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Sample records for zirconium oxide formed

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

    Directory of Open Access Journals (Sweden)

    Silva G.L.J.P. da

    2002-01-01

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

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

    Science.gov (United States)

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

    2014-01-01

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

  3. 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

  4. 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)

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  8. 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.

  9. 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

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

    International Nuclear Information System (INIS)

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

    1989-01-01

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

  11. 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

  12. 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.

  13. 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)

  14. 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

  15. 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.

  16. 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

  17. 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)

  18. 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.

  19. 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

  20. 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

  1. 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.

  2. 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)

  3. 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

  4. 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.

  5. 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

  6. 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)

  7. 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.

  8. 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)

  9. 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

  10. 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.

  11. 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.

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

    International Nuclear Information System (INIS)

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

    2007-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-01

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

  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. Variation on wettability of anodic zirconium oxide nanotube surface

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  16. 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...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  19. 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)

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

    International Nuclear Information System (INIS)

    Wang Luning; Luo Jingli

    2011-01-01

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

  1. 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.

  2. 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

  3. 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.

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

    Science.gov (United States)

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

    2017-02-01

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

  6. 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.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  8. 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.

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

    International Nuclear Information System (INIS)

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

    1987-01-01

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

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

    International Nuclear Information System (INIS)

    Godlewski, J.

    1990-07-01

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

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

    Science.gov (United States)

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

    2014-11-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-11-15

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

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

    International Nuclear Information System (INIS)

    Ribeiro, S.

    1991-05-01

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

  15. 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

  16. 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.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-15

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Bererd, N

    2003-07-01

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

  20. 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

  1. Extensive Bone Reaction From Catastrophic Oxidized Zirconium Wear.

    Science.gov (United States)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

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

    1976-02-01

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

  3. Oxidized zirconium: a potentially longer lasting hip implant

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  4. Synthesis of amorphous zirconium oxide with luminescent characteristics

    International Nuclear Information System (INIS)

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

    2004-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2011-01-01

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

  6. 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.

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  8. 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

  9. 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.

  10. 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.

  11. Hydrogenation and high temperature oxidation of Zirconium claddings

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Science.gov (United States)

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

    2016-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-09-15

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

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

    Science.gov (United States)

    Coleman, Nichola J; Li, Qiu

    2013-01-01

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

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

    Science.gov (United States)

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

    2017-02-01

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

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

    International Nuclear Information System (INIS)

    Ploc, R.A.

    1989-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  18. Zirconium phosphate waste forms for low-temperature stabilization of cesium-137-containing waste streams

    International Nuclear Information System (INIS)

    Singh, D.; Wagh, A.S.; Tlustochowicz.

    1996-04-01

    Novel chemically bonded phosphate ceramics are being developed and fabricated for low-temperature stabilization and solidification of waste streams that are not amenable to conventional high-temperature stabilization processes because volatiles are present in the wastes. A composite of zirconium-magnesium phosphate has been developed and shown to stabilize ash waste contaminated with a radioactive surrogate of 137 Cs. Excellent retainment of cesium in the phosphate matrix system was observed in Toxicity Characteristic Leaching Procedure tests. This was attributed to the capture of cesium in the layered zirconium phosphate structure by intercalation ion-exchange reaction. But because zirconium phosphate has low strength, a novel zirconium/magnesium phosphate composite waste form system was developed. The performance of these final waste forms, as indicated by compression strength and durability in aqueous environments, satisfy the regulatory criteria. Test results indicate that zirconium-magnesium-phosphate-based final waste forms present a viable technology for treatment and solidification of cesium-contaminated wastes

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  20. Fabrication of NiO/zirconium oxide nanofibers by electrospinning

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-12-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-04-15

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

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

    International Nuclear Information System (INIS)

    Pecheur, Dominique

    1993-01-01

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

  4. 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

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

    International Nuclear Information System (INIS)

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

    1987-08-01

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

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

    International Nuclear Information System (INIS)

    Seo, E.S.M.

    1983-01-01

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

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

    International Nuclear Information System (INIS)

    Mengatti, J.

    1980-01-01

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

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

    International Nuclear Information System (INIS)

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

    1994-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1994-06-01

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

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

    International Nuclear Information System (INIS)

    Coleman, Nichola J.; Li, Qiu

    2013-01-01

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

  11. Growth and characterization of oxide layers on zirconium alloys

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-15

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

  14. 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...

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

    Science.gov (United States)

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

    2015-12-01

    Charnley low-friction torque total hip arthroplasty (THA) remains the gold standard in THA. The main cause for failure is wear of the socket. Highly crosslinked polyethylene (HXLPE) has been associated with reduced wear rates. Also, oxidized zirconium has shown in vitro reduced wear rates. However, to our knowledge, there are no data comparing oxidized zirconium femoral heads with metal heads against HXLPE or ultrahigh-molecular-weight polyethylene (UHMWPE) when 22.25-mm bearings were used, which was the same size that performed so well in Charnley-type THAs. We hypothesized that after a minimal 4-year followup (1) use of HXLPE would result in lower radiographic wear than UHMWPE when articulating with a stainless steel head or with an oxidized zirconium head; (2) use of oxidized zirconium would result in lower radiographic wear than stainless steel when articulating with UHMWPE and HXLPE; and (3) there would be no difference in terms of Merle d'Aubigné scores between the bearing couple combinations. One hundred patients were randomized to receive cemented THA with either oxidized zirconium or a stainless steel femoral head. UHMWPE was used in the first 50 patients, whereas HXLPE was used in the next 50 patients. There were 25 patients in each of the four bearing couple combinations. All other parameters were identical in both groups. Complete followup was available in 86 of these patients. Femoral head penetration was measured using a validated computer-assisted method dedicated to all-polyethylene sockets. Clinical results were compared between the groups using the Merle d'Aubigné score. In the UHMWPE series, the median steady-state penetration rate from 1 year onward was 0.03 mm/year (range, 0.003-0.25 mm/year) in the oxidized zirconium group versus 0.11 mm/year (range, 0.03-0.29 mm/year) in the metal group (difference of medians 0.08, p zirconium group versus 0.05 mm/year (range, -0.39 to 0.11 mm/year) in the metal group (difference of medians 0.03, p

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-08-15

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

  17. 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)

  18. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1959-07-01

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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

  1. 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

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

    Science.gov (United States)

    Al-Thobity, Ahmad M

    2016-06-01

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

  3. Zirconium sponge and other forms of virgin metal for nuclear applications - approved standard 1973

    International Nuclear Information System (INIS)

    Anon.

    1975-01-01

    This specification covers virgin zirconium metal commonly designated as sponge because of its porous, sponge-like texture, but it may also take other forms such as chunklets. One grade is described which is designated as reactor grade R-1, suitable for use in nuclear applications. The most important characteristic of the reactor grade is its low nuclear cross section as achieved by removal of hafnium and careful quality control in manufacturing procedures to prevent contamination with other high cross section materials

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

    International Nuclear Information System (INIS)

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

    1977-10-01

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

  5. Process for forming seamless tubing of zirconium or titanium alloys from welded precursors

    International Nuclear Information System (INIS)

    Sabol, G.P.; Barry, R.F.

    1987-01-01

    A process is described for forming seamless tubing of a material selected from zirconium, zirconium alloys, titanium, and titanium alloys, from welded precursor tubing of the material, having a heterogeneous structure resulting from the welding thereof. The process consists of: heating successive axial segments of the welded tubing, completely through the wall thereof, including the weld, to uniformly transform the heterogeneous, as welded, material into the beta phase; quenching the beta phase tubing segments, the heating and quenching effected sufficiently rapid enough to produce a fine sized beta grain structure completely throughout the precursor tubing, including the weld, and to prevent growth of beta grains within the material larger than 200 micrometers in diameter; and subsequently uniformly deforming the quenched precursor tubing by cold reduction steps to produce a seamless tubing of final size and shape

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

    Science.gov (United States)

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

    2009-01-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-11-15

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

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

    International Nuclear Information System (INIS)

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

    1992-01-01

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

  12. 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

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

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

    International Nuclear Information System (INIS)

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

    1988-01-01

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

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

    Institute of Scientific and Technical Information of China (English)

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

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

    Science.gov (United States)

    Nejatidanesh, Farahnaz; Savabi, Omid; Shahtoosi, Mojtaba

    2013-08-01

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

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

    Directory of Open Access Journals (Sweden)

    Sialini P.

    2016-03-01

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

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

    Science.gov (United States)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

    Chosson, Raphael

    2014-01-01

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

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

    Science.gov (United States)

    Karidakis, George K; Karachalios, Theofilos

    2015-12-01

    Osteolysis resulting from wear debris production from the bearing surfaces is a major factor limiting long-term survival of hip implants. Oxidized zirconium head on crosslinked polyethylene (XLPE) is a modern bearing coupling. However, midterm in vivo wear data of this coupling are not known. The purpose of this study was to investigate in vivo whether the combination of an oxidized zirconium femoral head on XLPE produces less wear than a ceramic head on XLPE or a ceramic head on conventional polyethylene (CPE) couplings and whether any of these bearing combinations results in higher hip scores. Between 2003 and 2007, we performed 356 total hip arthroplasties in 288 patients; of those, 199 (69.1%) patients (199 hips) were enrolled in what began as a randomized trial. Unfortunately, after the 57(th) patient, the randomization process was halted because of patients' preference for the oxidized zirconium bearing instead of the ceramic after (as they were informed by the consent form), and after that, alternate allocation to the study groups was performed. Hips were allocated into four groups: in Group A, a 28-mm ceramic head on CPE was used; in Group B, a 28-mm ceramic head on XLPE; in Group C, a 28-mm Oxinium head on XLPE; and in Group D, a 32-mm Oxinium head on XLPE. The authors prospectively collected in vivo wear data (linear wear, linear wear rate, volumetric wear, and volumetric wear rate) using PolyWare software. Preoperative and postoperative clinical data, including Harris and Oxford hip scores, were also collected at regular intervals. Of those patients enrolled, 188 (95%) were available for final followup at a minimum of 7 years (mean, 9 years; range, 7-12 years). All bearing surfaces showed a varying high bedding-in effect (plastic deformation of the liner) up to the second postoperative year. At 5 years both oxidized zirconium on XLPE groups showed lower (p zirconium on XLPE groups also showed lower (p zirconium groups were compared, no differences were

  3. 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

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

    Science.gov (United States)

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

    2017-10-01

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

  5. 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)

  6. 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)

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

    Directory of Open Access Journals (Sweden)

    V. K. Shatalov

    2014-01-01

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

  8. Expanded heat treatment to form residual compressive hoop stress on inner surface of zirconium alloy tubing

    International Nuclear Information System (INIS)

    Megata, Masao

    1997-01-01

    A specific heat treatment process that introduces hoop stress has been developed. This technique can produce zirconium alloy tubing with a residual compressive hoop stress near the inner surface by taking advantage of the mechanical anisotropy in hexagonal close-packed zirconium crystal. Since a crystal having its basal pole parallel to the tangential direction of the tubing is easier to exhibit plastic elongation under the hoop stress than that having its basal pole parallel to the radial direction, the plastic and elastic elongation can coexist under a certain set of temperature and hoop stress conditions. The mechanical anisotropy plays a role to extend the coexistent stress range. Thus, residual compressive hoop stress is formed at the inner surface where more plastic elongation occurs during the heat treatment. This process is referred to as expanded heat treatment. Since this is a fundamental crystallographic principle, it has various applications. The application to improve PCI/SCC (pellet cladding interaction/stress corrosion cracking) properties of water reactor fuel cladding is promising. Excellent results were obtained with laboratory-scale heat treatment and an out-reactor iodine SCC test. These results included an extension of the time to SCC failure. (author)

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2011-01-01

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

  11. 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.

