hafnium subcategory.

    Science.gov (United States)

    2010-07-01

    ... primary zirconium and hafnium subcategory. 421.330 Section 421.330 Protection of Environment ENVIRONMENTAL... CATEGORY Primary Zirconium and Hafnium Subcategory § 421.330 Applicability: Description of the primary zirconium and hafnium subcategory. The provisions of this subpart are applicable to discharges resulting...

  11. 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.

  12. Zirconium behaviour during electrorefining of actinide-zirconium alloy in molten LiCl-KCl on aluminium cathodes

    Energy Technology Data Exchange (ETDEWEB)

    Meier, R. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Heidelberg University, Institute of Physical Chemistry, Im Neuenheimer Feld 253, Heidelberg 69120 (Germany); Souček, P., E-mail: Pavel.Soucek@ec.europa.eu [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Malmbeck, R.; Krachler, M.; Rodrigues, A.; Claux, B.; Glatz, J.-P. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Fanghänel, Th. [European Commission, Joint Research Centre (JRC), Institute for Transuranium Elements (ITU), Postfach 2340, Karlsruhe 76125 (Germany); Heidelberg University, Institute of Physical Chemistry, Im Neuenheimer Feld 253, Heidelberg 69120 (Germany)

    2016-04-15

    A pyrochemical electrorefining process for the recovery of actinides from metallic nuclear fuel based on actinide-zirconium alloys (An–Zr) in a molten salt is being investigated. In this process actinides are group-selectively recovered on solid aluminium cathodes as An–Al alloys using a LiCl–KCl eutectic melt at a temperature of 450 °C. In the present study the electrochemical behaviour of zirconium during electrorefining was investigated. The maximum amount of actinides that can be oxidised without anodic co-dissolution of zirconium was determined at a selected constant cathodic current density. The experiment consisted of three steps to assess the different stages of the electrorefining process, each of which employing a fresh aluminium cathode. The results indicate that almost a complete dissolution of the actinides without co-dissolution of zirconium is possible under the applied experimental conditions. - Highlights: • Recovery of actinides was shown by electrorefining of U/Pu–Zr alloys in LiCl–KCl. • Constant current density of 20 mA/cm{sup 2} is applied. • Most of the actinides were dissolved avoiding zirconium co-dissolution. • Deterioration of the deposit quality by a small amount of co-deposited Zr is not observed.

  13. A half-century of changes in zirconium alloys

    International Nuclear Information System (INIS)

    Mardon, J.P.; Barberis, P.; Hoffmann, P.B.

    2008-01-01

    This article presents the history of zirconium alloys for PWR and BWR technologies. For more than 20 years zirconium alloys have evolved to cope with demands of the reactor operators concerning the burn-up extension and new safety margins. The poor properties of Zircaloy-1 concerning corrosion have led researchers to add elements like iron by developing Zircaloy-3A and Zircaloy-3C, and resulting in Zircaloy-4 with tin addition (from 1.30% to 1.50%). Zircaloy-4 is now outdated for PWR and new zirconium alloys with niobium are used (M5, ZIRLO...) they present a better resistance to corrosion, to hydridation, to creep and they are less prone to dimensional changes under irradiation. (A.C.)

  14. 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

  15. Interrelationship between structure and corrosion behaviour of zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Guenther, T [Bayer A.G., Leverkusen (Germany, F.R.)

    1979-05-01

    Due to plant failures caused by the break-down of zirconium grade 702 subjected to sulphuric acid the structure and corrosion behaviour of welded and as delivered specimens were tested for various heat treatments. It was shown by structure investigations and electron microprobe analysis that the corrosion behaviour of zirconium (in boiling 65 pct sulphuric acid) is strongly infuenced by the structure, which in its turn is dependent on the grade of purity and the prehistory of the material. Type, amount, and distribution of residual elements or precipitations caused by them are responsible for the corrosion resistance. This is valid particularly for the element iron. The plant failures mentioned here coincided with the examination results. Measures to improve the chemical resistance of pure zirconium subjected to extremely aggressive media were derived.

  16. A new model for the in-reactor corrosion of zirconium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Cox, B [University of Toronto, ON (Canada). Centre for Nuclear Engineering

    1997-02-01

    Previous models for the in-reactor corrosion of zirconium alloys have assumed that the mechanism is a completely solid-state diffusion process, determined by the growth and breakdown of the protective oxide film. In-reactor kinetics have been related to out-reactor kinetics with the oxide-metal interface temperature calculated from effects of heat flux. Recent experimental results have suggested that oxide dissolution and reprecipitation may be a major process leading to the formation of thick porous oxide films in-reactor. The model described here is based on the dissolution of primary recoil tracks in the oxide as the primary process distinguishing in-reactor from out-reactor corrosion. The consequences of such a model would be a very different microscopic morphology of in-reactor and out-reactor thick films, a significant irradiation effect on non-heat transfer surfaces, and a change in the kinetics of the overall process. This model should be equally applicable to PWR and BWR water chemistries because of the amphoteric nature of ZrO{sub 2}, and the effects of LiOH should operate by an essentially identical mechanism. A reciprocal rate equation should fit these processes and with additive terms seems capable of accommodating all water chemistry effects, except for discontinuous processes such as nodular corrosion. (author). 60 refs, 6 figs.

  17. A new model for the in-reactor corrosion of zirconium alloys

    International Nuclear Information System (INIS)

    Cox, B.

    1997-01-01

    Previous models for the in-reactor corrosion of zirconium alloys have assumed that the mechanism is a completely solid-state diffusion process, determined by the growth and breakdown of the protective oxide film. In-reactor kinetics have been related to out-reactor kinetics with the oxide-metal interface temperature calculated from effects of heat flux. Recent experimental results have suggested that oxide dissolution and reprecipitation may be a major process leading to the formation of thick porous oxide films in-reactor. The model described here is based on the dissolution of primary recoil tracks in the oxide as the primary process distinguishing in-reactor from out-reactor corrosion. The consequences of such a model would be a very different microscopic morphology of in-reactor and out-reactor thick films, a significant irradiation effect on non-heat transfer surfaces, and a change in the kinetics of the overall process. This model should be equally applicable to PWR and BWR water chemistries because of the amphoteric nature of ZrO 2 , and the effects of LiOH should operate by an essentially identical mechanism. A reciprocal rate equation should fit these processes and with additive terms seems capable of accommodating all water chemistry effects, except for discontinuous processes such as nodular corrosion. (author). 60 refs, 6 figs

  18. Separation of zirconium from hafnium by ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Felipe, Elaine C.B.; Palhares, Hugo G.; Ladeira, Ana Claudia Q., E-mail: elainecfelipe@yahoo.com.br, E-mail: hugopalhares@gmail.com, E-mail: ana.ladeira@cdtn.br [Centro de Desenvolvimento da Tecnologia Nuclear (CDTN/CNEN-MG), Belo Horizonte, MG (Brazil)

    2013-07-01

    Zirconium and hafnium are two of the most important metals for the nuclear industry. Hafnium occurs in all zirconium ores usually in the range 2 - 3%. However, for the most nuclear industry applications, it is necessary to use a zirconium of extremely pure level. The current work consists in the separation of zirconium and hafnium by the ion exchange method in order to obtain a zirconium concentrate of high purity. The zirconium and hafnium liquors were produced from the leaching of the Zr(OH){sub 4} and Hf(OH){sub 4} with nitric acid for 24 hours. From these two liquors it was prepared one solution containing 7.5 x 10{sup -2} mol L{sup -1} of Zr and 5.8 x 10{sup -3} mol L{sup -1} of Hf with acidity of 1 M. Ion exchange experiments were carried out in batch with the resins Dowex 50WX4, Dowex 50WX8 100, Dowex 50WX8 50, Amberlite IR-120 and Marathon C at constant temperature 28 deg C. Other variables such as, acidity and agitation were kept constant. The data were adjusted to Langmuir equation in order to calculate the maximum loading capacity (q{sub max}) of the resins, the distribution coefficient (K{sub d}) for Zr and Hf and the separation factor (α{sub Hf}{sup Zr} ). The results of maximum loading capacity (q{sub max}) for Zr and Hf, in mmol g{sup -}1, showed that the most suitable resins for columns experiments are: Dowex 50WX4 50 (q{sub max} Z{sub r} = 2.21, Hf = 0.18), Dowex 50WX8 50 (q{sub max} Zr = 1.89, Hf = 0.13) and Amberlite (q{sub max} Zr = 1.64, Hf = 0.12). However, separations factors, α{sub Hf}{sup Zr}, showed that the resins are not selective. (author)

  19. On composition and thermal degradation of basic zirconium sulfates

    Energy Technology Data Exchange (ETDEWEB)

    Grizik, A A; Nekhamkin, L G; Kondrashova, I A; Serebrennikov, E L; Kerina, V P

    1988-02-01

    Methods of potentiometric titration, conductometry and thermal gravimetric analysis are used to study composition and properties of basic zirconium sulfates (BZS) obtained under different conditions of precipitation from aqueous solutions. Three X-ray amorphous phases of BZR with mole ratio SO/sub 4//sup 2-/:Zr, being 0.60+-0.03; 0.37+-0.04 and 0.176+-0.005, are identified. Different character of thermal decomposition of these phases in the process of zirconium dioxide preparation from BZS is confirmed.

  20. On composition and thermal degradation of basic zirconium sulfates

    International Nuclear Information System (INIS)

    Grizik, A.A.; Nekhamkin, L.G.; Kondrashova, I.A.; Serebrennikov, E.L.; Kerina, V.P.

    1988-01-01

    Methods of potentiometric titration, conductometry and thermal gravimetric analysis are used to study composition and properties of basic zirconium sulfates (BZS) obtained under different conditions of precipitation from aqueous solutions. Three X-ray amorphous phases of BZR with mole ratio SO 4 2- :Zr, being 0.60±0.03; 0.37±0.04 and 0.176±0.005, are identified. Different character of thermal decomposition of these phases in the process of zirconium dioxide preparation from BZS is confirmed

  1. In-situ stabilization of radioactive zirconium swarf

    Science.gov (United States)

    Hess, Clay C.

    1999-01-01

    The method for treating ignitable cutting swarf in accordance with the present invention involves collecting cutting swarf in a casting mold underwater and injecting a binder mixture comprising vinyl ester styrene into the vessel to fill void volume; and form a mixture comprising swarf and vinyl ester styrene; and curing the mixture. The method is especially useful for stabilizing the ignitable characteristics of radioactive zirconium cutting swarf, and can be used to solidify zirconium swarf, or other ignitable finely divided material, underwater. The process could also be performed out of water with other particulate wastes.

  2. Temperature dependence of lattice parameters of alpha-zirconium

    International Nuclear Information System (INIS)

    Versaci, R.A.; Ipohorski, M.

    1991-01-01

    This work presents a brief review of X-ray and thermal expansion determination of lattice parameters for α-Zirconium. Data reported by different authors cover almost all the field of existence of the hexagonal phase of Zirconium, from temperatures as low as 4.2 K up to about 1130 K, near the α→β transformation temperature. Polynomial expressions based on a least squares fitting of experimental data are also presented. The expressions obtained by Goldak et al. are considered to be the most complete. The influence of impurities on the lattice parameters is also discussed. (Author) [es

  3. On the mechanism of ion exchange in zirconium phosphates

    International Nuclear Information System (INIS)

    Clearfield, A.; Kalnins, J.M.

    1978-01-01

    The exchange of transition metal (M 2+ ) ions from manganese through cobalt, nickel, copper to zinc with γ-zirconium phosphate was examined. By using acetate salts the hydrogen ion concentration is kept low enough to achieve high loadings. The fully loaded solids have the composition ZrM(PO 4 ) 2 .4H 2 O. Near quantitative uptakes are achieved at 100 0 C. The interlayer spacings change very little with loading indicating that γ-zirconium phosphate is able to accommodate cations and water molecules without appreciable increase in volume. The copper exchanged phase readily forms an acetylacetonate when shaken with 2,4-pentanedione. (author)

  4. 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)

  5. 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)

  6. Pressure of saturated vapor of yttrium and zirconium acetylacetonates

    Energy Technology Data Exchange (ETDEWEB)

    Trembovetskij, G.V.; Berdonosov, S.S.; Murav' eva, I.A.; Martynenko, L.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1984-08-01

    The static method and the flow method using /sup 91/Y and /sup 95/Zr radioactive indicators have been applied to determine pressure of saturated vapour of yttrium and zirconium acetylacetonates. Values of thermodynamic functions ..delta..Hsub(subl)=(98+-16)kJ/mol and ..delta..Ssub(subl.)=(155+-30)J/mol x K are calculated for sublimation of yttrium acetylacetonate. For sublimation of zirconium acetylacetonates ..delta..Hsub(subl) equals (116+-38) kJ/mol and ..delta..Ssub(subl) is equal to (198+-65) J/molxK.

  7. Identification of the zirconium hydrides metallography in zircaloy-2

    International Nuclear Information System (INIS)

    Garcia Gonzalez, F.