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

    Science.gov (United States)

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

    2017-02-01

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

  13. 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.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    International Nuclear Information System (INIS)

    Desmaison, Jean; Billy, Michel

    1976-01-01

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

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

    International Nuclear Information System (INIS)

    Orlans, Patrick

    1987-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-06-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    Science.gov (United States)

    Camilleri, J; Cutajar, A; Mallia, B

    2011-08-01

    Zirconium oxide can be added to dental materials rendering them sufficiently radiopaque. It can thus be used to replace the bismuth oxide in mineral trioxide aggregate (MTA). Replacement of Portland cement with 30% zirconium oxide mixed at a water/cement ratio of 0.3 resulted in a material with adequate physical properties. This study aimed at investigating the microstructure, pH and leaching in physiological solution of Portland cement replaced zirconium oxide at either water-powder or water-cement ratios of 0.3 for use as a root-end filling material. The hydration characteristics of the materials which exhibited optimal behavior were evaluated. Portland cement replaced by zirconium oxide in varying amounts ranging from 0 to 50% in increments of 10 was prepared and divided into two sets. One set was prepared at a constant water/cement ratio while the other set at a constant water/powder ratio of 0.3. Portland cement and MTA were used as controls. The materials were analyzed under the scanning electron microscope (SEM) and the hydration products were determined. X-ray energy dispersive analysis (EDX) was used to analyze the elemental composition of the hydration products. The pH and the amount of leachate in Hank's balanced salt solution (HBSS) were evaluated. A material that had optimal properties that satisfied set criteria and could replace MTA was selected. The microstructure of the prototype material and Portland cement used as a control was assessed after 30 days using SEM and atomic ratio diagrams of Al/Ca versus Si/Ca and S/Ca versus Al/Ca were plotted. The hydration products of Portland cement replaced with 30% zirconium oxide mixed at water/cement ratio of 0.3 were calcium silicate hydrate, calcium hydroxide and minimal amounts of ettringite and monosulphate. The calcium hydroxide leached in HBSS solution resulted in an increase in the pH value. The zirconium oxide acted as inert filler and exhibited no reaction with the hydration by-products of Portland

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

    Science.gov (United States)

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

    2011-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-08-31

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

  2. 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

  3. Zirconium oxide based ceramic solid electrolytes for oxygen detection

    International Nuclear Information System (INIS)

    Caproni, Erica

    2007-01-01

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

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

    International Nuclear Information System (INIS)

    Mazeres, Benoit

    2013-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Sumita Rani

    2016-04-01

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

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

    International Nuclear Information System (INIS)

    Rivera Montalvo, Teodoro; Furetta, Claudio

    2008-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-01-01

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

  9. 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.

  10. Rare earth zirconium oxide buffer layers on metal substrates

    Science.gov (United States)

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

    2001-01-01

    A laminate article comprises a substrate and a biaxially textured (RE.sub.x A.sub.(1-x)).sub.2 O.sub.2-(x/2) buffer layer over the substrate, wherein 0layer can be deposited using sol-gel or metal-organic decomposition. The laminate article can include a layer of YBCO over the (RE.sub.x A.sub.(1-x)).sub.2 O.sub.2-(x/2) buffer layer. A layer of CeO.sub.2 between the YBCO layer and the (RE.sub.x A.sub.(1-x)).sub.2 O.sub.2-(x/2) buffer layer can also be include. Further included can be a layer of YSZ between the CeO.sub.2 layer and the (RE.sub.x A.sub.(1-x)).sub.2 O.sub.2-(x/2) buffer layer. The substrate can be a biaxially textured metal, such as nickel. A method of forming the laminate article is also disclosed.

  11. 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

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

    Directory of Open Access Journals (Sweden)

    Saif Ali Chaudhry

    2017-06-01

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

  13. The phases formed by the dehydration of disodium zirconium (IV) bis(orthophosphate) trihydrate and their ion-exchange behavior

    International Nuclear Information System (INIS)

    Inoue, Yasushi; Yamada, Yoshimune

    1982-01-01

    The phase transformation of Na 2 Zr(PO 4 ) 2 .3H 2 O which had been obtained from zirconium (IV) bis(hydrogenphosphate) monohydrate(α-zirconium phosphate), prepared by the direct precipitation method, was studied by means of gravimetry, X-ray analysis, and acid-base titration. When the material was heated for 2d, it was transformed to a monohydrate at 80 0 C and then successively to three anhydrous phases, depending on the temperature. The monohydrate was also formed by letting the trihydrate stand over P 2 O 5 at room temperature for longer than two weeks. The processes were confirmed to be irreversible by an examination of the rehydration behavior, from which the conditions of the storage of five modifications of disodium zirconium (IV) bis(orthophosphate) were established. It is of special interest that the second anhydrous phase reverted to the first one when it was allowed to stand at room temperature in air or in a desiccator. The rate of the reversion decreased with the temperature of heat-treatment and with a decrease in the relative humidity of the surroundings. The difference between the present results and Clearfield's was clarified and attributed mainly to the difference in the crystallinity of the starting α-zirconium phosphate. (author)

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

    International Nuclear Information System (INIS)

    Cabrera-Salcedo, A.

    2012-01-01

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

    Parise, M.

    1996-12-01

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

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

    NARCIS (Netherlands)

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

    1982-01-01

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

  18. 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

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

    Science.gov (United States)

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

    2009-01-01

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

  20. 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.

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

    International Nuclear Information System (INIS)

    Kohli, R.

    1980-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-09-15

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2011-05-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

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

    Science.gov (United States)

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

    2017-10-15

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

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  8. Solid state diffusion in zirconium-copper and zirconium-nickel systems. Study of the intermetallic compounds formed; Diffusion a l'etat solide dans les systemes zirconium-cuivre et zirconium-nickel. Etude des composes intermetalliques formes

    Energy Technology Data Exchange (ETDEWEB)

    Meny, L; Champigny, M [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1968-07-01

    Solid state diffusion has been provoked in pure Zr-Cu and Zr-Ni metal couples. The tests were carried out in the following experimental conditions : the samples were maintained at a mechanical pressure of 30 kg/cm{sup 2}; annealing was carried out in a secondary vacuum during 100 and 500 hours, at temperatures of between 650 C and 900 C. In all cases, a diffusion zone made up of several parallel layers was formed. The various intermetallic compounds have been studied by metallography (optical microscopy and micro-hardness) X-ray diffraction and micro-analysis with an electronic probe. In the Zr-Cu system, six compounds have been determined, Zr{sub 2}Cu, ZrCu, Zr{sub 2}Cu{sub 3}, ZrCu{sub 4} and ZrCu{sub 5}. These results confirm a recent publication mentioning for the first time the existence of ZrCu{sub 5} and demonstrating the formulae ZrCu{sub 3} and ZrCu{sub 4}. In a similar manner, we have found six compounds, stable at room temperature, in the Zr-Ni system: these are Zr{sub 2}Ni, ZrNi, Zr{sub 7}Ni{sub 10}, ZrNi{sub 3}, ZrNi{sub 4} and ZrNi{sub 5}; the results of American workers are confirmed for four of these compounds; however we identify as ZrNi{sub 3} and ZrNi{sub 4} the compounds for which they proposed the formulae Zr{sub 2}Ni{sub 5} and Zr{sub 2}Ni{sub 7}. A comparison of these results suggests that the two systems ZrCu and ZrNi have the same type of equilibrium diagrams. (authors) [French] Des diffusions a l'etat solide ont ete effectuees entre les couples de metaux purs Zr-Cu et Zr-Ni. Les essais ont eu lieu dans les conditions experimentales suivantes: les echantillons ont ete maintenus par une pression mecanique de 3O kg/cm{sup 2}; les recuits ont ete effectues sous vide secondaire pendant des temps de 100 et 500 heures, a des temperatures comprises entre 650 C et 900 C. Dans tous les cas, il y a eu formation d'une zone de diffusion formee de plusieurs couches paralleles. Les differents composes intermetalliques ont ete etudies par metallographie

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

    Science.gov (United States)

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

    2013-01-01

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

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

    Science.gov (United States)

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

    2014-10-01

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

  11. 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.

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

    OpenAIRE

    Felemban, Nayef H.; Ebrahim, Mohamed I.

    2017-01-01

    Background The purpose of this in-vitro study was to examine the effect of incorporating different concentrations of Zirconium oxide-Titanium dioxide (ZrO2-TiO2) nanoparticles, which can have antibacterial properties, on the mechanical properties of an orthodontic adhesive. Methods ZrO2-TiO2 (Zirconium oxide, HWNANO, Hongwu International Group Ltd, China) -Titanium dioxide, Nanoshell, USA) nanopowder were incorporated into orthodontic adhesive (Transbond XT, 3?M Unitek, Monrovia, USA) with di...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-12-30

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

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

    International Nuclear Information System (INIS)

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

    2002-01-01

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

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

    Science.gov (United States)

    intermediate and final products, and also during the calculation of approximate heat values of their formation, the passage of the reaction is confirmed...for obtaining TiC, and ZrC through the stage of intermediate oxides Ti2O3, Ti3O5, TiO and Zr2O3, ZrO, respectively and also for the reaction of...forming carbides of V (from V2O3 + 5C), of Nb and Ta (from Nb2O5 + 7C and Ta205 + 7C) through the stage of intermediate oxides VO, V4O and TaO2, Ta4O. The

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

    Science.gov (United States)

    Aziz, Md. Abdul; Shanmugam, Sangaraju

    2017-01-01

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

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

    International Nuclear Information System (INIS)

    Do, N.-L.

    2012-01-01

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

  19. 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.

  20. 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.