    1968-01-01

    Technique for the Identification of the zirconium hydrides in metallographic specimens have been developed. Microhardness, quantitative estimation and relative orientation of the present hydrides as well as grain size determination of the different Zircaloy-2 tube specimens have also been made. The specimens used were corrosion- tested in water during various periods of time at 300 degree castrating, prior to the metallographic examination. Reference specimens, as received, and heavily hydride specimens in a hydrogen atmosphere at 800 degree centigrees, have been used in the previous stages of the work. No difficulties have been met in this early stage of acquaintanceship with the zirconium hydrides. (Author) 5 refs

  8. Peculiarities of formation of zirconium aluminides in hydride cycle mode

    International Nuclear Information System (INIS)

    Muradyan, G.N.

    2016-01-01

    The zirconium aluminides are promising structural materials in aerospace, mechanical engineering, chemical industry, etc. They are promising for manufacturing of heat-resistant wires, that will improve the reliability and efficiency of electrical networks. In the present work, the results of study of zirconium aluminides formation in the Hydride Cycle (HC) mode, developed in the Laboratory of high-temperature synthesis of the Institute of Chemical Physics of NAS RA, are described. The formation of zirconium aluminides in HC proceeded according to the reaction xZrH_2+(1-x)Al → alloy Zr_xAl(1-x)+H_2↑. The samples were certified using: chemical analysis to determine the content of hydrogen (pyrolysis method); differential thermal analysis (DTA, derivatograph Q-1500, T_heating = 1000°C, rate 20°C/min); X-ray analysis (XRD, diffractometer DRON-0.5). The influences of the ratio of powders ZrH_2/Al in the reaction mixture, compacting pressure, temperature and heating velocity on the characteristics of the synthesized aluminides were determined. In HC, the solid solutions of Al in Zr, single phase ZrAl_2 and ZrAl_3 aluminides and Zr_3AlH_4.49 hydride were synthesized. Formation of aluminides in HC mode took place by the solid-phase mechanism, without melting of aluminum. During processing, the heating of the initial charge up to 540°C resulted in the decomposition of zirconium hydride (ZrH_2) to HCC ZrH_1.5, that interacted with aluminum at 630°C forming FCC alumohydride of zirconium. Further increase of the temperature up to 800°C led to complete decomposition of the formed alumohydride of zirconium. The final formation of the zirconium aluminide occurred at 1000-1100°C in the end of HC process. Conclusion: in the synthesis of zirconium aluminides, the HC mode has several significant advantages over the conventional modes: lower operating temperatures (1000°C instead of 1800°C); shorter duration (1.5-2 hours instead of tens of hours); the availability of

  9. Tracing of salicylic acid additive during precipitation of zirconium

    International Nuclear Information System (INIS)

    Bharati Misra, U.; Gopala Krishna, K.; Narasimha Murty, B.; Yadav, R.B.

    2011-01-01

    This paper presents the results of experimental study carried out to know whether the salicylic acid used as an additive during the precipitation of zirconium using ammonium hydroxide solution goes into the filtrate, remains in the hydrated zirconia or gets distributed between the both under the ambient conditions of precipitation. Keeping its simplicity and amenability to adopt on a routine basis, spectrophotometric method has been chosen for the purpose among the many methods available and the problems associated in determining salicylic acid in the presence of zirconium and the medial measures to circumvent the same have been brought out in detail. (author)

  10. High temperature evaporation of titanium, zirconium and hafnium carbides

    International Nuclear Information System (INIS)

    Gusev, A.I.; Rempel', A.A.

    1991-01-01

    Evaporation of cubic nonstoichiometric carbides of titanium, zirconium and hafnium in a comparatively low-temperature interval (1800-2700) with detailed crystallochemical sample certification is studied. Titanium carbide is characterized by the maximum evaporation rate: at T>2300 K it loses 3% of sample mass during an hour and at T>2400 K titanium carbide evaporation becomes extremely rapid. Zirconium and hafnium carbide evaporation rates are several times lower than titanium carbide evaporation rates at similar temperatures. Partial pressures of metals and carbon over the carbides studied are calculated on the base of evaporation rates

  11. Photometric determination of yttrium in zirconium-containing materials

    International Nuclear Information System (INIS)

    Barbina, T.M.; Polezhaev, Yu.M.

    1984-01-01

    Comparative evaluation of the effect of different ways of eliminating the zirconium interfering effect on the results of yttrium photometric determination with arsenazo 2 in artificial mixtures of Y 2 O 3 and ZrO 2 , containing 5 and 10 mol.% Y 2 O 3 , has been carried out. The effect of Zr is eliminated by means of its precipitation by ammonium solution in the form of hydroxide and using camouflaging with 25% sulfosalicylic acid. Both ways do not provide a correct enough result. The use of non-reagent thermohydrolytic Zr precipitation during the analysis of zirconium-containing materials permits to obtain correct and well-reproducible results

  12. Heavy Ion Irradiation Effects in Zirconium Nitride

    International Nuclear Information System (INIS)

    Egeland, G.W.; Bond, G.M.; Valdez, J.A.; Swadener, J.G.; McClellan, K.J.; Maloy, S.A.; Sickafus, K.E.; Oliver, B.

    2004-01-01

    Polycrystalline zirconium nitride (ZrN) samples were irradiated with He + , Kr ++ , and Xe ++ ions to high (>1.10 16 ions/cm 2 ) fluences at ∼100 K. Following ion irradiation, transmission electron microscopy (TEM) and grazing incidence X-ray diffraction (GIXRD) were used to analyze the microstructure and crystal structure of the post-irradiated material. For ion doses equivalent to approximately 200 displacements per atom (dpa), ZrN was found to resist any amorphization transformation, based on TEM observations. At very high displacement damage doses, GIXRD measurements revealed tetragonal splitting of some of the diffraction maxima (maxima which are associated with cubic ZrN prior to irradiation). In addition to TEM and GIXRD, mechanical property changes were characterized using nano-indentation. Nano-indentation revealed no change in elastic modulus of ZrN with increasing ion dose, while the hardness of the irradiated ZrN was found to increase significantly with ion dose. Finally, He + ion implanted ZrN samples were annealed to examine He gas retention properties of ZrN as a function of annealing temperature. He gas release was measured using a residual gas analysis (RGA) spectrometer. RGA measurements were performed on He-implanted ZrN samples and on ZrN samples that had also been irradiated with Xe ++ ions, in order to introduce high levels of displacive radiation damage into the matrix. He evolution studies revealed that ZrN samples with high levels of displacement damage due to Xe implantation, show a lower temperature threshold for He release than do pristine ZrN samples. (authors)

  13. Stainless steel-zirconium alloy waste forms

    International Nuclear Information System (INIS)

    McDeavitt, S.M.; Abraham, D.P.; Keiser, D.D. Jr.; Park, J.Y.

    1996-01-01

    An electrometallurgical treatment process has been developed by Argonne National Laboratory to convert various types of spent nuclear fuels into stable storage forms and waste forms for repository disposal. The first application of this process will be to treat spent fuel alloys from the Experimental Breeder Reactor-II. Three distinct product streams emanate from the electrorefining process: (1) refined uranium; (2) fission products and actinides extracted from the electrolyte salt that are processed into a mineral waste form; and (3) metallic wastes left behind at the completion of the electrorefining step. The third product stream (i.e., the metal waste stream) is the subject of this paper. The metal waste stream contains components of the chopped spent fuel that are unaffected by the electrorefining process because of their electrochemically ''noble'' nature; this includes the cladding hulls, noble metal fission products (NMFP), and, in specific cases, zirconium from metal fuel alloys. The selected method for the consolidation and stabilization of the metal waste stream is melting and casting into a uniform, corrosion-resistant alloy. The waste form casting process will be carried out in a controlled-atmosphere furnace at high temperatures with a molten salt flux. Spent fuels with both stainless steel and Zircaloy cladding are being evaluated for treatment; thus, stainless steel-rich and Zircaloy-rich waste forms are being developed. Although the primary disposition option for the actinides is the mineral waste form, the concept of incorporating the TRU-bearing product into the metal waste form has enough potential to warrant investigation

  14. Influence of zirconium ions on the sorption of carrier-free radiophosphate (32P)

    International Nuclear Information System (INIS)

    Friedmann, Ch.; Schoenfeld, T.

    1975-01-01

    In acid solutions the addition of zirconium ions largely affects the sorption of carrier-free radiophosphate on various materials. With some sorbents, such as diatomeceous earth, clay minerals or activated charcoal, the addition of small quantities of zirconium leads to a substantial increase of 32 P adsorption. On the other hand, important quantities of zirconium cause decrease of sorption. With alumina as an adsorbent, any addition of zirconium leads to reduced adsorption of radiophosphate. These phenomena are due to the formation of soluble zirconium-phosphate complex ions. (author)

  15. 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

  16. 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

  17. Effects of ion implantation on corrosion of zirconium and zirconium base alloys

    International Nuclear Information System (INIS)

    Zelenskij, V.F.; Petel'guzov, I.A.; Rekova, L.P.; Rodak, A.G.

    1989-01-01

    The influence of He and Ar ion bombardment on the corrosion of Zr and Zr-1%Nb and Zr-2.5%Nb alloys is investigated with the aims of finding the irradiation influence laws, obtaining the dependences of the effect of increasing the corrosiuon resistance on the type and dose of bombarding ions and of finding the conditions for the maximum effect. The prolonged corrosion test of specimens (3500 hours) have shown that the strongest effect is obtained for the irradiation with Ar ions up to the dose 1x10 16 ion/cm 2 . The kinetics of ion thermosorption after corrosion of irradiated materials is studied, the temperature threshold of implanted ion stability in zirconium and its alloys is found to be 400 deg C

  18. Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

    International Nuclear Information System (INIS)

    McLaughlin, D.F.

    1989-01-01

    This patent describes an improvement in a method for separating hafnium tetrachloride from zirconium tetrachloride where a complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride is prepared from zirconium-hafnium tetrachlorides and the complex of zirconium-hafnium tetrachlorides and phosphorus oxychloride 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 where a hafnium tetrachloride enriched stream is taken from the top of the column and a zirconium enriched tetrachloride stream is taken from the bottom of the column. The improvement comprising: prepurifying the zirconium-hafnium tetrachlorides, prior to preparation of the complex and introduction of the complex into a distillation column, to substantially eliminate iron chloride from the zirconium hafnium tetrachlorides, whereby buildup or iron chloride in the distillation column and in the reboiler is substantially eliminated and the column can be operated in a continuous, stable and efficient manner

  19. p-chlorophenol anchored onto zirconium tungstate

    Indian Academy of Sciences (India)

    Unknown

    framework host materials with organic guests (Ozin 1992) and thin film .... DT-30 thermal analyser at a heating rate of 10°C min 1. ..... for particular metal ions enables it to act as an efficient ... Dines M B and Digiacomo P M 1981 Inorg. Chem.

  20. Antimicrobial effects of silver zeolite, silver zirconium phosphate silicate and silver zirconium phosphate against oral microorganisms

    Institute of Scientific and Technical Information of China (English)

    Sirikamon Saengmee-anupharb; Toemsak Srikhirin; Boonyanit Thaweboon; Sroisiri Thaweboon; Taweechai Amornsakchai; Surachai Dechkunakorn; Theeralaksna Suddhasthira

    2013-01-01

    Objective: To evaluate the antimicrobial activities of silver inorganic materials, including silver zeolite (AgZ), silver zirconium phosphate silicate (AgZrPSi) and silver zirconium phosphate (AgZrP), against oral microorganisms. In line with this objective, the morphology and structure of each type of silver based powders were also investigated. Methods: The antimicrobial activities of AgZ, AgZrPSi and AgZrP were tested against Streptococcus mutans, Lactobacillus casei, Candidaalbicans and Staphylococcus aureus using disk diffusion assay as a screening test. The minimum inhibitory concentration (MIC) and minimum lethal concentration (MLC) were determined using the modified membrane method. Scanning electron microscope and X-ray diffraction were used to investigate the morphology and structure of these silver materials. Results: All forms of silver inorganic materials could inhibit the growth of all test microorganisms. The MIC of AgZ, AgZrPSi and AgZrP was 10.0 g/L whereas MLC ranged between 10.0-60.0 g/L. In terms of morphology and structure, AgZrPSi and AgZrP had smaller sized particles (1.5-3.0 µm) and more uniformly shaped than AgZ. Conclusions: Silver inorganic materials in the form of AgZ, AgZrPSi and AgZrP had antimicrobial effects against all test oral microorganisms and those activities may be influenced by the crystal structure of carriers. These results suggest that these silver materials may be useful metals applied to oral hygiene products to provide antimicrobial activity against oral infection.