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2017-02-28

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

  3. 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

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    Science.gov (United States)

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

    2014-03-01

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

  6. 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

  7. 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)

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

    Science.gov (United States)

    Guerreiro-Tanomaru, Juliane Maria; Trindade-Junior, Adinael; Cesar Costa, Bernardo; da Silva, Guilherme Ferreira; Drullis Cifali, Leonardo; Basso Bernardi, Maria Inês

    2014-01-01

    The aim of the present study was to evaluate the antibiofilm activity against Enterococcus faecalis, compressive strength. and radiopacity of Portland cement (PC) added to zirconium oxide (ZrO2), as radiopacifier, with or without nanoparticulated zinc oxide (ZnO). The following experimental materials were evaluated: PC, PC + ZrO2, PC + ZrO2 + ZnO (5%), and PC + ZrO2 + ZnO (10%). Antibiofilm activity was analyzed by using direct contact test (DCT) on Enterococcus faecalis biofilm, for 5 h or 15 h. The analysis was conducted by using the number of colony-forming units (CFU/mL). The compressive strength was performed in a mechanical testing machine. For the radiopacity tests, the specimens were radiographed together with an aluminium stepwedge. The results were submitted to ANOVA and Tukey tests, with level of significance at 5%. The results showed that all materials presented similar antibiofilm activity (P > 0.05). The addition of nanoparticulated ZnO decreased the compressive strength of PC. All materials presented higher radiopacity than pure PC. It can be concluded that the addition of ZrO2 and ZnO does not interfere with the antibiofilm activity and provides radiopacity to Portland cement. However, the presence of ZnO (5% or 10%) significantly decreased the compressive strength of the materials. PMID:25431798

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

    Science.gov (United States)

    Qiu, Hui; Liang, Chen; Zhang, Xiaolin; Chen, Mindong; Zhao, Yunxia; Tao, Tao; Xu, Zhengwen; Liu, Gang

    2015-09-23

    Advanced removal of phosphate by low-cost adsorbents from municipal wastewater or industrial effluents is an effective and economic way to prevent the occurrence of eutrophication. Here, we proposed a novel method to immobilize hydrous zirconium oxide nanoparticle within quaternary-aminated wheat straw, and obtained an inexpensive, eco-friendly nanocomposite Ws-N-Zr. The biomass-based Ws-N-Zr exhibited higher preference toward phosphate than commercial anion exchanger IRA-900 when competing sulfate ions coexisted at relatively high levels. Such excellent performance of Ws-N-Zr resulted from its specific hybrid structure, the quaternary ammonium groups bonded on the host favor the preconcentration of phosphate ions inside the wheat straw based on Donnan effect, and the encapsulated HZO nanoparticle exhibits preferable sequestration of phosphate ions through specific interaction, as further demonstrated by FTIR and X-ray photoelectron spectroscopy. Cycle adsorption and regeneration experiments demonstrated that Ws-N-Zr could be employed for repeated use without significant capacity loss, when the binary NaOH-NaCl solution was employed as the regenerant. The influence of solution pH and contact time was also examined. The results suggested that Ws-N-Zr has a great potential in efficient removal of phosphate in contaminated waters.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2012-07-15

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

    Davila N, M. L.

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2003-05-01

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

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

    Science.gov (United States)

    Viapiana, R; Flumignan, D L; Guerreiro-Tanomaru, J M; Camilleri, J; Tanomaru-Filho, M

    2014-05-01

    To evaluate the physicochemical and mechanical properties of Portland cement-based experimental sealers (ES) with different radiopacifying agents (zirconium oxide and niobium oxide micro- and nanoparticles) in comparison with the following conventional sealers: AH Plus, MTA Fillapex and Sealapex. The materials were tested for setting time, compressive strength, flow, film thickness, radiopacity, solubility, dimensional stability and formaldehyde release. Data were subjected to anova and Tukey tests (P 0.05) and lower solubility when compared with MTA Fillapex and Sealapex (P Portland cement-based experimental endodontic sealers presented physicochemical properties according to the specifications no 57 ANSI/ADA (ADA Professional Product Review, 2008) and ISO 6876 (Dentistry - Root Canal Sealing Materials, 2012, British Standards Institution, London, UK). The sealers had setting times and flow ability that was adequate for clinical use, satisfactory compressive strength and low solubility. Additional studies should be carried out with the purpose of decreasing the film thickness and to determine the ideal ratio of radiopacifying agents in Portland cement-based root canal sealers. © 2013 International Endodontic Journal. Published by John Wiley & Sons Ltd.

  15. Introduction of polycrystal constitutive laws in a finite element code with applications to zirconium forming

    International Nuclear Information System (INIS)

    Maudlin, P.J.; Tome, C.N.; Kaschner, G.C.; Gray, G.T. III

    1998-01-01

    In this work the authors simulate the compressive deformation of heavily textured zirconium sheet using a finite element code with the constitutive response given by a polycrystal self-consistent model. They show that the strong anisotropy of the response can be explained in terms of the texture and the relative activity of prismatic (easy) and pyramidal (hard) slip modes. The simulations capture the yield anisotropy observed for so-called through-thickness and in-plane compression tests in terMs of the loading curves and final specimen geometries

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Maciej Sowa

    2018-05-01

    Full Text Available Zr is a valve metal, the biocompatibility of which is at least on par with Ti. Recently, numerous attempts of the formation of bioactive coatings on Zr by plasma electrolytic oxidation (PEO in solutions that were based on calcium acetate and calcium β-glycerophosphate were made. In this study, the direct current (DC PEO of commercially pure zirconium in the solutions that contained Ca(H2PO22, Ca(HCOO2, and Mg(CH3COO2 was investigated. The treatment was conducted at 75 mA/cm2 up to 200, 300, or 400 V. Five process stages were discerned. The treatment at higher voltages resulted in the formation of oxide layers that had Ca/P or (Mg+Ca/P ratios that were close to that of hydroxyapatite (Ca/P = 1.67, determined by SEM/EDX. The corrosion resistance studies were performed using electrochemical impedance spectroscopy (EIS and DC polarization methods. R(Q[R(QR] circuit model was used to fit the EIS data. In general, the coatings that were obtained at 200 V were the most corrosion resistant, however, they lacked the porous structure, which is typical for PEO coatings, and is sought after in the biomedical applications. The treatment at 400 V resulted in the formation of the coatings that were more corrosion resistant than those that were obtained at 300 V. This was determined mainly by the prevailing plasma regime at the given process voltage. The pitting resistance of Zr was also improved by the treatment, regardless of the applied process conditions.

  18. 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)

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

    International Nuclear Information System (INIS)

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

    1977-12-01

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

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

    International Nuclear Information System (INIS)

    Pawel, R.E.

    1976-10-01

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

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

    Science.gov (United States)

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

    2017-02-01

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

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

    Science.gov (United States)

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

    2015-03-02

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

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

    Science.gov (United States)

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

    2016-10-20

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

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

    Science.gov (United States)

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-15

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  7. 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.

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Science.gov (United States)

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

    2015-12-01

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

  10. Uranium oxidation: characterization of oxides formed by reaction with water

    International Nuclear Information System (INIS)

    Fuller, E.L. Jr.; Smyrl, N.R.; Condon, J.B.; Eager, M.H.

    1983-01-01

    Three different uranium oxide samples have been characterized with respect to the different preparation techniques. Results show that the water reaction with uranium metal occurs cyclically forming laminar layers of oxide which spall off due to the strain at the oxide/metal interface. Single laminae are released if liquid water is present due to the prizing penetration at the reaction zone. The rate of reaction of water with uranium is directly proportional to the amount of adsorbed water on the oxide product. Rapid transport is effected through the open hydrous oxide product. Dehydration of the hydrous oxide irreversibly forms a more inert oxide which cannot be rehydrated to the degree that prevails in the original hydrous product of uranium oxidation with water. 27 figures

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

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

    International Nuclear Information System (INIS)

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

    2000-01-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2008-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-11-15

    The reduction behaviors of ZrO{sub 2}, Li{sub 2}ZrO{sub 3} and (U,Pu,Zr)O{sub 2} in a LiCl–Li{sub 2}O salt bath at 923 K were investigated. This study was conducted as part of a feasibility study on the pyrochemical treatment of damaged fuel debris generated by severe accidents at light water reactors. It was demonstrated in electrolytic reduction tests that the uranium in synthetic corium specimens of (U,Pu,Zr)O{sub 2} with various ZrO{sub 2} contents could be reduced to the metallic form and that part of the zirconium was converted to Li{sub 2}ZrO{sub 3}. Zirconium metal and Li{sub 2}ZrO{sub 3} were obtained by the reduction of ZrO{sub 2}. The reduction of Li{sub 2}ZrO{sub 3} did not proceed even in LiCl containing no Li{sub 2}O. Moreover, the stable chemical forms of the ZrO{sub 2}–Li{sub 2}O complex oxide were investigated as a function of the Li{sub 2}O concentration in LiCl. ZrO{sub 2} was converted to Li{sub 2}ZrO{sub 3} at a Li{sub 2}O concentration of 0.018 wt%. As the Li{sub 2}O concentration was increased, Li{sub 2}ZrO{sub 3} was converted to Li{sub 6}Zr{sub 2}O{sub 7} and then to Li{sub 8}ZrO{sub 6}. It is suggested that the removal of Li{sub 2}ZrO{sub 3} from the reduction product is a key point in the pyrochemical treatment of corium. - Highlights: • The uranium in (U,Pu,Zr)O{sub 2} could be reduced to the metallic form in LiCl–Li{sub 2}O. • Part of the zirconium was converted to Li{sub 2}ZrO{sub 3} during electrolytic reduction. • Li{sub 6}Zr{sub 2}O{sub 7} and Li{sub 8}ZrO{sub 6} formed at high Li{sub 2}O concentrations in LiCl.

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

    International Nuclear Information System (INIS)

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

    1981-01-01

    An improved method of producing a composite nuclear fuel container is described which comprises a casing or fuel sheath of zirconium or its alloy with a lining cladding of deposited copper superimposed over the inside surface of the zirconium or alloy and a layer of oxide of the zirconium or alloy formed on the inside surface of the casing or sheath. (U.K.)

  16. 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.

  17. Determination of the stability of the uranyl ion sipped in τ-hydrogen phosphate of zirconium in sodic form

    International Nuclear Information System (INIS)

    Ordonez R, E.; Fernandez V, S.M.; Drot, R.; Simoni, E.

    2005-01-01

    The stability of the uranyl sipped in the zirconium τ-hydrogen phosphate in sodic form (τ-NaZrP), was carried out characterizing the complexes formed by Laser spectroscopy in the visible region and by X-ray photoelectron spectroscopy. The material was prepared by a new synthesis technique working in nitrogen atmosphere and to low temperatures. The sorption of the uranyl ion was made in acid media with concentrations of 10 -4 and 10 -5 of uranyl nitrate and with ion forces of 0.1 and 0.5 M of NaClO 4 . The spectra of induced fluorescence with laser (TRLFS) show that the uranyl is fixed in very acid media in three well differentiated species, to pH less acid, the specie of long half life disappears and are only those of short half life. The results of the binding energy obtained by XPS indicate that the binding energy of the uranyl confer it a stable character to the complex formed in the τ-NaZP, that makes to this material appropriate to retain to the uranyl in solution to high ion forces and in acid media. (Author)

  18. 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

  19. 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.

  20. 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

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

    International Nuclear Information System (INIS)

    Mayuzumi, Masami; Fujita, Tomonari

    1994-01-01

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

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

    International Nuclear Information System (INIS)

    Dali, Yacoub

    2007-01-01

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

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

    Science.gov (United States)

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

    2015-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2004-07-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Zielke, U.

    1988-10-15

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

  6. 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.

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

    Science.gov (United States)

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

    2018-05-08

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

  8. 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

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

    International Nuclear Information System (INIS)

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

    2001-01-01

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

  10. Low temperature synthesis of {tau}-zirconium hydrogenophosphate [{tau}-Zr(HPO{sub 4}){sub 2}] and a new sodic form obtained by ion exchange

    Energy Technology Data Exchange (ETDEWEB)

    Fernandez-Valverde, Suilma M., E-mail: suilma.fernandez@inin.gob.mx [Depto. de Quimica, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico); Contreras-Ramirez, Aida [Depto. de Quimica, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico); Depto. de Tecnologia de Materiales, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico); Facultad de Ciencias, Universidad Autonoma del Estado de Mexico, Piedras Blancas El Cerrillo, Tlachaloya Estado de Mexico, CP.5000 (Mexico); Ordonez-Regil, Eduardo [Depto. de Quimica, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico); Fernandez-Garcia, M. Eufemia [Depto. de Tecnologia de Materiales, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico); Perez-Alvarez, Mario [Depto. de Ambientales, Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, Mexico D.F. C.P. 11801 (Mexico)

    2013-02-15

    A new method for the synthesis of 3-D {tau}-zirconium hydrogenophosphate (TZP) was developed using solid-state reactions at low temperature and atmospheric pressure in a nitrogen atmosphere in a two-hour reaction time. The characterization of the compound was performed using X-ray diffraction, infrared spectroscopy, scanning electron microscopy, energy dispersive X-ray spectroscopy, differential scanning calorimetric, thermochemical analysis and X-ray photoelectron spectroscopy. A sodic form of the compound obtained by the immersion of TZP in a sodium hydroxide solution was characterized using the same techniques along with neutron activation analysis. The XPS spectra confirm the binding energy value for sodium-oxygen, and the XRD diffraction reveals the formation of a new sodium compound. - Graphical abstract: DRX, XPS and MEB of {tau}-zirconium hydrogenophosphate and its sodic form on the surface of TZP. Highlights: Black-Right-Pointing-Pointer New method for the syntheses of 3-D {tau}-zirconium hydrogenophosphate (TZP). Black-Right-Pointing-Pointer A sodic form of the TZP was obtained by the immersion of TZP in a sodium hydroxide. Black-Right-Pointing-Pointer The sodium compound is only formed on the TZP surface.

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

    Science.gov (United States)

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

    2014-01-01

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

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

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

    International Nuclear Information System (INIS)

    Widjaja, Yuniarto; Musgrave, Charles B.

    2002-01-01

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

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

    Science.gov (United States)

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

    2018-04-01

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

  15. 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.)

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

    International Nuclear Information System (INIS)

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

    1996-01-01

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

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  18. Bulk glass formation and crystallization in zirconium based bulk metallic glass forming alloys

    International Nuclear Information System (INIS)

    Savalia, R.T.; Neogy, S.; Dey, G.K.; Banerjee, S.

    2002-01-01

    The microstructures of Zr based metallic glasses produced in bulk form have been described in the as-cast condition and after crystallization. Various microscopic techniques have been used to characterize the microstructures. The microstructure in the as-cast condition was found to contain isolated crystals and crystalline aggregates embedded in the amorphous matrix. Quenched-in nuclei of crystalline phases were found to be present in fully amorphous regions. These glasses after crystallization gave rise to nanocrystalline solids. (author)

  19. 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

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

    Science.gov (United States)

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

    2015-07-29

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

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

    Directory of Open Access Journals (Sweden)

    Qifeng Lu

    2015-07-01

    Full Text Available A powerful characterization technique, pulse capacitance-voltage (CV technique, was used to investigate oxide traps before and after annealing for lanthanide zirconium oxide thin films deposited on n-type Si (111 substrates at 300 °C by liquid injection Atomic Layer Deposition (ALD. The results indicated that: (1 more traps were observed compared to the conventional capacitance-voltage characterization method in LaZrOx; (2 the time-dependent trapping/de-trapping was influenced by the edge time, width and peak-to-peak voltage of a gate voltage pulse. Post deposition annealing was performed at 700 °C, 800 °C and 900 °C in N2 ambient for 15 s to the samples with 200 ALD cycles. The effect of the high temperature annealing on oxide traps and leakage current were subsequently explored. It showed that more traps were generated after annealing with the trap density increasing from 1.41 × 1012 cm−2 for as-deposited sample to 4.55 × 1012 cm−2 for the 800 °C annealed one. In addition, the leakage current density increase from about 10−6 A/cm2 at Vg = +0.5 V for the as-deposited sample to 10−3 A/cm2 at Vg = +0.5 V for the 900 °C annealed one.

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

    International Nuclear Information System (INIS)

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

    2016-01-01

    An accurate and precise determination of terbutaline has been carried out using a glassy carbon electrode (GCE) modified with a composite of multi-walled carbon nanotubes (MWCNTs) and nanoparticles of zirconium oxide (ZrO_2NPs). Energy dispersive X-ray and scanning electron microscopic techniques were utilized for the characterization of the composite layer. Terbutaline exhibited a broad oxidation peak at 770 mV on a GCE. However, MWCNTs/GCE presented an electrocatalytic effect toward the oxidation of terbutaline with a better anodic peak at 660 mV. Furthermore, the electrochemical behavior of terbutaline has greatly been improved at a GCE modified with a composite of MWCNTs and nanoparticles of ZrO_2. The ZrO_2NPs/MWCNTs/GCE exhibited a sharp anodic wave at 645 mV with a large enhancement of the current response for terbutaline. Square wave voltammetry (SWV) was performed for the determination of terbutaline at ZrO_2NPs/MWCNTs/GCE. A linear plot was obtained for the current responses of terbutaline against concentrations in the range of 10–160 nM yielding a detection limit of 2.25 nM (based on 3S_b/m). Improved voltammetric behavior, long-time stability and good reproducibility were obtained for terbutaline at the proposed electrode. A mean recovery of 101.2% with an RSD% of 1.9 was obtained for the analysis of the drug formulation. The accurate and precise quantification of terbutaline makes the ZrO_2NPs/MWCNTs/GCE system of great interest for monitoring its therapeutic use. - Graphical abstract: A sensitive determination of terbutaline in pharmaceuticals and urine samples using a composite electrode based on zirconium oxide nanoparticles. Display Omitted - Highlights: • A composite electrode was prepared using nanoparticles of ZrO_2 and MWCNTs. • The ZrO_2NPs/MWCNTs/GCE has greatly improved the voltammetry of terbutaline • The proposed electrode enabled a detection limit of 2.25 nM. • The proposed electrode exhibited good reproducibility and long

  3. 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.)

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

    Directory of Open Access Journals (Sweden)

    Heriberto Esteban Benito

    2015-01-01

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

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

    Science.gov (United States)

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

    2017-08-01

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

  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. 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

  8. Corium Oxidation at Temperatures Above 2000 K

    International Nuclear Information System (INIS)

    Hagrman, Donald L.; Rempe, Joy L.

    2001-01-01

    A mechanistic model, based on a quasi-equilibrium analysis of oxidation reactions, is proposed for predicting high-temperature corium oxidation. The analysis suggests that oxide forming on the surface of corium containing uranium, zirconium, and iron is similar to the oxides formed on zirconium and uranium as long as there is a small percentage of unoxidized zirconium or uranium in the metallic phase. This is because of the higher affinity of zirconium and uranium for oxygen. Hence, oxidation rates and heat production rates are similar to (U,Zr) compounds until nearly all the uranium and zirconium in the corium oxidizes. Oxidation rates after this point are predicted to be similar to those implied by the oxide thickness present when the forming oxide ceases to be protective, and heat generation rates should be similar to those implied by iron oxidation, i.e., ∼4% of the zirconium oxidation heating rate.The maximum atomic ratio of unoxidized iron to unoxidized liquid zirconium plus uranium for the formation of a solid protective oxide below 2800 K is estimated for a temperature, T (in Kelvin), as follows:(unoxidized iron)/(unoxidized zirconium + turanium) = (1/28){5.7/exp[-(147 061 + 12.08T log(T) - 61.03T - 0.000555T 2 /1.986T)]} 1/2 .As long as this limit is not exceeded, either zirconium or uranium metal oxidation rates and heating describe the corium oxidation rate. If this limit is exceeded, diffusion of steam to the corium surface will limit the oxidation rate, and linear time-dependent growth of a nonprotective, mostly FeO, layer will occur below the protective (Zr,U) O 2 scale. When this happens, the oxidation should be at the constant rate given by the thickness of the protective layer. Heat generation should be similar to that of iron oxidation

  9. Corium Oxidation at Temperatures Above 2000 K

    Energy Technology Data Exchange (ETDEWEB)

    Hagrman, Donald Lee; Rempe, Joy Lynn

    2001-02-01

    A mechanistic model, based on a quasi-equilibrium analysis of oxidation reactions, is proposed for predicting high-temperature corium oxidation. The analysis suggests that oxide forming on the surface of corium containing uranium, zirconium, and iron is similar to the oxides formed on zirconium and uranium as long as there is a small percentage of unoxidized zirconium or uranium in the metallic phase. This is because of the higher affinity of zirconium and uranium for oxygen. Hence, oxidation rates and heat production rates are similar to (U,Zr) compounds until nearly all the uranium and zirconium in the corium oxidizes. Oxidation rates after this point are predicted to be similar to those implied by the oxide thickness present when the forming oxide ceases to be protective, and heat generation rates should be similar to those implied by iron oxidation, i.e., ~4% of the zirconium oxidation heating rate. The maximum atomic ratio of unoxidized iron to unoxidized liquid zirconium plus uranium for the formation of a solid protective oxide below 2800 K is estimated for a temperature, T (in Kelvin), as follows: (unoxidized iron)/(unoxidized zirconium + turanium) = (1/28){5.7/exp[-(147 061 + 12.08T log(T) - 61.03T - 0.000555T2/1.986T)]}1/2. As long as this limit is not exceeded, either zirconium or uranium metal oxidation rates and heating describe the corium oxidation rate. If this limit is exceeded, diffusion of steam to the corium surface will limit the oxidation rate, and linear time-dependent growth of a nonprotective, mostly FeO, layer will occur below the protective (Zr,U) O2 scale. When this happens, the oxidation should be at the constant rate given by the thickness of the protective layer. Heat generation should be similar to that of iron oxidation.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1997-02-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1977-01-01