  1. Irradiation behaviour of mixed uranium-plutonium carbides, nitrides and carbonitrides; Comportement a l'irradiation de carbures, nitrures et carbonitrures mixtes d'uranium et de plutonium

    Energy Technology Data Exchange (ETDEWEB)

    Mikailoff, H; Mustelier, J P; Bloch, J; Leclere, J; Hayet, L [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1967-07-01

    In the framework of the research program of fast reactor fuels two irradiation experiments have been carried out on mixed uranium-plutonium carbides, nitrides and carbo-nitrides. In the first experiment carried out with thermal neutrons, the fuel consisted of sintered pellets sheathed in a stainless steel can with a small gap filled with helium. There were three mixed mono-carbide samples and the maximum linear power was 715 W/cm. After a burn-up slightly lower than 20000 MW day/tonne, a swelling of the fuel which had ruptured the cans was observed. In the second experiment carried out in the BR2 reactor with epithermal neutrons, the samples consisted of sintered pellets sodium bonded in a stainless steel tube. There were three samples containing different fuels and the linear power varies between 1130 and 1820 W/cm. Post-irradiation examination after a maximal burn-up of 1550 MW day/tonne showed that the behaviour of the three fuel elements was satisfactory. (authors) [French] Dans le cadre du programme d'etude des conibustiles pour reacteurs rapides, on a realise deux experiences d'irradiation de carbures, nitrures et carbonitrures mixtes d'uranium et de plutonium. Dans la premiere experience, faite en neutrons thermiques, le combustible etait constitue de,pastilles frittees gainees dans un tube d'acier inoxydable avec un faible jeu rempli d'helium. Il y avait trois echantillons de monocarbures mixtes, et la puissance lineaire maximale etait de 715 W/cm. Apres un taux de combustion legerement inferieur a 20 000 MWj/t, on a observe un gonflement des combustible qui a provoque, la rupture des gaines. Pans la seconde experience, realisee dans le reacteur BR2 en neutrons epithermiques, les echantillons etaient constitues de pastilles frittees gainees dans un tube d'acier avec un joint sodium. Il y avait trois echantillons contenant des combustibles differents, et la puissance lineaire variait de 1130 a 1820 W/cm. Les examens apres irradiation a un taux maximal de

  2. Young's modulus of crystal bar zirconium and zirconium alloys (zircaloy-2, zircaloy-4, zirconium-2.5wt% niobium) to 1000 K

    International Nuclear Information System (INIS)

    Rosinger, H.E.; Ritchie, I.G.; Shillinglaw, A.J.

    1975-09-01

    This report contains experimentally determined data on the dynamic elastic moduli of zircaloy-2, zircaloy-4, zirconium-2.5wt% niobium and Marz grade crystal bar zirconium. Data on both the dynamic Young's moduli and shear moduli of the alloys have been measured at room temperature and Young's modulus as a function of temperature has been determined over the temperature range 300 K to 1000 K. In every case, Young's modulus decreases linearly with increasing temperature and is expressed by an empirical equation fitted to the data. Differences in Young's modulus values determined from specimens with longitudinal axes parallel and perpendicular to the rolling direction are small, as are the differences between Young's moduli determined from strip, bar stock and fuel sheathing. (author)

  3. Photodegradation of DMMP and CEES on zirconium doped titania nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Mattsson, A.; Lejon, C.; Štengl, Václav; Bakardjieva, Snejana; Opluštil, F.; Andersson, P.O.; Osterlund, L.

    2009-01-01

    Roč. 92, 3-4 (2009), s. 401-410 ISSN 0926-3373 Institutional research plan: CEZ:AV0Z40320502 Keywords : TiO2 * zirconium * photocatalysis Subject RIV: CA - Inorganic Chemistry Impact factor: 5.252, year: 2009

  4. Mechanical and irradiation properties of zirconium alloys irradiated in HANARO

    International Nuclear Information System (INIS)

    Kwon, Oh Hyun; Eom, Kyong Bo; Kim, Jae Ik; Suh, Jung Min; Jeon, Kyeong Lak

    2011-01-01

    These experimental studies are carried out to build a database for analyzing fuel performance in nuclear power plants. In particular, this study focuses on the mechanical and irradiation properties of three kinds of zirconium alloy (Alloy A, Alloy B and Alloy C) irradiated in the HANARO (High-flux Advanced Neutron Application Reactor), one of the leading multipurpose research reactors in the world. Yield strength and ultimate tensile strength were measured to determine the mechanical properties before and after irradiation, while irradiation growth was measured for the irradiation properties. The samples for irradiation testing are classified by texture. For the irradiation condition, all samples were wrapped into the capsule (07M-13N) and irradiated in the HANARO for about 100 days (E > 1.0 MeV, 1.1 10 21 n/cm 2 ). These tests and results indicate that the mechanical properties of zirconium alloys are similar whether unirradiated or irradiated. Alloy B has shown the highest yield strength and tensile strength properties compared to other alloys in irradiated condition. Even though each of the zirconium alloys has a different alloying content, this content does not seem to affect the mechanical properties under an unirradiated condition and low fluence. And all the alloys have shown the tendency to increase in yield strength and ultimate tensile strength. Transverse specimens of each of the zirconium alloys have a slightly lower irradiation growth tendency than longitudinal specimens. However, for clear analysis of texture effects, further testing under higher irradiation conditions is needed

  5. Mono- and binuclear complexes of low-valent zirconium

    NARCIS (Netherlands)

    Wielstra, IJtsen

    1990-01-01

    This thesis is a study on the synthesis and reactivity of low-valent zirconium. The investigation can be divided in two parts: the first describes the chemistry of mono-cyclopentadienyl Zr (II) complexes (Chapter II, III and IV), and the second describes some synthetic pathways successfully used for

  6. 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.

  7. 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

  8. Zirconium determination in rocks by solid-phase spectrophotometry

    International Nuclear Information System (INIS)

    Brykina, G.D.; Lebedeva, G.G.; Agapova, G.F.; AN SSSR, Moscow

    1990-01-01

    A method was developed for determination of zirconium in rocks by solid-phase spectrophotometry using AV-17x8-Cl anion exchanger modified with xylenol orange. Relative standard deviation at the level of (2-4.9)x10 -3 % ZrO 2 was about 0.245

  9. Synthesis and characterization of new zirconium 4-sulfophenylphosphonates

    Czech Academy of Sciences Publication Activity Database

    Zima, Vítězslav; Svoboda, Jan; Melánová, Klára; Beneš, L.; Casciola, M.; Sganappa, M.; Brus, Jiří; Trchová, Miroslava

    2010-01-01

    Roč. 181, č. 15-16 (2010), s. 705-713 ISSN 0167-2738 R&D Projects: GA AV ČR IAA400500602; GA ČR GA203/08/0208 Institutional research plan: CEZ:AV0Z40500505 Keywords : zirconium * phosphonate * infrared spectra Subject RIV: CA - Inorganic Chemistry Impact factor: 2.496, year: 2010

  10. The determination of zirconium by atomic absorption spectrophotometry

    International Nuclear Information System (INIS)

    Rodriguez, E.R.; Cunha, M.T.C. da

    1975-01-01

    The interference of iron in the determination of zirconium by atomic absorption spectrophotometry was studied. Attempts were made to emininate this interference by complexing the iron with EDTA, ascorbic acid and hydrazine; also by the addition of ammonium fluoride to the solution. Some experiments were carried out in order to explain the results obtained [pt

  11. High strength corrosion-resistant zirconium aluminum alloys

    International Nuclear Information System (INIS)

    Schulson, E.M.; Cameron, D.J.

    1976-01-01

    A zirconium-aluminum alloy is described possessing superior corrosion resistance and mechanical properties. This alloy, preferably 7.5-9.5 wt% aluminum, is cast, worked in the Zr(Al)-Zr 2 Al region, and annealed to a substantially continuous matrix of Zr 3 Al. (E.C.B.)

  12. Separation of zirconium and hafnium using paper distribution chromatography

    International Nuclear Information System (INIS)

    Lebedeva, G.G.; Viktorova, M.E.

    1981-01-01

    A method is suggested of chromatographic separation of zirconium and hafnium in a CCl 4 -tributyl phosphate system (1:9) containing KCl as a salting-out agent in 5 M HNO 3 at 28-30 deg C. Zr and Hf are deterfmined in articiial mixtures under optimal chromatography conditions using visual colorimetry [ru

  13. Growth and high pressure studies of zirconium sulphoselenide ...

    Indian Academy of Sciences (India)

    Growth and high pressure studies of zirconium sulphoselenide single ... tance was monitored in a Bridgman opposed anvil set-up up to 8 GPa pressure to identify .... The optical band gaps of the as-grown crystals were obtained by optical ab-.

  14. Microstructure of lead zirconium titanate (PZT) by electron microscopy

    International Nuclear Information System (INIS)

    Bursill, L.A.; Peng JuLin

    1989-01-01

    Transmission and high-resolution electron microscopy reveal the microtexture of lead zirconium titanate ceramics. Fine scale (≤ 500 Aangstroem) ferroelastic and ferroelectric twin domains, as well as dislocations were found in a complex texture. Correlations between stoichiometry, microstructure and piezoelectric properties are discussed. 6 refs., 3 figs

  15. Nitrogen annealing of zirconium or titanium metals and their alloys

    International Nuclear Information System (INIS)

    Eucken, C.M.

    1982-01-01

    A method is described of continuously nitrogen annealing zirconium and titanium metals and their alloys at temperatures at from 525 0 to 875 0 C for from 1/2 minute to 15 minutes. The examples include the annealing of Zircaloy-4. (U.K.)

  16. Diffusion model of delayed hydride cracking in zirconium alloys

    NARCIS (Netherlands)

    Shmakov, AA; Kalin, BA; Matvienko, YG; Singh, RN; De, PK

    2004-01-01

    We develop a method for the evaluation of the rate of delayed hydride cracking in zirconium alloys. The model is based on the stationary solution of the phenomenological diffusion equation and the detailed analysis of the distribution of hydrostatic stresses in the plane of a sharp tensile crack.

  17. Highly corrosion resistant zirconium based alloy for reactor structural material

    International Nuclear Information System (INIS)

    Ito, Yoichi.

    1996-01-01

    The alloy of the present invention is a zirconium based alloy comprising tin (Sn), chromium (Cr), nickel (Ni) and iron (Fe) in zirconium (Zr). The amount of silicon (Si) as an impurity is not more than 60ppm. It is preferred that Sn is from 0.9 to 1.5wt%, that of Cr is from 0.05 to 0.15wt%, and (Fe + Ni) is from 0.17 to 0.5wt%. If not less than 0.12wt% of Fe is added, resistance against nodular corrosion is improved. The upper limit of Fe is preferably 0.40wt% from a view point of uniform suppression for the corrosion. The nodular corrosion can be suppressed by reducing the amount of Si-rich deposition product in the zirconium based alloy. Accordingly, a highly corrosion resistant zirconium based alloy improved for the corrosion resistance of zircaloy-2 and usable for a fuel cladding tube of a BWR type reactor can be obtained. (I.N.)

  18. Mathematical modelling of zirconium salicylate solvent extraction process

    International Nuclear Information System (INIS)

    Smirnova, N.S.; Evseev, A.M.; Fadeeva, V.I.; Kochetkova, S.K.

    1979-01-01

    Mathematical modelling of equilibrium multicomponent physicochemical system at the extraction of zirconium salicylates by chloroform is carried out from HCl aqueous solutions at pH 0.5-4.7. Adequate models, comprising different molecular forms, corresponding to equilibrium phase composition are built

  19. Mathematical modelling of zirconium salicylate solvent extraction process

    Energy Technology Data Exchange (ETDEWEB)

    Smirnova, N S; Evseev, A M; Fadeeva, V I; Kochetkova, S K [Moskovskij Gosudarstvennyj Univ. (USSR)

    1979-11-01

    Mathematical modelling of equilibrium multicomponent physicochemical system at the extraction of zirconium salicylates by chloroform is carried out from HCl aqueous solutions at pH 0.5-4.7. Adequate models, comprising different molecular forms, corresponding to equilibrium phase composition are built.