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

  12. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-07-01

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

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

    Science.gov (United States)

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

    2016-10-01

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

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

    Science.gov (United States)

    Vanlommel, Jan; De Corte, Ronny; Luyckx, Jean Philippe; Anderson, Melissa; Labey, Luc; Bellemans, Johan

    2017-01-01

    Oxidized zirconium (OxZr) is produced by thermally driven oxidization creating an oxidized surface with the properties of a ceramic at the top of the Zr metal substrate. OxZr is much harder and has a lower coefficient of friction than cobalt-chrome (CoCr), both leading to better wear characteristics. We evaluated and compared damage to the cartilage of porcine patella plugs, articulating against OxZr vs CoCr. Our hypothesis was that, owing to its better wear properties, OxZr would damage cartilage less than CoCr. If this is true, OxZr might be a better material for the femoral component during total knee arthroplasty if the patella is not resurfaced. Twenty-one plugs from porcine patellae were prepared and tested in a reciprocating pin-on-disk machine while lubricated with bovine serum and under a constant load. Three different configurations were tested: cartilage-cartilage as the control group, cartilage-OxZr, and cartilage-CoCr. Macroscopic appearance, cartilage thickness, and the modified Mankin score were evaluated after 400,000 wear cycles. The control group showed statistically significant less damage than plugs articulating against both other materials. Cartilage plugs articulating against OxZr were statistically significantly less damaged than those articulating against CoCr. Although replacing cartilage by an implant always leads to deterioration of the cartilage counterface, OxZr results in less damage than CoCr. The use of OxZr might thus be preferable to CoCr in case of total knee arthroplasty without patella resurfacing. Copyright © 2016 Elsevier Inc. All rights reserved.

  16. 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

  17. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2014-04-01

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

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

    Science.gov (United States)

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

    2016-01-01

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

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

    Directory of Open Access Journals (Sweden)

    Raphael Pilo

    2016-03-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-05-30

    A composite adsorbent capable of simultaneous removal of both cationic and anionic contaminants from aqueous solutions was developed by impregnating hydrous zirconium oxide (HZO) into chitosan beads (CB). The optimal mass ratio of chitosan to HZO was 2:2. The composite adsorbent (HZOCB) had the rugged surface (52.74 m{sup 2} g{sup −1}) with irregular cracks caused by HZO inclusion and amine functional groups. The rate of Pb{sup 2+} adsorption by HZOCB was relatively rapid. Most of Pb{sup 2+} (89%) was adsorbed within 2.5 h. A binary sorbate system was noticeably favorable for F{sup −} adsorption as compared to single sorbate system. Adsorption of F{sup −} and Pb{sup 2+} followed pseudo-second order kinetics. The maximum sorption capacities obtained from Langmuir isotherm model were 22.1 and 222.2 mg g{sup −1}, respectively. The study demonstrates that the developed composite could be a potential adsorbent for the simultaneous remediation of F{sup −} and Pb{sup 2+} contamination in water.

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

    International Nuclear Information System (INIS)

    Di Patrizio, Nicolas

    2015-01-01

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

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

    Science.gov (United States)

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

    2017-09-01

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

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

    Science.gov (United States)

    Krajczewski, Jan; Abdulrahman, Heman Burhanalden; Kołątaj, Karol; Kudelski, Andrzej

    2018-03-01

    One tool that can be used for determining the structure and composition of surfaces of various materials (even in in situ conditions) is shell-isolated nanoparticle-enhanced Raman spectroscopy (SHINERS). In SHINERS measurements, the surface under investigation is covered with a layer of surface-protected plasmonic nanoparticles, and then the Raman spectrum of the surface analysed is recorded. The plasmonic cores of the used core-shell structures act as electromagnetic nanoresonators, significantly locally enhancing the intensity of the electric field of the incident radiation, leading to a large increase in the efficiency of the generation of the Raman signal from molecules in the close proximity to the deposited SHINERS nanoresonators. A protective layer (from transparent dielectrics such as SiO2, Al2O3 or TiO2) prevents direct interaction between the plasmonic metal and the analysed surface (such interactions may lead to changes in the structure of the surface) and, in the case of plasmonic cores other than gold cores, the dielectric layer increases the chemical stability of the metal core. In this contribution, we show for the first time that core-shell nanoparticles having a silver core (both a solid and hollow one) and a shell of zirconium(IV) oxide are very efficient SHINERS nanoresonators that are significantly more stable in acidic and alkaline media than the silver-silica core-shell structures typically used for SHINERS experiments.

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

    KAUST Repository

    Kelly, Michael J.

    2017-06-12

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

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

    KAUST Repository

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

    2017-01-01

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

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

    Directory of Open Access Journals (Sweden)

    D.Nirmal

    2014-07-01

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

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

    International Nuclear Information System (INIS)

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

    1986-01-01

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

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

    International Nuclear Information System (INIS)

    Costa, I.; Ramanathan, L.V.

    1986-01-01

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

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

    International Nuclear Information System (INIS)

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

    1977-11-01

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

  11. 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

  12. A Glass-Ceramic Waste Forms for the Immobilization of Rare Earth Oxides from the Pyroprocessing Waste salt

    International Nuclear Information System (INIS)

    Ahn, Byung-Gil; Park, Hwan-Seo; Kim, Hwan-Young; Kim, In-Tae

    2008-01-01

    The fission product of rare earth (RE) oxide wastes are generates during the pyroprocess . Borosilicate glass or some ceramic materials such as monazite, apatite or sodium zirconium phosphate (NZP) have been a prospective host matrix through lots of experimental results. Silicate glasses have long been the preferred waste form for the immobilization of HLW. In immobilization of the RE oxides, the developed process on an industrial scale involves their incorporation into a glass matrix, by melting under 1200 ∼ 1300 .deg. C. Instead of the melting process, glass powder sintering is lower temperature (∼ 900 .deg. C) required for the process which implies less demanding conditions for the equipment and a less evaporation of volatile radionuclides. This study reports the behaviors, direct vitrification of RE oxides with glass frit, glass powder sintering of REceramic with glass frit, formation of RE-apatite (or REmonazite) ceramic according to reaction temperature, and the leach resistance of the solidified waste forms

  13. 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

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

    International Nuclear Information System (INIS)

    Actis-Dato, L.O.

    2000-02-01

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

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

    Czech Academy of Sciences Publication Activity Database

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

    2010-01-01

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

  16. 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}.

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

    International Nuclear Information System (INIS)

    Debeusscher, S.

    2008-12-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-15

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

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

    Science.gov (United States)

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

    2016-06-07

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

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

    International Nuclear Information System (INIS)

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

    1984-01-01

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

  1. 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.

  2. 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.

  3. Method of forming buried oxide layers in silicon

    Science.gov (United States)

    Sadana, Devendra Kumar; Holland, Orin Wayne

    2000-01-01

    A process for forming Silicon-On-Insulator is described incorporating the steps of ion implantation of oxygen into a silicon substrate at elevated temperature, ion implanting oxygen at a temperature below 200.degree. C. at a lower dose to form an amorphous silicon layer, and annealing steps to form a mixture of defective single crystal silicon and polycrystalline silicon or polycrystalline silicon alone and then silicon oxide from the amorphous silicon layer to form a continuous silicon oxide layer below the surface of the silicon substrate to provide an isolated superficial layer of silicon. The invention overcomes the problem of buried isolated islands of silicon oxide forming a discontinuous buried oxide layer.

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

    Directory of Open Access Journals (Sweden)

    S. Riedel

    2016-09-01

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

  5. 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.

  6. Adsorptive binding of methanol and ethanol on the oxides of silicon, titanium, zirconium, and thorium

    Energy Technology Data Exchange (ETDEWEB)

    Huettig, G F; Pietzka, G

    1948-01-01

    The authors plot adsorption isotherms for methyl alcohol, ethyl alcohol, and CCl/sub 4/ on SiO/sub 2/, TeO/sub 2/, ZrO/sub 2/, and ThO/sub 2/. The results seem to show that for a given adsorbent the volume of gas required to form a monolayer is independent of the absorbent temperature and that a greater volume of methyl alcohol than of ethyl alcohol is required to form a monolayer. The ratio of the specific rate of absorption to the specific rate of desorption is larger for ethyl alcohol than for methyl alcohol. The value of this ratio decreases with increase in temperature for a given adsorbate and a given adsorbent.

  7. Effect of zirconium purity on the glass-forming-ability and notch toughness of Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Andersen, Laura M. [Department of NanoEngineering, University of California, San Diego, 9500 Gilman Drive, La Jolla, CA (United States); Hofmann, Douglas C. [Materials Development and Manufacturing Technology Group, NASA Jet Propulsion Laboratory/California Institute of Technology, MS 18-105, 4800 Oak Grove Dr. Pasadena, CA 91109 (United States); Vecchio, Kenneth S., E-mail: kvecchio@ucsd.edu [Department of NanoEngineering, University of California, San Diego, 9500 Gilman Drive, La Jolla, CA (United States)

    2016-09-30

    The effect of substituting standard grade zirconium lump (99.8% excluding up to 4% hafnium) for high purity zirconium crystal bar (99.5%) in a Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7} bulk metallic glass (BMG) is examined. The final hafnium content in the BMG specimens was found to range from 0 to 0.44 at%. Introducing low purity zirconium significantly decreased the glass-forming-ability and reduced the notch toughness of the BMG. In contrast, when adding high purity hafnium to Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7} made with high purity zirconium, no significant change in the glass-forming-ability or toughness was observed. This suggests that the introduction of low purity zirconium in BMGs creates a more complex response than a simple addition of hafnium. It is likely that other impurities in the material, such as oxygen, play a role in the complex crystallization kinetics and change in mechanical properties. The notch toughness was measured through four-point-bend tests, which showed a decrease in notch toughness from an average of ~53 MPa m{sup 1/2} for the high purity samples to an average of ~29 MPa m{sup 1/2} with full substitution of low purity zirconium. A similar decrease in glass-forming-ability and toughness is observed in commercially synthesized high purity Cu{sub 43}Zr{sub 43}Al{sub 7}Be{sub 7}. The large scale commercial process is expected to introduced some unintentional impurities, which decrease the properties of the BMG in the same way as the lower purity elements. Lastly, Weibull statistics are used to provide an analysis of variability in toughness for both ingots synthesized in a small laboratory arc-melter and those synthesized commercially.