  20. 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

  1. Corrosion resistance of zirconium oxynitride coatings deposited via DC unbalanced magnetron sputtering and spray pyrolysis-nitriding

    Energy Technology Data Exchange (ETDEWEB)

    Cubillos, G.I., E-mail: gcubillos@unal.edu.co [Department of Chemistry, Group of Materials and Chemical Processes, Universidad Nacional de Colombia, Av. Cra. 30 No 45-03, Bogotá (Colombia); Bethencourt, M., E-mail: manuel.bethencourt@uca.es [Department of Materials Science, Metallurgy Engineering and Inorganic Chemistry, International Campus of Excellence of the Sea - CEI-MAR, University of Cadiz, Avda. República Saharaui s/n, 11510 Puerto Real, Cádiz (Spain); Olaya, J.J., E-mail: jjolayaf@unal.edu.co [Faculty of Engineering, Group of Materials and Chemical Processes, Universidad Nacional de Colombia, Av. Cra. 30 No 45-03, Bogotá (Colombia)

    2015-02-01

    Highlights: • New ZrO{sub x}N{sub y} films were deposited on stainless steel 316L using PSY-N and UBMS. • ZrO{sub x}N{sub y} rhombohedral polycrystalline film grew with PSY-N. • Zr{sub 2}ON{sub 2} crystalline structures, mostly oriented along the (2 2 2) plane, grew with UBMS. • Layers improved corrosion behavior in NaCl media, especially those deposited by UBMS. - Abstract: ZrO{sub x}N{sub y}/ZrO{sub 2} thin films were deposited on stainless steel using two different methods: ultrasonic spray pyrolysis-nitriding (SPY-N) and the DC unbalanced magnetron sputtering technique (UBMS). Using the first method, ZrO{sub 2} was initially deposited and subsequently nitrided in an anhydrous ammonia atmosphere at 1023 K at atmospheric pressure. For UBMS, the film was deposited in an atmosphere of air/argon with a Φair/ΦAr flow ratio of 3.0. Structural analysis was carried out through X-ray diffraction (XRD), and morphological analysis was done through scanning electron microscopy (SEM) and atomic force microscopy (AFM). Chemical analysis was carried out using X-ray photoelectron spectroscopy (XPS). ZrO{sub x}N{sub y} rhombohedral polycrystalline film was produced with spray pyrolysis-nitriding, whereas using the UBMS technique, the oxynitride films grew with cubic Zr{sub 2}ON{sub 2} crystalline structures preferentially oriented along the (2 2 2) plane. Upon chemical analysis of the surface, the coatings exhibited spectral lines of Zr3d, O1s, and N1s, characteristic of zirconium oxynitride/zirconia. SEM analysis showed the homogeneity of the films, and AFM showed morphological differences according to the deposition technique of the coatings. Zirconium oxynitride films enhanced the stainless steel's resistance to corrosion using both techniques. The protective efficacy was evaluated using electrochemical techniques based on linear polarization (LP). The results indicated that the layers provide good resistance to corrosion when exposed to chloride

  2. Synthesis, Characterization and Antimicrobial Activity of Zirconium (IV) Complexes

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Shobhana; Jain, Asha; Saxena, Sanjiv [Univ. of Rajasthan, Jaipur (India)

    2012-08-15

    Heteroleptic complexes of zirconium (IV) derived from bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones of the general formula ZrLL' (where L'H{sub 2}=RCNH(C{sub 6}H{sub 4})SC : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R=-C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl(p) and L'H{sub 2}=R'C : (NOH)C : C(OH)N(C{sub 6}H{sub 5})N : CCH{sub 3}, R' = -CH{sub 2}CH{sub 3}, -C{sub 6}H{sub 5}, -C{sub 6}H{sub 4}Cl (p) were prepared by the reactions of zirconium tetrachloride with disodium salts of Schiff bases (L Na{sub 2}) and oximes of heterocyclic β-diketones (L' Na{sub 2}) in 1:1:1 molar ratio in dry refluxing THF. The structures of these monomeric zirconium (IV) complexes were elucidated with the help of elemental analysis, molecular weight measurements, spectroscopic (IR, NMR and mass) studies. A distorted trigonal bipyramidal geometry may be suggested for these heteroleptic zirconium (IV) complexes. The ligands (bulky Schiff base ligands containing a sulphur atom and oximes of heterocyclic β-diketones) and their heteroleptic complexes of zirconium (IV) were screened against A. flavus, P. aeruginesa and E. coli.

  3. 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.

  4. Shear Bond Strength of Orthodontic Brackets Bonded to Zirconium Crowns.

    Science.gov (United States)

    Mehmeti, Blerim; Azizi, Bleron; Kelmendi, Jeta; Iljazi-Shahiqi, Donika; Alar, Željko; Anić-Milošević, Sandra

    2017-06-01

    An increasing demand for esthetic restorations has resulted in an increased use of all-ceramic restorations, such as zirconium. However, one of the challenges the orthodontist must be willing to face is how to increase bond strength between the brackets and various ceramic restorations.Bond strength can beaffected bybracket type, by the material that bracketsaremade of, and their base surface design or retention mode. ​: A im: of this study was to perform a comparative analysis of the shear bond strength (SBS) of metallic and ceramic orthodontic brackets bonded to all-zirconium ceramic surfaces used for prosthetic restorations, and also to evaluate the fracture mode of these two types of orthodontic brackets. Twenty samples/semi-crowns of all-zirconium ceramic, on which orthodontic brackets were bonded, 10 metallic and 10 ceramic polycrystalline brackets, were prepared for this research. SBS has been testedby Universal Testing Machine, with a load applied using a knife edged rod moving at a fixed rate of 1 mm/min, until failure occurred. The force required to debond the brackets was recorded in Newton, then SBS was calculated to MPa. In addition, the samples were analyzed using a digital camera magnifier to determine Adhesive Remnant Index (ARI). Statistical data were processed using t-test, and the level of significance was set at α = 0.05. Higher shear bond strength values were observed in metallic brackets bonded to zirconium crowns compared tothoseof ceramic brackets, with a significant difference. During the test, two of the ceramic brackets were partially or totally damaged. Metallic brackets, compared to ceramic polycrystalline brackets, seemed tocreate stronger adhesion with all-zirconium surfaces due to their better retention mode. Also, ceramic brackets showed higher fragility during debonding.

  5. Synthesis and cathodoluminescence characterization of ZrO2:Er3+ films

    International Nuclear Information System (INIS)

    Martínez-Hernández, A.; Guzmán-Mendoza, J.; Rivera-Montalvo, T.; Sánchez-Guzmán, D.; Guzmán-Olguín, J.C.; García-Hipólito, M.; Falcony, C.

    2014-01-01

    Trivalent erbium doped zirconium oxide films were deposited by the ultrasonic spray pyrolysis technique. Films were deposited using zirconium tetrachloride octahydrate (ZrCl 4 O·8H 2 O) and erbium nitrate hexahydrate ((NO 3 ) 3 Er·6H 2 O) as precursors and deionized water as solvent. The dopant concentrations in the spray solution were 1, 3, 5, 10 and 15 at% in ratio to zirconium content. The films were deposited on corning glass substrates at different temperatures from 400 up to 550 °C. Films deposited at temperatures lower than 400 °C were amorphous, however, as substrate temperatures are increased, the ZrO 2 films presented a better crystallinity and showed a tetragonal phase. Cathodoluminescence (CL) emission spectra showed bands centred at 524, 544 and 655 nm associated with the electronic transition of Er 3+ . - Highlights: • The films of ZrO 2 :Er 3+ were obtained by spray pyrolysis. • Emission spectra of ZrO 2 :Er 3+ films were reported. • Cathodoluminescence of ZrO 2 :Er 3+ films was analyzed. • Cathodoluminescence of ZrO 2 :Er 3+ films showed strong dependence on substrate temperature and electron voltage

  6. 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.

  7. Wear and chemistry of zirconium-silicate, aluminium-silicate and zirconium-aluminium-silicate glasses in alkaline medium

    International Nuclear Information System (INIS)

    Rouse, C.G.; Lemos Guenaga, C.M. de

    1984-01-01

    A study of the chemical durability, in alkaline solutions, of zirconium silicate, aluminium silicate, zirconium/aluminium silicate glasses as a function of glass composition is carried out. The glasses were tested using standard DIN-52322 method, where the glass samples are prepared in small polished pieces and attacked for 3 hours in a 800 ml solution of 1N (NaOH + NA 2 CO 3 ) at 97 0 C. The results show that the presence of ZrO 2 in the glass composition increases its chemical durability to alkaline attack. Glasses of the aluminium/zirconium silicate series were melted with and without TiO 2 . It was shown experimentally that for this series of glasses, the presence of both TiO 2 and ZrO 2 gave better chemical durability results. However, the best overall results were obtained from the simpler zirconium silicate glasses, where it was possible to make glasses with higher values of ZrO 2 . (Author) [pt

  8. Materials properties of hafnium and zirconium silicates: Metal interdiffusion and dopant penetration studies

    Science.gov (United States)

    Quevedo Lopez, Manuel Angel

    Hafnium and Zirconium based gate dielectrics are considered potential candidates to replace SiO2 or SiON as the gate dielectric in CMOS processing. Furthermore, the addition of nitrogen into this pseudo-binary alloy has been shown to improve their thermal stability, electrical properties, and reduce dopant penetration. Because CMOS processing requires high temperature anneals (up to 1050°C), it is important to understand the diffusion properties of any metal associated with the gate dielectric in silicon at these temperatures. In addition, dopant penetration from the doped polysilicon gate into the Si channel at these temperatures must also be studied. Impurity outdiffusion (Hf, Zr) from the dielectric, or dopant (B, As, P) penetration through the dielectric into the channel region would likely result in deleterious effects upon the carrier mobility. In this dissertation extensive thermal stability studies of alternate gate dielectric candidates ZrSixOy and HfSixO y are presented. Dopant penetration studies from doped-polysilicon through HfSixOy and HfSixOyNz are also presented. Rutherford Backscattering Spectroscopy (RBS), Heavy Ion RBS (HI-RBS), X-ray Photoelectron Spectroscopy (XPS), High Resolution Transmission Electron Microscopy (HR-TEM), and Time of Flight and Dynamic Secondary Ion Mass Spectroscopy (ToF-SIMS, D-SIMS) methods were used to characterize these materials. The dopant diffusivity is calculated by modeling of the dopant profiles in the Si substrate. In this disseration is reported that Hf silicate films are more stable than Zr silicate films, from the metal interdiffusion point of view. On the other hand, dopant (B, As, and P) penetration is observed for HfSixO y films. However, the addition of nitrogen to the Hf - Si - O systems improves the dopant penetration properties of the resulting HfSi xOyNz films.

  9. Lithium uptake and the corrosion of zirconium alloys in aqueous lithium hydroxide solutions

    International Nuclear Information System (INIS)

    Ramasubramanian, N.

    1991-01-01

    This paper reports on corrosion films on zirconium alloys that were analyzed for lithium by Atomic Absorption Spectroscopy (AAS), Secondary Ion Mass Spectrometry (SIMS), and Infrared Reflection Absorption Spectroscopy (IRAS). The oxides grown in reactor in dilute lithium hydroxide solution, specimens cut from Zircaloy, and Zr-2.5Nb alloy pressure tubes removed from CANDU (Canada Deuterium Uranium, Registered Trademark) reactors showed low concentrations of lithium (4 to 50 ppm). The lithium was not leachable in a warm dilute acid. 6 Li undergoes transmutation by the 6 Li(n,t) 4 He reaction. However, SIMS profiles for d 7 Li were identical through the bulk oxide and the isotopic ratio was close to the natural abundance value. The lithium in the oxide, existing as adsorbed lithium on the surface, has been in dynamic equilibrium with lithium in the coolant, and, in spite of many Effective Full Power Years (EFPY) of operation, lithium added to the CANDU coolant at ∼2.5 ppm is not concentrating in the oxides. On the other hand, corrosion films grown in the laboratory in concentrated lithium hydroxide solutions were very porous and contained hundreds of ppm of lithium in the oxide

  10. Diffusion in the plutonium zirconium system; Diffusion dans le systeme plutonium zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Lauthier, J C [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    1967-01-15

    Research on the compound PuZr{sub 2}: It cannot be obtained by a direct synthesis. We suppose that its formation is due to an oxygen amount which enhances diffusion processes by a contribution of bound extrinsic vacancies. This investigation which concerned a great range of alloys (from 15 to 50 at per cent Pu) has led us to point out the nature of the isothermal transformation. It takes place at 615 deg. + 5 deg. C and is of the peritectoid type. Pu {epsilon} (bcc) + Zr {alpha} (hex) {r_reversible} Pu {delta} (f. cc) Diffusion in hexagonal phase: Diffusion coefficients have been determined from couples made of Pu Zr dilute alloys (1.15 and 0.115 at per cent Pu) and of pure zirconium; these couples have been annealed between 700 and 840 deg. C from 1000 to 3000 hours. The curves C = f(x) were plotted by X ray microanalysis and a autoradiography. They have been analysed assuming that the diffusion coefficient was constant. Our results are the following: D Zr Pu (1.15 % = 11.1 exp (-65000/RT) and D Zr Pu (0.115 %) 0.1 exp (-54000/RT). (author) [French] Recherche du compose PuZr2: II ne peut etre obtenu par synthese directe. Nous pensons que sa formation est liee a la presence d'oxygene, qui, par son apport de lacunes extrinseques accelere les processus de diffusion. Cette etude qui a porte sur toute une serie d'alliages (de 15 a 50 pour cent atomique de Pu), nous a permis de preciser la nafure de la transformation isotherme. Elle situe a 615 deg. + 5 deg. C et est du type peritectoide. Pu {epsilon} (c.c.) + Zr {alpha} (h.c.) {r_reversible} Pu {delta} (c.f.c.) Diffusion en phase {alpha} hexagonale: Les coefficients de diffusion chimique ont ete determines a partir de couples constitues d'alliages PuZr dilues (1,15 pour cent et 0,115 pour cent atomique de Pu) et de zirconium pur. Ces couples ont ete recuits entre 700 et 840 deg. C durant des temps de 1000 a 3000 heures. Les courbes C = f(x) ont ete tracees par microanalyse X et autoradiographie {alpha}. Elles ont ete

  11. Pitting corrosion of zirconium in aqueous solution

    International Nuclear Information System (INIS)

    El Shayeb, H.A.; Abd El Wahab, F.M.; Abd Elk Meguid, E.A.

    1994-01-01

    The open circuit potentials of the Zr electrode are followed as a function of time in various aqueous solutions till attainment of steady state values.The results are discussed on the basis of oxide film thickening and repair. Pitting corrosion of Zr was examined in chloride solutions using the potentiodynamic technique. The effect of some inorganic and organic additives was also investigated for inhibiting the pitting corrosion of Zr and the relative performance is presented and discussed. (author). 21 refs., 6 figs., 1 tab

  12. Are zirconia corrosion films a form of partially stabilised zirconia (PSZ)?

    International Nuclear Information System (INIS)

    Cox, B.