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

    Science.gov (United States)

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

    2011-11-01

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

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

    Science.gov (United States)

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

    2014-09-01

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

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  11. Characterization of oxidation products on a ZrFe2-type laves intermetallic exposed to 200degreeC steam

    International Nuclear Information System (INIS)

    Abraham, D. P.; Dietz, N.; Finnegan, N.

    2000-01-01

    The release of radioactive elements from the stainless steel-15 wt% zirconium (SS-15Zr) metal waste form will be governed by the corrosion behavior of ZrFe 2 -type intermetallics phases present in the alloy. In this article, oxidation products that formed on a ZrFe 2 -type intermetallic sample exposed to 200 C steam were characterized by Auger Electron Spectroscopy (AES) and Transmission Electron Microscopy (TEM). The data revealed two oxide layers on the sample surface: an outer crystalline iron-oxide layer and an inner amorphous zirconium-rich layer believed to be zirconium oxide. Thermodynamic considerations indicate that the zirconium-rich layer formed first. The iron-oxide layer appears to have resulted from the diffusion of iron through the zirconium-rich layer to the oxide-vapor interface

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

    Science.gov (United States)

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

    2015-10-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  14. Comparative study on nano-Zirconium Oxide Materials used in Nuclear Technology

    International Nuclear Information System (INIS)

    Khalil, T.; Dakroury, G.A.; Abou El-Nour, F.; Abdel-Khlik, M.

    2004-01-01

    Nano-ZrO 2 powders were prepared using two advanced methods, namely SoI-GeI and Gelation techniques. Y 2 O 3 , Ce0 2 and Mg0 were used as stabilizers during the preparation processes. The function of these materials is to stabilize the meta stable tetragonal Zr0 2 phase responsible for the nano character of produced materials. The applied experimental procedures proved to be suitable to produce nano powders composed of crystallites of few nano-meter size with an interfacial component formed by all atoms situated in the grain boundaries. These two structure components (nano-sized crystallites and boundaries) of comparable volume fractions are crucial for the nano-structure materials. Powder agglo-meration, contamination during processing and remaining of the residual pores in the bodies were overcome during the sintering process of the powder by special treatment. Different analytical procedures such as DTA-TG, specific surface area, pore size analysis, density, scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were carried out for Zr0 2 produced by both SoI-GeI and Gelation techniques

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

    Energy Technology Data Exchange (ETDEWEB)

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

    1966-02-15

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

  16. 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.

  17. Microscopic characterization of pretransition oxide formed on Zr–Nb–Sn alloy under various Zn and dissolved hydrogen concentrations

    Directory of Open Access Journals (Sweden)

    Sungyu Kim

    2018-04-01

    Full Text Available Microstructure of oxide formed on Zr–Nb–Sn tube sample was intensively examined by scanning transmission electron microscopy after exposure to simulated primary water chemistry conditions of various concentrations of Zn (0 or 30 ppb and dissolved hydrogen (H2 (30 or 50 cc/kg for various durations without applying desirable heat flux. Microstructural analysis indicated that there was no noticeable change in the microstructure of the oxide corresponding to water chemistry changes within the test duration of 100 days (pretransition stage and no significant difference in the overall thickness of the oxide layer. Equiaxed grains with nano-size pores along the grain boundaries and microcracks were dominant near the water/oxide interface, regardless of water chemistry conditions. As the metal/oxide interface was approached, the number of pores tended to decrease. However, there was no significant effect of H2 concentration between 30 cc/kg and 50 cc/kg on the corrosion of the oxide after free immersion in water at 360°C. The adsorption of Zn on the cladding surface was observed by X-ray photoelectron spectroscopy and detected as ZnO on the outer oxide surface. From the perspective of OH− ion diffusion and porosity formation, the absence of noticeable effects was discussed further. Keywords: Dissolved Hydrogen Effect, Porosity, Pretransition Oxide, Transmission Electron Microscopy (TEM, Zirconium Alloys

  18. Methods for forming complex oxidation reaction products including superconducting articles

    International Nuclear Information System (INIS)

    Rapp, R.A.; Urquhart, A.W.; Nagelberg, A.S.; Newkirk, M.S.

    1992-01-01

    This patent describes a method for producing a superconducting complex oxidation reaction product of two or more metals in an oxidized state. It comprises positioning at least one parent metal source comprising one of the metals adjacent to a permeable mass comprising at least one metal-containing compound capable of reaction to form the complex oxidation reaction product in step below, the metal component of the at least one metal-containing compound comprising at least a second of the two or more metals, and orienting the parent metal source and the permeable mass relative to each other so that formation of the complex oxidation reaction product will occur in a direction towards and into the permeable mass; and heating the parent metal source in the presence of an oxidant to a temperature region above its melting point to form a body of molten parent metal to permit infiltration and reaction of the molten parent metal into the permeable mass and with the oxidant and the at least one metal-containing compound to form the complex oxidation reaction product, and progressively drawing the molten parent metal source through the complex oxidation reaction product towards the oxidant and towards and into the adjacent permeable mass so that fresh complex oxidation reaction product continues to form within the permeable mass; and recovering the resulting complex oxidation reaction product

  19. 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.

  20. Strengthening and elongation mechanism of Lanthanum-doped Titanium-Zirconium-Molybdenum alloy

    Energy Technology Data Exchange (ETDEWEB)

    Hu, Ping, E-mail: huping1985@126.com [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Jinduicheng Molybdenum Co., Ltd., Xi’an 710068 (China); Hu, Bo-liang; Wang, Kuai-she; Song, Rui; Yang, Fan [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Yu, Zhi-tao [Ruifulai Tungsten & Molybdenum Co., Ltd., Xi’an 721914 (China); Tan, Jiang-fei [School of Metallurgy Engineering, Xi’an University of Architecture and Technology, Xi’an 710055 (China); Cao, Wei-cheng; Liu, Dong-xin; An, Geng [Jinduicheng Molybdenum Co., Ltd., Xi’an 710068 (China); Guo, Lei [Ruifulai Tungsten & Molybdenum Co., Ltd., Xi’an 721914 (China); Yu, Hai-liang [School of Mechanical, Materials and Mechatronics Engineering, University of Wollongong, NSW 2522 (Australia)

    2016-12-15

    The microstructural contributes to understand the strengthening and elongation mechanism in Lanthanum-doped Titanium-Zirconium-Molybdenum alloy. Lanthanum oxide particles not only act as heterogeneous nucleation core, but also act as the second phase to hinder the grain growth during sintering crystallization. The molybdenum substrate formed sub-grain under the effect of second phase when the alloy rolled to plate.

  1. 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

  2. Influence de l’irradiation et de la radiolyse sur la vitesse et les mécanismes de corrosion des alliages de zirconium

    OpenAIRE

    Verlet , Romain

    2015-01-01

    The nuclear fuel of pressurized water reactors (PWR) in the form of uranium oxide UO2 pellets (or MOX) is confined in a zirconium alloy cladding. This cladding is very important because it represents the first containment barrier against the release of fission products generated by the nuclear reaction to the external environment. Corrosion by the primary medium of zirconium alloys, particularly the Zircaloy-4, is one of the factors limiting the reactor residence time of the fuel rods (UO2 pe...

  3. Synthesis and Properties of Metallic Technetium and Technetium-Zirconium Alloys as Transmutation Target and Radioactive waste storage form in the UREX+1 Process

    Energy Technology Data Exchange (ETDEWEB)

    Hartmann, Thomas [Idaho State University/Idaho National Laboratory, 1776 Science Center Drive, Idaho Falls, ID 83402 (United States)]|[Harry Reid Center, University Nevada - Las Vegas, 4505 Maryland Parkway, Las Vegas, NV (United States); Poineau, Frederic; Czerwinski, Kenneth R. [Harry Reid Center, University Nevada - Las Vegas, 4505 Maryland Parkway, Las Vegas, NV (United States)

    2008-07-01

    In the application of UREX+1 process, technetium will be separated together with uranium and iodine within the first process step. After the separation of uranium, technetium and iodine must be immobilized by their incorporation in a suitable waste storage-form. Based on recent activities within the AFCI community, a potential candidate as waste storage form to immobilize technetium is to alloy the metal with excess zirconium. Alloys in the binary Tc-Zr system may act as potential transmutation targets in order to transmute Tc-99 into Ru-100. We are presenting first results in the synthesis of metallic technetium, and the synthesis of equilibrium phases in the binary Tc-Zr system at 1400 deg. C after arc-melting and isothermal annealing under inert conditions. Samples were analyzed using X-ray powder diffraction, Rietveld analysis, scanning electron microscopy, and electron probe micro-analysis, which allows us to construct the binary Tc-Zr phase diagram for the isothermal section at 1400 deg. C. (authors)

  4. 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

  5. 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.

  6. 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

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

    Science.gov (United States)

    Zhao, Hongting; Moore, Robert C.

    2004-11-30

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-07-01

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

  9. Electronic properties of thermally formed thin iron oxide films

    International Nuclear Information System (INIS)

    Wielant, J.; Goossens, V.; Hausbrand, R.; Terryn, H.

    2007-01-01

    The oxide layer, present between an organic coating and the substrate, guarantees adhesion of the coating and plays a determinating role in the delamination rate of the organic coating. The purpose of this study is to compare the resistive and semiconducting properties of thermal oxides formed on steel in two different atmospheres at 250 deg. C: an oxygen rich atmosphere, air, and an oxygen deficient atmosphere, N 2 . In N 2 , a magnetite layer grows while in air a duplex oxide film forms composed by an inner magnetite layer and a thin outer hematite scale. The heat treatment for different amounts of time at high temperature was used as method to sample the thickness variation and change in electronic and semiconducting properties of the thermal oxide layers. Firstly, linear voltammetric measurements were performed to have a first insight in the electrochemical behavior of the thermal oxides in a borate buffer solution. Electrochemical impedance spectroscopy in the same buffer combined with the Mott-Schottky analysis were used to determine the semiconducting properties of the thermal oxides. By spectroscopic ellipsometry (SE) and atomic force microscopy (AFM), respectively, the thickness and roughness of the oxide layers were determined supporting the physical interpretation of the voltammetric and EIS data. These measurements clearly showed that oxide layers with different constitution, oxide resistance, flatband potential and doping concentration can be grown by changing the atmosphere

  10. Uranium oxidation: Characterization of oxides formed by reaction with water by infrared and sorption analyses

    Science.gov (United States)

    Fuller, E. L.; Smyrl, N. R.; Condon, J. B.; Eager, M. H.

    1984-04-01

    Three different uranium oxide samples have been characterized with respect to the different preparation techniques. The results show that the water reaction with uranium metal occurs cyclically forming laminar layers of oxide which spall off due to the strain at the oxide/metal interface. Single laminae are released if liquid water is present due to the prizing penetration at the reaction zone. The rate of reaction of water with uranium is directly proportional to the amount of adsorbed water on the oxide product. Rapid transport is effected through the open hydrous oxide product. Dehydration of the hydrous oxide irreversibly forms a more inert oxide which cannot be rehydrated to the degree that prevails in the original hydrous product of uranium oxidation with water. Inert gas sorption analyses and diffuse reflectance infrared studies combined with electron microscopy prove valuable in defining the chemistry and morphology of the oxidic products and hydrated intermediates.

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

    Science.gov (United States)

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

    2014-02-01

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

  12. 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

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

    Science.gov (United States)

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

    2013-01-14

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

  14. MICROSTRUCTURE, THERMO-PHYSICAL, MECHANICAL AND WEAR PROPERTIES OF IN-SITU FORMED BORON CARBIDE - ZIRCONIUM DIBORIDE COMPOSITE

    Directory of Open Access Journals (Sweden)

    T. S. R. Ch. Murthy

    2017-12-01

    Full Text Available Microstructure, thermos-physical, mechanical and wear properties of in-situ formed B₄C- ZrB₂ composite were investigated. Coefficient of thermal expansion, thermal diffusivity and electrical resistivity of the composite were measured at different temperatures up to 1000 °C in inert atmosphere. Flexural strength was measured up to 900 °C in air. Friction and wear properties have been studied at different loads under reciprocative sliding, using a counter body (ball of cemented tungsten carbide (WC-Co at ambient conditions. X-ray diffraction (XRD and electron probe microanalysis (EPMA confirmed the formation of ZrB₂ as the reaction product in the composite. Electrical resistivity was measured as 3.02 x 10-4Ω.m at 1000°C. Thermal conductivity measured at temperatures between 25°C and 1000 °C was in the range of 8 to 10 W/m-K. Flexural strength of the composite decreased with increase in temperature and reached a value of 92 MPa at 900°C. The average value of coefficient of friction (COF was measured as 0.15 at 20 N load and 10 Hz frequency. Increase of load from 5 N to 20 N resulted in decrease in COF from 0.24 to 0.15 at 10 Hz frequency. Specific wear rate data observed was of the order of 10-6 mm³/N-m. Both abrasive and tribo-chemical reaction wear mechanisms were observed on the worn surface of flat and counter body materials. At higher loads (≥10 N a tribo-chemical reaction wear mechanism was dominant.

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

    Science.gov (United States)

    Felemban, Nayef H; Ebrahim, Mohamed I

    2017-01-13

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

  16. Estimation of the nitric oxide formed from hydroxylamine by Nitrosomonas

    Science.gov (United States)

    Anderson, J. H.

    1965-01-01

    1. Nitric oxide that was produced by reducing nitrite with an excess of acidified potassium iodide under nitrogen in Warburg respirometer flasks was rapidly absorbed by a solution of permanganate in sodium hydroxide held in the side arm. A small amount of nitrous oxide (or nitrogen) that was also produced was not absorbed. 2. By using a quantitative method for the recovery of nitrite from samples of the alkaline permanganate, it was found that the sum of the nitrite N formed and the residual nitrous oxide N was equivalent to the nitrite N used to generate the gases. These results showed that alkaline permanganate completely oxidized nitric oxide to nitrite. The method was suitable for determining 0·4–20 μmoles of nitric oxide. 3. The technique was used to determine the nitric oxide content of the nitrogenous gas that was produced anaerobically from hydroxylamine by an extract of the autotrophic nitrifying micro-organism Nitrosomonas in the presence of methylene blue as electron acceptor. PMID:14342235

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

    International Nuclear Information System (INIS)

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

    2006-03-01

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

  18. 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.

  19. Cationic polyelectrolyte induced separation of some inorganic contaminants and their mixture (zirconium silicate, kaolin, K-feldspar, zinc oxide) as well as of the paraffin oil from water.

    Science.gov (United States)

    Ghimici, Luminita

    2016-03-15

    The flocculation efficiency of a cationic polyelectrolyte with quaternary ammonium salt groups in the backbone, namely PCA5 was evaluated on zirconium silicate (kreutzonit), kaolin, K- feldspar and zinc oxide (ZnO) suspensions prepared either with each pollutant or with their mixture. The effect of several parameters such as settling time, polymer dose and the pollutant type on the separation efficacy was evaluated and followed by optical density and zeta potential measurements. Except for ZnO, the interactions between PCA5 and suspended particles led to low residual turbidity values (around 4% for kreutzonit, 5% for kaolin and 8% for K-feldspar) as well as to the reduction of flocs settling time (from 1200 min to 30 min and 120 min in case of kaolinit and K-feldspar, respectively), that meant a high efficiency in their separation. The negative value of the zeta potential and flocs size measurements, at the optimum polymer dose, point to contribution from charge patch mechanism for the particles flocculation. A good efficiency of PCA5 in separation of paraffin oil (a minimum residual turbidity of 9.8%) has been also found. Copyright © 2015 Elsevier Ltd. All rights reserved.

  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. 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.

  2. 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.

  3. Atomistic studies of cation transport in tetragonal ZrO2 during zirconium corrosion

    International Nuclear Information System (INIS)

    Bai, Xian-Ming; Zhang, Yongfeng; Tonks, Michael R.

    2015-01-01

    Zirconium alloys are the major fuel cladding materials in current reactors. The water-side corrosion is a significant degradation mechanism of these alloys. During corrosion, the transport of oxidizing species in zirconium dioxide (ZrO 2 ) determines the corrosion kinetics. Previously, it has been argued that the outward diffusion of cations is important for forming protective oxides. In this work, the migration of Zr defects in tetragonal ZrO 2 is studied with temperature accelerated dynamics and molecular dynamics simulations. The results show that Zr interstitials have anisotropic diffusion and migrate preferentially along the [001] or c direction in tetragonal ZrO 2 . The compressive stresses can increase the Zr interstitial migration barrier significantly. The migration of Zr interstitials at a grain boundary is much slower than in a bulk oxide. The implications of these atomistic simulation results in the Zr corrosion are discussed. (authors)

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

    Science.gov (United States)

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

    2017-06-27

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

  5. 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

  6. Effect of additive on electrochemical corrosion properties of plasma electrolytic oxidation coatings formed on CP Ti under different processing frequency

    Energy Technology Data Exchange (ETDEWEB)

    Babaei, Mahdi, E-mail: mahdi.babaei@ut.ac.ir; Dehghanian, Changiz; Vanaki, Mojtaba

    2015-12-01

    Highlights: • PEO coatings formed on Cp Ti from phosphate electrolyte with zirconate additive. • The SEM results provide information of microdischarge behavior. • The effect of additive on structure and long-term corrosion behavior was investigated. • The additive influence on coating performance varies with processing frequency. - Abstract: The plasma electrolytic oxidation (PEO) coating containing zirconium oxide was fabricated on CP Ti at different processing frequencies viz., 100 Hz and 1000 Hz in a (Na{sub 2}ZrO{sub 3}, Na{sub 2}SiO{sub 3})-additive containing NaH{sub 2}PO{sub 4}-based solution, and long-term electrochemical corrosion behavior of the coatings was studied using electrochemical impedance spectroscopy (EIS) in 3.5 wt.% NaCl solution. Electrochemical degradation behavior of two-layered coatings formed at different frequencies was turned out to be governed by concentration of electrolyte additive. With increasing additive concentration, the coating obtained at frequency of 1000 Hz exhibited enhanced corrosion resistance. However, corrosion resistance of the coating prepared at 100 Hz was found to decrease with increased additive, which was attributed to intensified microdischarges damaging the protective effect of inner layer. Nevertheless, the electrolyte additive was found to mitigate the long-term degradation of the coatings to a significant extent.

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

    Energy Technology Data Exchange (ETDEWEB)

    Sridharan, Kumar [University of Wisconsin-Madison; Mariani, Robert [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bai, Xianming [Idaho National Lab. (INL), Idaho Falls, ID (United States); Xu, Peng [Westinghouse Electric Company; Lahoda, Ed [Westinghouse Electric Company

    2018-03-31

    Given the long-term goal of developing such coatings for use with nuclear reactor fuel cladding, this work describes results of oxidation and corrosion behavior of bulk zirconium-silicide and fabrication of zirconium-silicide coatings on zirconium-alloy test flats, tube configurations, and SiC test flats. In addition, boiling heat transfer of these modified surfaces (including ZrSi2 coating) during clad quenching experiments is discussed in detail. Oxidation of bulk ZrSi2 was found to be negligible compared to Zircaloy-4 (a common Zr-alloy cladding material) and mechanical integrity of ZrSi2 was superior to that of bulk Zr2Si at high temperatures in ambient air. Very interesting and unique multi-nanolayered composite of ZrO2 and SiO2 were observed. Physical model for the oxidation has been proposed wherein Zr–Si–O mixture undergoes a spinodal phase decomposition into ZrO2 and SiO2, which is manifested as a nanoscale assembly of alternating layer of the two oxides. Steam corrosion at high pressure (10.3 MPa) led to weight loss of ZrSi2 and produced oxide scale with depletion of silicon, possibly attributed to volatile silicon hydroxide, gaseous silicon monoxide, and a solubility of silicon dioxide in water. Only Zircon phase (ZrSiO4) formed during oxidation of ZrSi2 at 1400°C in air, and allowed for immobilization silicon species in oxide scale in the aqueous environments. Zirconium-silicide coatings (on zirconium-alloy substrates) investigated in this study were deposited primarily using magnetron sputter deposition method and slurry method, although powder spray deposition processes cold spray and thermal spray methods were also investigated. The optimized ZrSi2 sputtered coating exhibited a highly protective nature at elevated temperatures in ambient air by mitigating oxygen permeation to the underlying zirconium alloy substrate. The high oxidation resistance of the coating has been shown to be due to nanocrystalline SiO2 and ZrSiO4 phases in the amorphous

  8. 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)

  9. 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.)