    1987-03-01

    The problem of understanding the development of porosity in a zirconium oxide film still under biaxial compression is discussed. The oxide film is compared with partially stabilised zirconia (PSZ) where stress induced transformation of tetragonal zirconia has been observed to lead to microcracking of the structure. The similarities between PSZ and the thermal oxide films formed on zirconium alloys are enumerated, and an hypothesis is proposed that can both explain the penetration of pores or microcracks in oxides on Zircaloy-2 to a point very close to the oxide/metal interface, and explain the observation that such a phenomenon does not occur in oxide films on Zr-2.5%Nb. This hypothesis could be tested by laser Raman spectroscopy on oxide films during growth at elevated temperatures. 87 refs

  13. TiCN thin films grown by reactive crossed beam pulsed laser deposition

    Science.gov (United States)

    Escobar-Alarcón, L.; Camps, E.; Romero, S.; Muhl, S.; Camps, I.; Haro-Poniatowski, E.

    2010-12-01

    In this work, we used a crossed plasma configuration where the ablation of two different targets in a reactive atmosphere was performed to prepare nanocrystalline thin films of ternary compounds. In order to assess this alternative deposition configuration, titanium carbonitride (TiCN) thin films were deposited. Two crossed plasmas were produced by simultaneously ablating titanium and graphite targets in an Ar/N2 atmosphere. Films were deposited at room temperature onto Si (100) and AISI 4140 steel substrates whilst keeping the ablation conditions of the Ti target constant. By varying the laser fluence on the carbon target it was possible to study the effect of the carbon plasma on the characteristics of the deposited TiCN films. The structure and composition of the films were analyzed by X-ray Diffraction, Raman Spectroscopy and non-Rutherford Backscattering Spectroscopy. The hardness and elastic modulus of the films was also measured by nanoindentation. In general, the experimental results showed that the TiCN thin films were highly oriented in the (111) crystallographic direction with crystallite sizes as small as 6.0 nm. It was found that the hardness increased as the laser fluence was increased, reaching a maximum value of about 33 GPa and an elastic modulus of 244 GPa. With the proposed configuration, the carbon content could be easily varied from 42 to 5 at.% by changing the laser fluence on the carbon target.

  14. A computation model for the corrosion resistance of nanocrystalline zirconium metal

    International Nuclear Information System (INIS)

    Zhang Xiyan; Shi Minghua; Liu Nianfu; Wei Yiming; Li Cong; Qiu Shaoyu; Zhang Qiang; Zhang Pengcheng

    2007-01-01

    In this paper a computation model of corrosion rate-grain size of nanocrystalline and ultra-fine zirconium has been presented. The model is based on the Wagner's theory and the electron theory of solids. The conductivity, electronic mean free path and grain size of metal were considered. By this model, the corrosion rate of zirconium metal under different temperature was computed. The results show that the corrosion weight gain and rate constant of nanocrystalline zirconium is lower than that of zirconium with coarse grain size. And the corrosion rate constant and weight gain of nanocrystalline zirconium metal decrease with the decrease of grain size. So the refinement of grain size can remarkably improve the corrosion resistance of zirconium metal. (authors)

  15. Method of purifying zirconium tetrachloride and hafnium tetrachloride in a vapor stream

    International Nuclear Information System (INIS)

    Snyder, T.S.; Stolz, R.A.

    1992-01-01

    This patent describes a method of purifying zirconium tetrachloride and hafnium tetrachloride in a vapor stream from a sand chlorinator in which the silicon and metals present in sand fed to the chlorinator are converted to chlorides at temperatures over about 800 degrees C. It comprises cooling a vapor stream from a sand chlorinator, the vapor stream containing principally silicon tetrachloride, zirconium tetrachloride, and hafnium tetrachloride contaminated with ferric chloride, to a temperature of from about 335 degrees C to about 600 degrees C; flowing the vapor stream through a gaseous diffusion separative barrier to produce a silicon tetrachloride-containing vapor stream concentrated in zirconium tetrachloride and hafnium tetrachloride and a silicon tetrachloride-containing vapor stream depleted in zirconium tetrachloride and hafnium tetrachloride; adsorbing the ferric chloride in the separative barrier; and recovering the silicon tetrachloride stream concentrated in zirconium tetrachloride and hafnium tetrachloride separately from the silicon tetrachloride stream depleted in zirconium tetrachloride and hafnium tetrachloride

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

    Science.gov (United States)

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

    2018-05-01

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

  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. Microstructure, Residual Stress, Corrosion and Wear Resistance of Vacuum Annealed TiCN/TiN/Ti Films Deposited on AZ31

    Directory of Open Access Journals (Sweden)

    Haitao Li

    2016-12-01

    Full Text Available Composite titanium carbonitride (TiCN thin films deposited on AZ31 by DC/RF magnetron sputtering were vacuum annealed at different temperatures. Vacuum annealing yields the following on the structure and properties of the films: the grain grows and the roughness increases with an increase of annealing temperature, the structure changes from polycrystalline to single crystal, and the distribution of each element becomes more uniform. The residual stress effectively decreases compared to the as-deposited film, and their corrosion resistance is much improved owing to the change of structure and fusion of surface defects, whereas the wear-resistance is degraded due to the grain growth and the increase of surface roughness under a certain temperature.

  19. Plastic deformation of particles of zirconium and titanium carbide subjected to vibration grinding

    Energy Technology Data Exchange (ETDEWEB)

    Kravchik, A.E.; Neshpor, V.S.; Savel' ev, G.A.; Ordan' yan, S.S.

    1976-12-01

    A study is made of the influence of stoichiometry on the characteristics of microplastic deformation in powders of zirconium and titanium carbide subjected to vibration grinding. The carbide powders were produced by direct synthesis from the pure materials: metallic titanium and zirconium and acetylene black. As to the nature of their elastic deformation, zirconium and titanium carbides can be considered elastic-isotropic materials. During vibration grinding, the primary fracture planes are the (110) planes. Carbides of nonstoichiometric composition are more brittle.

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

    Science.gov (United States)

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

    2014-01-15

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

  1. Evaluation of macrocyclic hydroxyisophthalamide ligands as chelators for zirconium-89.

    Science.gov (United States)

    Bhatt, Nikunj B; Pandya, Darpan N; Xu, Jide; Tatum, David; Magda, Darren; Wadas, Thaddeus J

    2017-01-01

    The development of bifunctional chelators (BFCs) for zirconium-89 immuno-PET applications is an area of active research. Herein we report the synthesis and evaluation of octadentate hydroxyisophthalamide ligands (1 and 2) as zirconium-89 chelators. While both radiometal complexes could be prepared quantitatively and with excellent specific activity, preparation of 89Zr-1 required elevated temperature and an increased reaction time. 89Zr-1 was more stable than 89Zr-2 when challenged in vitro by excess DTPA or serum proteins and in vivo during acute biodistribution studies. Differences in radiometal complex stability arise from structural changes between the two ligand systems, and suggest further ligand optimization is necessary to enhance 89Zr chelation.

  2. Evaluation of macrocyclic hydroxyisophthalamide ligands as chelators for zirconium-89.

    Directory of Open Access Journals (Sweden)

    Nikunj B Bhatt

    Full Text Available The development of bifunctional chelators (BFCs for zirconium-89 immuno-PET applications is an area of active research. Herein we report the synthesis and evaluation of octadentate hydroxyisophthalamide ligands (1 and 2 as zirconium-89 chelators. While both radiometal complexes could be prepared quantitatively and with excellent specific activity, preparation of 89Zr-1 required elevated temperature and an increased reaction time. 89Zr-1 was more stable than 89Zr-2 when challenged in vitro by excess DTPA or serum proteins and in vivo during acute biodistribution studies. Differences in radiometal complex stability arise from structural changes between the two ligand systems, and suggest further ligand optimization is necessary to enhance 89Zr chelation.

  3. Proceedings [of the] symposium on zirconium alloys for reactor components

    International Nuclear Information System (INIS)

    1992-01-01

    A two day symposium on zirconium alloys for reactor components (ZARC-91) was organised during 12-13, 1991. There were 6 invited talks and 43 contributed papers in 10 technical sessions. This symposium, took stock of the progress achieved in the development, design, fabrication and quality assurance of zirconium alloy components and emphasized the R and D efforts required for meeting the challenges posed by the rapid growth of nuclear power in our country. Topics like physical metallurgy, corrosion and irradiation behaviour, and in-service inspection were also covered. The proceedings/papers are arranged under the headings: (1)invited talks, (2)fabrication, (3)design requirement, (4)quality assurance, (5)irradiation damage and PIE, (6)corrosion and hydriding, and (7)in-service inspection. (N.B.). refs., figs., tabs

  4. Extraction and determination of hydrogen in uranium and zirconium

    International Nuclear Information System (INIS)

    Champeix, L.; Coblence, G.; Darras, R.

    1959-01-01

    The method of desorption under vacuum at high temperatures in the solid phase, which gives good results in the case of steels, has been applied to uranium and zirconium. In these two metals hydrogen is found mainly in the form of hydride. It is chiefly a question of determining the most suitable temperature and the heating time necessary to obtain an almost total extraction of hydrogen. Two considerations must be taken into account in the choice of temperature. It should be such that on the one hand the hydride decomposes rapidly and completely at the reduced pressure applied, and on the other hand the diffusion of hydrogen through the metal takes place fairly quickly. The apparatus and the method used are described; systematic tests have led to the adoption of temperatures of 650 deg. C for uranium and 1050 deg. C for zirconium. (author) [fr

  5. Scandium and zirconium ion complexing with salicylic acid

    International Nuclear Information System (INIS)

    Fadeeva, V.I.; Kochetkova, S.K.

    1979-01-01

    A study has been made of the extraction of complexes containing scandium and zirconium compounds and salicylic acid by using benzene, nitrobenzene, chloroform and isoamyl alcohol. It is shown that in the metal concentration range 10 -5 -10 -3 mole/l scandium forms mononuclear complexes composed of Sc(HSal) 3 (pH 2 (pH>4), zirconium - polynuclear complexes Zrsub(x)(OH)sub(y)(HSal)sub(n), where the x:n ratio varies from 0.5 to 1.5. Stability constants have been calculated for the salicylate scandium complexes in aqueous solution, equal to β 1 =(3+-1)x10 2 ; β 2 =(5.0+-0.6)x10 4 ; β 3 =(5.3+-0.3)x10 6

  6. Effects of solutes on damage production and recovery in zirconium

    International Nuclear Information System (INIS)

    Zee, R.H.; Birtcher, R.C.; MacEwen, S.R.; Abromeit, C.

    1986-04-01

    Dilute zirconium-based alloys and pure zirconium were irradiated at 10 K with spallation neutrons at IPNS. Four types of alloys - Zr-Ti, Zr-Sn, Zr-Dy and Zr-Au - each with three concentration levels, were used. Low-temperature resistivity damage rates are enhanced by the presence of any of the four solutes. The greatest enhancement was produced by Au while the least by Dy. Within each alloy group, damage production also increased but at a decreasing rate, with increasing concentration. Post-irradiation annealing experiments, up to 400 K, showed that all four solutes suppress recovery due to interstitial migration, indicative of interstitial trapping by the solutes. Vacancy recovery is also suppressed by the presence of Sn, Dy or Au. The effect of Ti is to shift this stage to lower temperature. No clear correlation between the results with solute size was detected

  7. Scandium and zirconium ion complexing with salicylic acid

    Energy Technology Data Exchange (ETDEWEB)

    Fadeeva, V I; Kochetkova, S K [Moskovskij Gosudarstvennyj Univ. (USSR)

    1979-08-01

    A study has been made of the extraction of complexes containing scandium and zirconium compounds and salicylic acid by using benzene, nitrobenzene, chloroform and isoamyl alcohol. It is shown that in the metal concentration range 10/sup -5/-10/sup -3/ mole/l scandium forms mononuclear complexes composed of Sc(HSal)/sub 3/ (pH<=4) and Sc(OH)(HSal)/sub 2/ (pH>4), zirconium - polynuclear complexes Zrsub(x)(OH)sub(y)(HSal)sub(n), where the x:n ratio varies from 0.5 to 1.5. Stability constants have been calculated for the salicylate scandium complexes in aqueous solution, equal to ..beta../sub 1/=(3+-1)x10/sup 2/; ..beta../sub 2/=(5.0+-0.6)x10/sup 4/; ..beta../sub 3/=(5.3+-0.3)x10/sup 6/.

  8. 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

  9. 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)

  10. Modelling zirconium hydrides using the special quasirandom structure approach

    KAUST Repository

    Wang, Hao; Chroneos, Alexander I.; Jiang, Chao; Schwingenschlö gl, Udo

    2013-01-01

    The study of the structure and properties of zirconium hydrides is important for understanding the embrittlement of zirconium alloys used as cladding in light water nuclear reactors. Simulation of the defect processes is complicated due to the random distribution of the hydrogen atoms. We propose the use of the special quasirandom structure approach as a computationally efficient way to describe this random distribution. We have generated six special quasirandom structure cells based on face centered cubic and face centered tetragonal unit cells to describe ZrH2-x (x = 0.25-0.5). Using density functional theory calculations we investigate the mechanical properties, stability, and electronic structure of the alloys. © the Owner Societies 2013.

  11. 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.

  12. Study on the scattering law and scattering kernel of hydrogen in zirconium hydride

    International Nuclear Information System (INIS)

    Jiang Xinbiao; Chen Wei; Chen Da; Yin Banghua; Xie Zhongsheng

    1999-01-01

    The nuclear analytical model of calculating scattering law and scattering kernel for the uranium zirconium hybrid reactor is described. In the light of the acoustic and optic model of zirconium hydride, its frequency distribution function f(ω) is given and the scattering law of hydrogen in zirconium hydride is obtained by GASKET. The scattering kernel σ l (E 0 →E) of hydrogen bound in zirconium hydride is provided by the SMP code in the standard WIMS cross section library. Along with this library, WIMS is used to calculate the thermal neutron energy spectrum of fuel cell. The results are satisfied

  13. Electrocnecical behaviour of zirconium during its anodic polarization in nitrate solutions

    International Nuclear Information System (INIS)

    Stabrovskij, A.I.; Karasev, A.F.

    1983-01-01

    Electrochemical behaviour of zirconium during its anodic polarization in nitrate solutions is investigated in detail to find the method of its complete dissolution. A study has been made of the influence of varioUs factors: current density electric potential, composition and temperature of the solution, anodic polarization duration on the Zr anodic polarization in nitric acid, on the maximum permissible current density and on the zirconium yield to the solution. The zirconium polarization decreases with an acid concentration and temperature increase and increases with the current density. Iron nitrate additions to nitric acid decrease, while ammonium fluoride additions increase zirconium yield into the solution

  14. The addition zirconium effect on the solubility and activity of sulfur in liquid iron

    International Nuclear Information System (INIS)

    Burylev, B.P.; Mojsov, L.P.

    1994-01-01

    Critical analysis of reference data on thermodynamic properties of zirconium sulfides is conducted for evaluation of zirconium desulfonation ability in liquid steel. Sulfur solubility dependence on zirconium concentration in liquid iron is presented. Curves of sulfur solubility in liquid iron in the presence of other elements, including titanium, manganese, vanadium and chromium are presented for comparison. It is shown that equilibrium concentration of sulfur is much lower than standard sulfur concentrations in steel, therefore zirconium appears to be the best desulfonator among the metals considered

  15. Photometric determination of zirconium in phosphorites by reaction with arsenazo III

    Energy Technology Data Exchange (ETDEWEB)

    Nikol' skaya, I V; Maksimov, A V

    1976-05-01

    The reaction between zirconium and arsenazo III has been studied over a wide range of hydrochloric acid concentration and under different conditions. 6 and 9 M HCl solutions are optimal for determining zirconium; the least effect of phosphate ions and color stability in time are observed in this case. The determination of zirconium should be carried out using 10-fold reagent excess and in 15-20 min after adding the reagent. The interference of phosphate ions has been estimated. A procedure has been developed for photometric determination of zirconium in phosphorites with prior acid separation of soluble impurities.

  16. 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.

  17. Sintering nanodisperse zirconium powders with various stabilizing additives

    Directory of Open Access Journals (Sweden)

    Antsiferov V.N.

    2011-01-01

    Full Text Available Effect of various stabilizing additives on sintering kinetics of nanodisperse powders was studied by thermomechanical analysis. Temperature ranges of the most intense shrinking, characteristic points of shrinking rate changes were established. Peaks characterizing the most intense shrinking of nanodisperse zirconium powder samples were shown to allow to arrange the stabilizing additives as follows: Y2O3→CeO2→TiO2.

  18. Many-beam electron extinction distances in zirconium

    International Nuclear Information System (INIS)

    Cann, C.D.

    1977-05-01

    Many-beam extinction distances have been calculated for twenty-two of the lowest order reflections in zirconium. Ten beams comprising the directly transmitted and the nine lowest order systematic reflections were included in each calculation. Extinction distances for each reflection were determined for electron accelerating voltages of 100 and 200 kV, both at the exact Bragg condition and at deviations up to two Bragg angles from this condition. (author)

  19. Pentamethylcyclopentadienyl Zirconium and Hafnium Polyhydride Complexes : Synthesis, Structure, and Reactivity

    NARCIS (Netherlands)

    Visser, Cindy; Hende, Johannes R. van den; Meetsma, Auke; Hessen, Bart; Teuben, Jan H.

    2001-01-01

    The half-sandwich zirconium and hafnium N,N-dimethylaminopropyl complexes Cp*M[(CH2)3NMe2]Cl2 (Cp* = η5-C5Me5, M = Zr, 1; Hf, 2) and Cp*M[(CH2)3NMe2]2Cl (M = Zr, 3; Hf, 4) were synthesized by mono- or dialkylation of Cp*MCl3 with the corresponding alkyllithium and Grignard reagents. Hydrogenolysis

  20. Acoustic emission from zirconium alloys during mechanical and fracture testing

    International Nuclear Information System (INIS)

    Coleman, C.E.

    1986-10-01

    The application of acoustic emission during the mechanical and fracture testing of zirconium alloys is reviewed. Acoustic emission is successful in following delayed hydride cracking quantitatively. It is especially useful when great sensitivity is required. Application to fatigue, tensile deformation and stress corrosion cracking appears promising but requires more work to separate phenomena before it can be used quantitatively. This report is based on an invited review for the American Society of Non-Destructive Testing Handbook: Volume 5, Acoustic Emission Testing

  1. Annealing of chemical radiation damage in zirconium nitrate

    International Nuclear Information System (INIS)

    Mahamood, Aysha; Chandunni, E.; Nair, S.M.K.

    1979-01-01

    A kinetic study of the annealing of γ-irradiation damage in zirconium nitrate is presented. The annealing can be represented as a combination of a first order and a second order process. It is considered that the first order process is the combination of close correlated pairs of Osup(-) and NO fragments and the second order process involves the single reaction of random recombination of the fragments throughout the crystal. (auth.)

  2. Activation analysis in zirconium and alloys for nuclear application

    International Nuclear Information System (INIS)

    Cohen, I.M.; Mila, M.I.; Gomez, C.D.

    1981-01-01

    A study has been performed with the purpose to ascertain the possibilities of using neutron activation analysis in non-destructive determination of several elements present in zirconium and its alloys. Those elements must be limited within acceptable top levels, in accordance to standards for nuclear applications. The experimental techniques used are described and the results obtained are discussed, showing that the method is adequate for determining Cl, Co, Hf, Mn, and W, but not Ni and U. (M.E.L.) [es

  3. Rapid radiochemical separation of zirconium-95 and niobium-95

    International Nuclear Information System (INIS)

    Downey, D.M.; McLaughlin, C.L.

    1983-01-01

    A rapid method for the quantitative separation of 95 Zr and 95 Nb has been developed. The method is based on the ion flotation of cationic zirconium complex ions with sodium lauryl sulfate (NaLS) from niobium which is masked with hydrogen peroxide. The separation was applied to mixtures of 95 Zr and 95 Nb initially in oxalic acid solution and quantitative recoveries of the radiochemically pure radioisotopes were obtained. (orig.)

  4. Rapid radiochemical separation of zirconium-95 and niobium-95

    Energy Technology Data Exchange (ETDEWEB)

    Downey, D.M.; McLaughlin, C.L.

    1983-01-01

    A rapid method for the quantitative separation of /sup 95/Zr and /sup 95/Nb has been developed. The method is based on the ion flotation of cationic zirconium complex ions with sodium lauryl sulfate (NaLS) from niobium which is masked with hydrogen peroxide. The separation was applied to mixtures of /sup 95/Zr and /sup 95/Nb initially in oxalic acid solution and quantitative recoveries of the radiochemically pure radioisotopes were obtained.

  5. Automated reconstruction of pre-transformation microstructures in zirconium

    International Nuclear Information System (INIS)

    Krishna, K.V. Mani; Tripathi, P.; Hiwarkar, V.D.; Pant, P.; Samajdar, I.; Srivastava, D.; Dey, G.K.

    2010-01-01

    An automated reconstruction of the pre-transformation microstructure from the microtexture data of the post-transformation product phase is proposed. The method involves identifying triplets of neighboring product grains with a common variant and linking such neighboring triplets via a generalized misorientation criterion. The approach is non-iterative and extremely efficient computationally. The method was tested successfully for different post-transformation microstructures in zirconium.

  6. 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

  7. Geometry optimization of zirconium sulfophenylphosphonate layers by molecular simulation methods

    Czech Academy of Sciences Publication Activity Database

    Škoda, J.; Pospíšil, M.; Kovář, P.; Melánová, Klára; Svoboda, J.; Beneš, L.; Zima, Vítězslav

    2018-01-01

    Roč. 24, č. 1 (2018), s. 1-12, č. článku 10. ISSN 1610-2940 R&D Projects: GA ČR(CZ) GA14-13368S; GA ČR(CZ) GA17-10639S Institutional support: RVO:61389013 Keywords : zirconium sulfophenylphosphonate * intercalation * molecular simulation Subject RIV: CA - Inorganic Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 1.425, year: 2016

  8. Thermodynamics of hydrogen and deuterium solutions in α-zirconium

    International Nuclear Information System (INIS)

    Vinokurov, Yu.V.; Mogutnov, B.M.

    1979-01-01

    Interaction of H 2 and D 2 with α-Zr are studied in the 700-890 K temperature range using a high-temperature colorimeter. It is shown that hydrogen and deuterium partial enthalpies in zirconium do not depend on the temperature and concentration and compose -48.9+-1.0 and -46.2+-1.2 kJ/g-at. Calculated is an excess entropy of hydrogen in a solution and analyzed are contributions composing it

  9. Preparation of high quality zirconium oxychloride from zircon of Vietnam

    International Nuclear Information System (INIS)

    Ngo Van Tuyen; Vu Thanh Quang; Trinh Giang Huong; Vuong Huu Anh

    2007-01-01

    This paper introduces a sodium hydroxide decomposition method for zirconium oxychloride production from zircon sand of Vietnam such as Ha Tinh, Hue, Binh Thuan seaside. Techniques for separation of impurities in ZOC final product such as SiO 2 , Fe 2 O 3 , TiO 2 , rare earths, uranium, and thorium have also been introduced. Content of uranium and thorium in the final product of ZOC is less than 1 ppm. (author)

  10. The spread analysis of pollutants for zirconium cycle company

    International Nuclear Information System (INIS)

    Kozhevnikova, M.F.; Levenets, V.V.; Rolik, I.L.; Mets, K.A.

    2013-01-01

    The spread analysis of pollutants in the atmosphere above location area of the zirconium cycle company in Ukraine is presented. It is proposed the data processing method for the pollution source detection. An analysis of the air mass movement above the industrial area of Volnohirsk in Dnipropetrovsk region was performed. The air flow path maps and the distribution of major pollutants on the study area were obtained

  11. Thermodynamic and kinetic characterization of a zirconium chelate

    International Nuclear Information System (INIS)

    Stumpf, H.O.; Ekman, M.F.; Souza, R.F.; Costa, V.H.; Dick, Y.P.

    1980-01-01

    The chemical preparation, composition and characteristics of a zirconium complex with hemateine was studied. Hematein is the common name of an organic compound containing hydroxy-aromatic and hydroxyquinonic groups. The stability constant of this complex was determined spectrophotometrically. Other thermodynamic parameters for the complex formation were also determined; the effect of temperature on these parameters was examined. Reaction kinetics was investigated, as well as the charge of reacting species for the formation of the activated complex. (C.L.B.) [pt

  12. Zirconium molybdate gel as a generator for technetium-99m

    International Nuclear Information System (INIS)

    Evans, J.V.; Shying, M.E.

    1984-12-01

    A new sup(99m)Tc generator based on zirconium molybdate gel is described. Essentially the gel is a cation ion exchanger which permits the elution of the pertechnetate ion. The high molybdenum content of this gel, its stability under self-irradiation, and the absence of organic materials during preparation provide a generator concept that eliminates high processing costs, active waste storage costs and stability problems in other types of generator

  13. Research on development and application of titanium and zirconium alloys

    International Nuclear Information System (INIS)

    Suzuki, Toshiyuki; Sasano, Hisaoki; Uehara, Shigeaki; Nakano, Osamu; Shibata, Michio

    1983-01-01

    It can be said that titanium and zirconium are new metals from the viewpoint of the history of metals, but both have grown to the materials supporting modern industries, titanium alloys in aerospace and ocean development, and zirconium alloys in nuclear power application. However, the properties of both alloys have not yet been clarified. In this study, the synthesis of TiNi and its properties, precipitation hardening type titanium alloys, and the effect of oxygen on the mechanical properties of both alloys were examined. TiNi is the typical intermetallic compound which shows the peculiar properties. The method of its synthesis by diffusion was examined, and it was clarified that it is useful as a structural material and also as a functional material. Precipitation hardening type alloys have not been developed in titanium alloys, but in this study, the feasibility of several alloy systems was found. Both titanium and zirconium have large affinity to oxygen, and the oxygen absorbed in the manufacturing process cannot be reduced. The tensile property of both alloys was examined in wide temperature range, and the effect of oxygen was clarified. (Kako, I.)

  14. Ferrier rearrangement promoted by an electrochemically generated zirconium catalyst.

    Science.gov (United States)

    Stevanović, Dragana; Pejović, Anka; Damljanović, Ivan; Minić, Aleksandra; Bogdanović, Goran A; Vukićević, Mirjana; Radulović, Niko S; Vukićević, Rastko D

    2015-04-30

    In situ generated zirconium catalyst from a sacrificial zirconium anode was successfully applied to promote Ferrier rearrangement of 3,4,5-tri-O-acetyl-D-glucal and 6-deoxy-3,4-di-O-acetyl-L-glucal (3,4-di-O-acetyl-L-rhamnal) in the presence of three thiols and eleven thiophenols as nucleophiles. A simple constant current electrolysis (20 mA, 0.4 F mol(-1)) of an acetonitrile solution of lithium perchlorate (0.1 M) containing the corresponding glycal and S-nucleophiles, using a zirconium anode and a platinum cathode resulted in the successful synthesis of the corresponding 2,3-unsaturated peracetylated thioglycosides (with an average anomer ratio α/β=4.129 in the case of peracetylated D-glucal and 8.740 in the case of L-rhamnal). The same procedure proved to be appropriate in synthesizing dihydropyran derivatives ('C-glycosides') using allyltrimethylsilane as the nucleophile (only 'α-anomers' were obtained). All new compounds were fully characterized by spectral data, whereas single-crystal X-ray analysis was performed for two thioglycosides. Copyright © 2015 Elsevier Ltd. All rights reserved.

  15. Control of microstructure during hot working of zirconium alloys

    International Nuclear Information System (INIS)

    Chakravartty, J.K.; Banerjee, S.

    2005-01-01

    Hot working is considered to be the most important step involved in the fabrication of zirconium alloys for nuclear reactor applications for two reasons: i) the scale of the microstructure and texture of the final product is decided at this stage and ii) the hot deformed microstructure provides a suitable starting microstructure for the subsequent fabrication steps. The resultant microstructure in turn controls the properties of the final product. In order to obtain final product with a suitable microstructure and with specified mechanical properties on a repeatable basis the control of microstructure during hot working is of paramount importance. This is usually done by studying the constitutive behaviour of the material under hot working conditions and by constructing processing maps. In the latter method, strain rate sensitivity is mapped as a function of temperature and strain rate to delineate domains within the bounds of which a specific deformation mechanism dominates. Detail microstructural analysis is then carried out on the samples deformed within the domains. Using this methodology, processing maps have been constructed for various zirconium alloys. These maps have been found to be very useful for optimizing the hot workability and control of microstructure of zirconium alloys. (author)

  16. Development of microstructure in thermomechanical processing of zirconium alloys

    International Nuclear Information System (INIS)

    Jha, S.K.; Saibaba, N.; Jayaraj, R.N.

    2009-01-01

    Zirconium based alloys are used for the manufacture of fuel tubes pressure tubes calandria tubes and other components of Pressurized Heavy Water Reactors (PHWRS). In single or two phase zirconium alloy system a variety of microstructure can be generated by suitable heat treatments by the process of equilibrium and non equilibrium phase transformations Microstructure can also be modified by alloying with α and β stabilizers. The microstructure in Zr alloys could be single hexagonal phase (α alloys) two phase bcc and hexagonal (α + β alloys) phase, single metastable martensitic microstructure and β with ω phase. The microstructural and micro textural evolution during thermo mechanical treatments depends strongly on such initial microstructure. Hot extrusion is a significant bulk deformation step which decides the initial microstructure of the alloy. It is carried out at elevated temperature i e above the recrystallization temperature, which enable imposition of large strains in single step. This deformation causes a significant change in the microstructure of the material and depends on extrusion process parameters such as temperature, strain rate (Ram speed), reduction ratio etc. In the present paper development of microstructures, microtexture and texture have been examined. An attempt is also made to optimise the hot working parameters for different Zirconium alloys with help of these studies. (author)

  17. Laves intermetallics in stainless steel-zirconium alloys

    International Nuclear Information System (INIS)

    Abraham, D.P.; McDeavitt, S.M.; Richardson, J.W. Jr.

    1997-01-01

    Laves intermetallics have a significant effect on properties of metal waste forms being developed at Argonne National Laboratory. These waste forms are stainless steel-zirconium alloys that will contain radioactive metal isotopes isolated from spent nuclear fuel by electrometallurgical treatment. The baseline waste form composition for stainless steel-clad fuels is stainless steel-15 wt.% zirconium (SS-15Zr). This article presents results of neutron diffraction measurements, heat-treatment studies and mechanical testing on SS-15Zr alloys. The Laves intermetallics in these alloys, labeled Zr(Fe,Cr,Ni) 2+x , have both C36 and C15 crystal structures. A fraction of these intermetallics transform into (Fe,Cr,Ni) 23 Zr 6 during high-temperature annealing; the authors have proposed a mechanism for this transformation. The SS-15Zr alloys show virtually no elongation in uniaxial tension, but exhibit good strength and ductility in compression tests. This article also presents neutron diffraction and microstructural data for a stainless steel-42 wt.% zirconium (SS-42Zr) alloy

  18. Development of tantalum–zirconium alloy for hydrogen purification

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Sanjay, E-mail: sanjay.barc@gmail.com [Fusion Reactor Materials Section, MG, BARC, Mumbai 85 (India); IAMR, Hiroshima University, Higashihiroshima 739-8530 (Japan); Singh, Anamika [GSASM Hiroshima University, Higashihiroshima 739-8530 (Japan); Jain, Uttam; Dey, Gautam Kumar [Fusion Reactor Materials Section, MG, BARC, Mumbai 85 (India)

    2016-11-01

    Highlights: • Terminal solid solubility of Ta increases with Zr addition. • Increase in lattice parameters of Ta due to Zr addition may be the possible reason. • Enhance H solubility could also be explained on the change in e-DOS of Ta–Zr alloys. • Ta–Zr alloys could be possible combination for hydrogen purification membrane. - Abstract: Terminal solid solubility of hydrogen in Ta–Zr alloys has been studied in connection with the development of tantalum based metallic membrane for hydrogen/tritium purification. The alloys were prepared by vacuum arc melting technique and subsequently cold rolled to 0.2 mm thickness. The terminal solid solubility of hydrogen in these cold rolled samples was investigated in a modified Sieverts apparatus. The terminal solid solubility of hydrogen was marginally increased with zirconium content. The change in the lattices parameter of tantalum upon zirconium addition and the higher affinity of zirconium for hydrogen as compared to tantalum could be the possible reasons.

  19. Influence of the electrical power applied to the target on the optical and structural properties of ZrON films produced via RF magnetron sputtering in a reactive atmosphere

    International Nuclear Information System (INIS)

    Pinzón, M.J.; Alfonso, J.E.; Olaya, J.J.; Cubillos, G.I.; Romero, E.

    2014-01-01

    The influence of the variation of electrical power applied to the target on the morphology and optical properties of zirconium oxynitride - zirconium oxide (ZrON) films deposited via RF magnetron sputtering on common glass substrates in a reactive atmosphere of N 2 /O 2 , with a flow ratio ΦN 2 /ΦO 2 of 1.25 was investigated. The crystallographic structure of the films was established through X-ray diffraction (XRD), the morphology was evaluated through scanning electron microscopy (SEM) and atomic force microscopy (AFM), and the optical behavior was evaluated through transmittance measurements. The XRD analysis showed that the films grew with mixed crystalline structures: monoclinic (ZrO 2 ) and body-centered cubic (Zr 2 ON 2 ). SEM analysis showed that the films grew with a homogeneous morphology, and AFM results established that as the electrical power applied to the target increased, there were changes in the grain size and the roughness of the films. The thickness, refractive index, and absorption coefficient of the films were calculated using the values of the transmittance through the Swanepoel method. Additionally, the energy band gap was determined via analysis of the free interference region. - Highlights: • We growth zirconium oxynitride films by RF magnetron sputtering in reactive atmosphere. • We determine the influence of the electrical power applied at the target in optical and structural properties. • We determine the crystallite size, grain size and roughness of the zirconium oxynitride films. • We determine the optical parameters such refractive index of the zirconium oxynitride films through Swanepoel method. • We calculated the absorption coefficient and optical band gap of the zirconium oxynitride films

  20. Influence of the electrical power applied to the target on the optical and structural properties of ZrON films produced via RF magnetron sputtering in a reactive atmosphere

    Energy Technology Data Exchange (ETDEWEB)

    Pinzón, M.J. [Grupo de Ciencia de Materiales y Superficies, Departamento de Física, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Alfonso, J.E., E-mail: jealfonsoo@unal.edu.co [Grupo de Ciencia de Materiales y Superficies, Departamento de Física, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Olaya, J.J. [Grupo de Ciencia de Materiales y Superficies, Departamento de Física, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Cubillos, G.I.; Romero, E. [Grupo de Materiales y Procesos Químicos, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia)

    2014-12-01

    The influence of the variation of electrical power applied to the target on the morphology and optical properties of zirconium oxynitride - zirconium oxide (ZrON) films deposited via RF magnetron sputtering on common glass substrates in a reactive atmosphere of N{sub 2}/O{sub 2}, with a flow ratio ΦN{sub 2}/ΦO{sub 2} of 1.25 was investigated. The crystallographic structure of the films was established through X-ray diffraction (XRD), the morphology was evaluated through scanning electron microscopy (SEM) and atomic force microscopy (AFM), and the optical behavior was evaluated through transmittance measurements. The XRD analysis showed that the films grew with mixed crystalline structures: monoclinic (ZrO{sub 2}) and body-centered cubic (Zr{sub 2}ON{sub 2}). SEM analysis showed that the films grew with a homogeneous morphology, and AFM results established that as the electrical power applied to the target increased, there were changes in the grain size and the roughness of the films. The thickness, refractive index, and absorption coefficient of the films were calculated using the values of the transmittance through the Swanepoel method. Additionally, the energy band gap was determined via analysis of the free interference region. - Highlights: • We growth zirconium oxynitride films by RF magnetron sputtering in reactive atmosphere. • We determine the influence of the electrical power applied at the target in optical and structural properties. • We determine the crystallite size, grain size and roughness of the zirconium oxynitride films. • We determine the optical parameters such refractive index of the zirconium oxynitride films through Swanepoel method. • We calculated the absorption coefficient and optical band gap of the zirconium oxynitride films.

  1. State and perspectives of methodological support of materials research of products from Zirconium alloys for fuel rods and fuel assemblies of VVER

    International Nuclear Information System (INIS)

    Gusev, A.; Markelov, V.; Novikov, V.; Zheltkovskaya, T.; Malgin, A.; Shevyakov, A.; Bekrenev, S.

    2015-01-01

    The basic methodological framework for the study of the characteristics of zirconium products was created in JSC «VNIINM». The reliability of experiments confirmed the results of metrological certification procedures. Further development of methodological support of «VNIINM» for Zr products research is the development and validation of methods to determine: mechanical characteristics under internal pressure; Determination of Contractile Strain Ratio (CSR); Expansion Due to Compression (EDC); Plane Strain Tensile (PST); characteristics of resistance multi-cycle and low-cyclic fatigue; texture parameters using the orientation distribution function; the electrical characteristics of the oxide film by impedance

  2. Spectrophotometric study of the complexation equilibria of zirconium(IV) with 1-amino-4-hydroxyanthraquinone and the determination of zirconium

    Energy Technology Data Exchange (ETDEWEB)

    Idriss, K A; Seleim, M M; Saleh, M S; Abu-Bakr, M S; Sedaira, Hassan

    1988-11-01

    The spectral absorption and acid-base characteristics of 1-amino-4-hydroxyanthraquinone (AMHA) were studied in water -ethanol media. The composition, molar absorptivities, equilibrium constants and stability constants of the chelates of this reagent with zirconium(IV) have been determined spectrophotometrically in 40% V/V ethanol at 20/sup 0/C and an ionic strength of 0.1 M (NaClO/sub 4/). Graphical logarithmic analysis of the absorbance graphs was used to demonstrate and characterise the complexation equilibria in solution. A simple, rapid, selective and sensitive method for the spectrophotometric determination of trace amounts of zirconium is proposed based on the formation of the Zr(AMHA)/sub 2/ complex at pH 3.5 (lambda/sub max/ = 600 nm, epsilon 1.621 x 10/sup 4/ l mol/sup -1/ cm/sup -1/). Interference caused by a number of ions was masked by the addition of cyanide ions.

  3. 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.

  4. Investigate of analysis for hydrogen contents in carbon films

    International Nuclear Information System (INIS)

    Yasui, Haruyuki; Hirose, Yukio; Sasaki, Toshihiko; Awazu, Kaoru; Naramoto, Hiroshi

    2001-01-01

    Hydrogen is a very common contaminant in carbon films. It can strongly influences on mechanical, physical and chemical properties of the films. The analysis of hydrogen is therefore a crucial problem to prepare the films with the reproducible property. We were measured two kinds of methods. Ion beam techniques using nuclear reactions are established methods for the quantitative determination of hydrogen concentration. A spectrometer has been constructed for the determination of hydrogen concentrations by detecting 4.43 MeV γ-rays from the resonant nuclear reactions 1 H( 15 N, α γ) 12 C at the 6.385 MeV. And the other measurement of hydrogen is GDOES (Glow Discharge Optical Emission Spectroscopy), with its high sputtering rates, had been used previously for depth profiling analysis of thin films. The depth profiling analysis was carried out at an argon atmosphere by applying an RF of 13.56 MHz. The sampling time interval was 0.1 sec. The detailed hydrogen analysis was made on BCN (Boron Carbonitride) and DLC (Diamond-like Carbon) thin films. The BCN films were prepared by ion beam assisted deposition, in which boron and carbon were deposited by electron beam heating of B 4 C solid and nitrogen was supplied by implantation simultaneously. The DLC films were prepared by HPPC (Hybrid-pulse plasma coating) system. It was a new coating system that we developed which consists fundamentally of plasma CVD (chemical vapor deposition) and ion-mixing. In this paper, we reported the comparison of analysis for hydrogen contents between RNRA and GDOES. (author)

  5. Investigate of analysis for hydrogen contents in carbon films

    Energy Technology Data Exchange (ETDEWEB)

    Yasui, Haruyuki; Hirose, Yukio; Sasaki, Toshihiko [Kanazawa Univ., Kanazawa, Ishikawa (Japan); Awazu, Kaoru [Industrial Research Institute of Ishikawa, Kanazawa, Ishikawa (Japan); Naramoto, Hiroshi [Japan Atomic Energy Research Inst., Takasaki, Gunma (Japan). Takasaki Radiation Chemistry Research Establishment

    2001-07-01

    Hydrogen is a very common contaminant in carbon films. It can strongly influences on mechanical, physical and chemical properties of the films. The analysis of hydrogen is therefore a crucial problem to prepare the films with the reproducible property. We were measured two kinds of methods. Ion beam techniques using nuclear reactions are established methods for the quantitative determination of hydrogen concentration. A spectrometer has been constructed for the determination of hydrogen concentrations by detecting 4.43 MeV {gamma}-rays from the resonant nuclear reactions {sup 1}H({sup 15}N, {alpha} {gamma}){sup 12}C at the 6.385 MeV. And the other measurement of hydrogen is GDOES (Glow Discharge Optical Emission Spectroscopy), with its high sputtering rates, had been used previously for depth profiling analysis of thin films. The depth profiling analysis was carried out at an argon atmosphere by applying an RF of 13.56 MHz. The sampling time interval was 0.1 sec. The detailed hydrogen analysis was made on BCN (Boron Carbonitride) and DLC (Diamond-like Carbon) thin films. The BCN films were prepared by ion beam assisted deposition, in which boron and carbon were deposited by electron beam heating of B{sub 4}C solid and nitrogen was supplied by implantation simultaneously. The DLC films were prepared by HPPC (Hybrid-pulse plasma coating) system. It was a new coating system that we developed which consists fundamentally of plasma CVD (chemical vapor deposition) and ion-mixing. In this paper, we reported the comparison of analysis for hydrogen contents between RNRA and GDOES. (author)

  6. Effect of Bi on the corrosion resistance of zirconium alloys

    International Nuclear Information System (INIS)

    Yao Meiyi; Zhou Bangxin; Li Qiang; Zhang Weipeng; Zhu Li; Zou Linghong; Zhang Jinlong; Peng Jianchao

    2014-01-01

    In order to investigate systematically the effect of Bi addition on the corrosion resistance of zirconium alloys, different zirconium-based alloys, including Zr-4 (Zr-l.5Sn-0.2Fe-0.1Cr), S5 (Zr-0.8Sn-0.35Nb-0.4Fe-0.1Cr), T5 (Zr-0.7Sn-l.0Nb-0.3Fe-0.1Cr) and Zr-1Nb, were adopted to prepare the zirconium alloys containing Bi of 0∼0.5% in mass fraction. These alloys were denoted as Zr-4 + xBi, S5 + xBi, T5 + xBi and Zr-1Nb + xBi, respectively. The corrosion behavior of these specimens was investigated by autoclave testing in lithiated water with 0.01 M LiOH or deionized water at 360 ℃/18.6 MPa and in superheated steam at 400 ℃/10.3 MPa. The microstructure of the alloys was examined by TEM and the second phase particles (SPPs) were analyzed by EDS. Microstructure observation shows that the addition of Bi promotes the precipitation of Sn as second phase particles (SPPs) because Sn is in solid solution in α-Zr matrix in Zr-4, S5 and T5 alloys. The concentration of Bi dissolved in α-Zr matrix increase with the increase of Nb in the alloys, and the excess Bi precipitates as Bi-containing SPPs. The corrosion results show that the effect of Bi addition on the corrosion behavior of different zirconium-based alloys is very complicated, depending on their compositions and corrosion conditions. In the case of higher Bi concentration in α-Zr, the zirconium alloys exhibit better corrosion resistance. However, in the case of precipitation of Bi-containing SPPs, the corrosion resistance gets worse. This indicates that the solid solution of Bi in α-Zr matrix can improve the corrosion resistance, while the precipitation of the Bi-containing SPPs is harmful to the corrosion resistance. (authors)

  7. Synthesis of nanostructured multiphase Ti(C,N)/a-C films by a plasma focus device

    International Nuclear Information System (INIS)

    Ghareshabani, E.; Rawat, R.S.; Sobhanian, S.; Verma, R.; Karamat, S.; Pan, Z.Y.

    2010-01-01

    Nanostructured multiphase Ti(C,N)/a-C films were deposited using a 3.3 kJ pulsed plasma focus device onto silicon (1 0 0) substrates at room temperature. The plasma focus device, fitted with solid titanium anode instead of usual hollow copper anode, was operated with nitrogen and Ar/CH 4 as the filling gas. Films were deposited with different number of shots, at 80 mm from top of the anode and at zero angular position with respect to anode axis. X-ray diffraction results show the diffraction peaks related to different compounds such as TiC 2 , TiN, Ti 2 CN, Ti and TiC 0.62 confirming the deposition of multiphase titanium carbo-nitride composite films on silicon. X-ray photoelectron spectroscopy confirms the formation of Ti-C, C-N, Ti-N, Ti-O and C-C bonds in the films. Scanning electron microscopy reveals that the nanostructure grains are agglomerates of smaller nanoparticles about 10-20 nm in size. Raman studies verify the formation of multiphase Ti(C,N) and also of amorphous graphite in the films. The maximum microhardness value of the composite film is 14.8 ± 1.3 GPa for 30 shots.

  8. Aqueous metal–organic solutions for YSZ thin film inkjet deposition

    DEFF Research Database (Denmark)

    Gadea, Christophe; Hanniet, Q.; Lesch, A.

    2017-01-01

    Inkjet printing of 8% Y2O3-stabilized ZrO2 (YSZ) thin films is achieved by designing a novel water-based reactive ink for Drop-on-Demand (DoD) inkjet printing. The ink formulation is based on a novel chemical strategy that consists of a combination of metal oxide precursors (zirconium alkoxide...

  9. 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

  10. Studies in group IV organometallic chemistry XXX. Synthesis of compounds containing tin---titanium and tin---zirconium bonds

    NARCIS (Netherlands)

    Creemers, H.M.J.C.; Verbeek, F.; Noltes, J.G.

    1968-01-01

    Starting from the tetrakis(diethylamino) derivatives of titanium and zirconium and pheyltin hydrides six intermetalic compounds contianing up to nine tin and titanium(or zirconium) atoms have been obtained by hydrostannolysis type reactions.

  11. Investigation on the effect of Zr doping in ZnO thin films by spray pyrolysis

    International Nuclear Information System (INIS)

    Gokulakrishnan, V.; Parthiban, S.; Jeganathan, K.; Ramamurthi, K.

    2011-01-01

    Zirconium doped zinc oxide thin films with enhanced optical transparency were prepared on Corning 1737 glass substrates at the substrate temperature of 400 o C by spray pyrolysis method for various doping concentrations of zirconium (IV) chloride in the spray solution. The X-ray diffraction studies reveal that the films exhibit hexagonal crystal structure with polycrystalline grains oriented along (0 0 2) direction. The crystalline quality of the films is found to be deteriorating with the increase of doping concentration and acquires amorphous state for higher concentration of 8 at.% in precursor solution. The average transmittance for 5 at.% (solution) zirconium doped ZnO film is significantly increased to ∼92% in the visible region of 500-800 nm. The room temperature photoluminescence (PL) spectra of films show a band edge between 3.41 and 3.2 eV and strong blue emission at 2.8 eV irrespective of doping concentration and however intensity increases consistently with doping levels. The vacuum annealing at 400 o C reduced the resistivity of the films significantly due to the coalescence of grains and the lowest resistivity of 2 x 10 -3 Ω cm is observed for 3 at.% (solution) Zr doped ZnO films which envisages that it is a good candidate for stable TCO material.

  12. Passive behaviour of zirconium, hafnium and niobium

    International Nuclear Information System (INIS)

    Hornkjoel, S.

    1990-01-01

    The paper deals mainly with the results of stationary and transient polarization measurements together with capacitance measurements on passive electrodes of Zr, Hf and Nb over the entire pH-scale. The passive current densities are exstremely low, and essentially both pH and potential independent, exept for Nb at high pH. The extrapolated potential of zero inverse capacitance seems to be different from the extrapolated potential of zero film thickness for Zr and Hf, but not for Nb. The potential versus time curves at constant current show a downwards bending for Zr and Hf. It is shown that the pitting potentials of Zr and Hf are dependent of the concentration of halide ions and the type of halide ion, but not on pH. It is also shown that the pitting induction is second-order stimulated by chloride ions and first-order hindered by sulphate ions. Results from electron transfer reactions on passive niobium are reported. 9 refs

  13. 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

  14. 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.

  15. 40 CFR 721.10152 - Oxirane, substituted silylmethyl-, hydrolysis products with alkanol zirconium(4+) salt and silica...

    Science.gov (United States)

    2010-07-01

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

  16. Mechanistic understanding of irradiation corrosion of zirconium alloys in nuclear power plants: stimuli, status and outlook

    International Nuclear Information System (INIS)

    Cox, B.; Ishigure, K.; Johnson, A.B.; Lemalgnan, J.C.; Nechaev, A.F.; Petrik, N.G.; Reznichenko, E.A.

    1990-01-01

    Extensive information about the corrosion behaviour of zirconium alloys under irradiation is presented. Review of the existing models of radiation corrosion is given. An accent is made on a necessity in conducting basic investigations to overcome contradictions in interpreting the experimental data available. Importance of solving the problem of zirconium alloy corrosion for safe NPP operation is underlined. 34 refs.; 6 figs.; 4 tabs

  17. On the stabilization of niobium(V) solutions by zirconium(IV) and hafnium(IV)

    DEFF Research Database (Denmark)

    Sørensen, E.; Bjerre, A.B.

    1992-01-01

    Niobium cannot be separated from zirconium or hafnium when these elements occur together in solution with common anions such as chloride and sulphate. This is ascribed to the co-polymerization of niobium(V) and the hydrolysed ionic species of zirconium(IV) and hafnium(IV) to form colloidal...

  18. The technologies of zirconium production for nuclear fuel components in Ukraine

    International Nuclear Information System (INIS)

    Semenov, G.R.

    2000-01-01

    Perspectives of development zirconium alloys and WWER-1000 assemble components production in Ukraine are considered. Basic technological production processes of zirconium alloys in conditions of Ukrainian enterprises and modern requirements are analyzed. The critical processes on technical and economic criteria are defined. The main directions of activity and steps on technological processes improvement for production quality providing are offered. (author)

  19. Zirconium phosphate coating on aluminium foams by electrophoretic deposition for acidic catalysis

    NARCIS (Netherlands)

    Ordomskiy, V.; Schouten, J.C.; Schaaf, van der J.; Nijhuis, T.A.

    2012-01-01

    The electrophoretic deposition method has been applied for the formation of an amorphous zirconium phosphate layer on the surface of open-cell aluminum foam. The aluminum foam was fully and uniformly covered by the zirconium phosphate layer with a good mechanical adherence to the support. The

  20. Decontamination and recycle of zirconium pressure tubes from Pressurized Heavy Water Reactor

    International Nuclear Information System (INIS)

    Gantayet, L.M.; Verma, R.; Remya Devi, P.S.; Banerjee, S.; Kotak, V.; Raha, A.; Sandeep, K.C.; Joshi, Shreeram W.; Lali, A.M.

    2009-01-01

    An ion exchange process has been developed for decontamination of zirconium pressure tubes from Pressurized Heavy Water Reactor and recycling of neutronically improved zirconium. Distribution coefficient, equilibrium isotherm, kinetic and breakthrough data were used to develop the separation process. Effect of gamma radiation on indigenous resins was also studied to assess their suitability in high radiation field. (author)