  10. MULTILAYER COMPOSITE PLASMA COATINGS ON SCREEN PROTECTION ELEMENTS BASED ON ZIRCONIUM DIOXIDE

    Directory of Open Access Journals (Sweden)

    V. A. Okovity

    2017-01-01

    Full Text Available The paper contains results of investigations pertaining to an influence of plasma jet parameters (current, spraying distance, consumption of plasma formation gas (nitrogen, fractional composition of initial powder and degree of cooling with compressed air on anti-meteoric coating characteristics. Optimum modes (arc current 600 A; spray distance of 110 mm; consumption of plasma formation gas (nitrogen – 50 l/min; fractional composition of zirconium dioxide powder <50 μm; compressed air consumption for cooling – 1 m3/min; p = 4 bar make it possible to obtain anti-meteoric coatings based on zirconium dioxide with material utilization rate of 62 %, total ceramic layer porosity of 6 %. After exposure of compression plasma flows on a coating in the nitrogen atmosphere a cubic modification of zirconium oxide is considered as the main phase being present in the coating. The lattice parameter of cubic zirconium oxide modification is equal to 0.5174 nm. Taking into consideration usage of nitrogen as plasma formation substance its interaction with zirconium coating atoms occurs and zirconium nitride (ZrN is formed with a cubic crystal lattice (lattice parameter 0.4580 nm. Melting of pre-surface layer takes place and a depth of the melted layer is about 8 μm according to the results of a scanning electron microscopy. Pre-surface layer being crystallized after exposure to compression plasma flows is characterized by a homogeneous distribution of ele-ments and absence of pores formed in the process of coating formation. The coating structure is represented by a set of lar- ge (5–7 μm and small (1–2 μm zirconium oxide particles sintered against each other. Melting of coating surface layer and speed crystallization occur after the impact of compression plasma flows on the formed coating. Cracking of the surface layer arises due to origination of internal mechanical stresses in the crystallized part. While using a scanning electron microscopy a

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

    International Nuclear Information System (INIS)

    Gala, A.; Schendler, W.

    1981-01-01

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

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  13. Microhardness of anodic aluminum oxide formed in an alkaline electrolyte

    Science.gov (United States)

    Kanygina, O. N.; Filyak, M. M.

    2017-04-01

    The microhardness of anodic aluminum oxide formed by anodizing of aluminum sheet in electrolyte on the basis of sodium hydroxide has been determined experimentally. The microhardness of the hard film/soft substrate system has been estimated by three approaches: indentation geometry (length of diagonals) in film surfaces, the sum of the hardnesses of the film and the surface with allowance for the indentation surface area and geometry, and with allowance for the indentation depth. It is demonstrated that the approach accounting for the indentation depth makes it possible to eliminate the influence of the substrate. It is established that the microhardness of the films formed in alkaline electrolytes is comparable with that formed in acid electrolytes.

  14. Method for forming H2-permselective oxide membranes

    Science.gov (United States)

    Gavalas, G.R.; Nam, S.W.; Tsapatsis, M.; Kim, S.

    1995-09-26

    Methods are disclosed for forming permselective oxide membranes that are highly selective to permeation of hydrogen by chemical deposition of reactants in the pore of porous tubes, such as Vycor{trademark} glass or Al{sub 2}O{sub 3} tubes. The porous tubes have pores extending through the tube wall. The process involves forming a stream containing a first reactant of the formula RX{sub n}, wherein R is silicon, titanium, boron or aluminum, X is chlorine, bromine or iodine, and n is a number which is equal to the valence of R; and forming another stream containing water vapor as the second reactant. Both of the reactant streams are passed along either the outside or the inside surface of a porous tube and the streams react in the pores of the porous tube to form a nonporous layer of R-oxide in the pores. The membranes are formed by the hydrolysis of the respective halides. In another embodiment, the first reactant stream contains a first reactant having the formula SiH{sub n}Cl{sub 4{minus}n} where n is 1, 2 or 3; and the second reactant stream contains water vapor and oxygen. In still another embodiment the first reactant stream containing a first reactant selected from the group consisting of Cl{sub 3}SiOSiCl{sub 3}, Cl{sub 3}SiOSiCl{sub 2}OSiCl{sub 3}, and mixtures thereof and the second reactant stream contains water vapor. In still another embodiment, membrane formation is carried out by an alternating flow deposition method. This involves a sequence of cycles, each cycle comprising introduction of the halide-containing stream and allowance of a specific time for reaction followed by purge and flow of the water vapor containing stream for a specific length of time. In all embodiments the nonporous layers formed are selectively permeable to hydrogen. 11 figs.

  15. Separation of zirconium--hafnium by nitride precipitation

    International Nuclear Information System (INIS)

    Anderson, R.N.; Parlee, N.A.

    1977-01-01

    A method is described for the separation of a light reactive metal (e.g., zirconium) from a heavy reactive metal (e.g., hafnium) by forming insoluble nitrides of the metals in a molten metal solvent (e.g., copper) inert to nitrogen and having a suitable density for the light metal nitride to form a separate phase in the upper portion of the solvent and for the heavy metal nitride to form a separate phase in the lower portion of the solvent. Nitriding is performed by maintaining a nitrogen-containing atmosphere over the bath. The light and heavy metals may be an oxide mixture and carbothermically reduced to metal form in the same bath used for nitriding. The nitrides are then separately removed and decomposed to form the desired separate metals. 16 claims, 1 figure

  16. 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)

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

    Science.gov (United States)

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

    2016-10-01

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

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

    Science.gov (United States)

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

    2018-06-15

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

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

    International Nuclear Information System (INIS)

    Brunet-Thibault, E.

    2006-12-01

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

  20. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2011-12-15

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

  2. 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

  3. 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

  4. 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)

  5. Oxidation of Alumina-Forming MAX Phases in Turbine Environments

    Science.gov (United States)

    Smialek, James; Garg, Anita; Harder, Bryan; Nesbitt, James; Gabb, Timothy; Gray, SImon

    2017-01-01

    Protective coatings for high temperature turbine components are based on YSZ thermal barriers and oxidation resistant, alumina-forming NiAl or NiCoCrAlY bond coats. Ti2AlC and Cr2AlC MAX phases are thus of special interest because of good oxidation resistance and CTE that can match Al2O3 and YSZ. Their alumina scales grow according to cubic kinetics due to grain growth in the scale, with initial heating dominated by fast TiO2 growth. Protective cubic kinetics are also found in high pressure burner rig tests of MAXthal 211 Ti2AlC, but with reduced rates due to volatile TiO(OH)2 formation in water vapor. YSZ-coatings on bulk Ti2AlC exhibit remarkable durability up to 1300C in furnace tests and at least a 25x life advantage compared to superalloys. At another extreme, Cr2AlC is resistant to low temperature Na2SO4 hot corrosion and exhibits thermal cycling stability bonded to a superalloy disk material. Accordingly, sputtered Cr2AlC coatings on disk specimens prevented hot corrosion detriments on LCF. Breakaway oxidation (Ti2AlC), scale spallation (Cr2AlC), interdiffusion, and processing as coatings still present serious challenges. However the basic properties of MAX phases provide some unusual opportunities for use in high temperature turbines.

  6. 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.

  7. 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

  8. 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)

  9. 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

  10. Influence of irradiation and radiolysis on the corrosion rates and mechanisms of zirconium alloys

    International Nuclear Information System (INIS)

    Verlet, Romain

    2015-01-01

    The nuclear fuel of pressurized water reactors (PWR) in the form of uranium oxide UO 2 pellets (or MOX) is confined in a zirconium alloy cladding. This cladding is very important because it represents the first containment barrier against the release of fission products generated by the nuclear reaction to the external environment. Corrosion by the primary medium of zirconium alloys, particularly the Zircaloy-4, is one of the factors limiting the reactor residence time of the fuel rods (UO 2 pellets + cladding). To optimize core management and to extend the lifetime of the fuel rods in reactor, new alloys based on zirconium-niobium (M5) have been developed. However, the corrosion mechanisms of these are not completely understood because of the complexity of these materials, corrosion environment and the presence of radiation from the nuclear fuel. Therefore, this thesis specifically addresses the effects of radiolysis and defects induced by irradiation with ions in the matrix metal and the oxide layer on the corrosion rate of Zircaloy-4 and M5. The goal is to separate the influence of radiation damage to the metal, that relating to defects created in the oxide and that linked to radiolysis of the primary medium on the oxidation rate of zirconium alloys in reactor. 1) Regarding effect of irradiation of the metal on the oxidation rate: type dislocation loops appear and increase the oxidation rate of the two alloys. For M5, in addition to the first effect, a precipitation of fines needles of niobium reduced the solid solution of niobium concentration in the metal and ultimately in the oxide, which strongly reduces the oxidation rate of the alloy. 2) Regarding the effect of irradiation of the oxide layer on the oxidation rate: defects generated by the nuclear cascades in the oxide increase the oxidation rate of the two materials. For M5, germination of niobium enriched zones in irradiated oxide also causes a decrease of the niobium concentration in solid solution

  11. Preparation of the electrochemically formed spinel-lithium manganese oxides

    Energy Technology Data Exchange (ETDEWEB)

    Katakura, Katsumi; Wada, Kohei; Kajiki, Yoshiyuki; Yamamoto, Akiko [Department of Chemical Engineering, Nara National College of Technology, 22 Yata-cho Yamotokoriyama, Nara 639-1080 (Japan); Ogumi, Zempachi [Graduate School of Engineering, Kyoto University, Nishikyo-ku, Kyoto 615-8510 (Japan)

    2009-04-01

    Electrochemically formed spinel-lithium manganese oxides were synthesized from manganese hydroxides prepared by a cathodic electrochemical precipitation from various concentrations of manganese nitrate solutions. Two types of manganese hydroxides were formed from diluted and concentrated Mn(NO{sub 3}){sub 2} aqueous solutions. Uniform and equi-sized disk shaped Mn(OH){sub 2} crystals of 0.2-5 {mu}m in diameter were obtained on a Pt substrate after the electrochemical precipitation from lower concentration of ranging from 2 mmol dm{sup -3} to 2 mol dm{sup -3} Mn(NO{sub 3}){sub 2} aq., while the grass blade-like precipitate which is ascribed to manganese hydroxide with 20-80 {mu}m long and 1-5 {mu}m wide were formed from concentrated Mn(NO{sub 3}){sub 2} aq. Both manganese hydroxides gave the electrochemically formed spinel-LiMn{sub 2}O{sub 4} onto a Pt sheet, which is ready for electrochemical measurement, after calcination of the Li incorporated precipitate at 750 C without any additives. While the shape and size of the secondary particle frameworks (aggregates) of the electrochemically formed spinel-LiMn{sub 2}O{sub 4} can be controlled by the electrolysis conditions, the nanostructured primary crystals of 200 nm in diameter were obtained in all cases except that the fiber-like nanostructured spinel-LiMn{sub 2}O{sub 4} crystals with 200 nm in diameter were obtained from concentrated Mn(NO{sub 3}){sub 2} aq. Though these two types of electrochemically formed spinel-LiMn{sub 2}O{sub 4} showed well-shaped CVs even in higher scan rates, it would be suitable for high power density battery applications. These behaviors are assumed to be ascribed to the crystal size and shape of the processed spinel-LiMn{sub 2}O{sub 4}. (author)

  12. 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.)

  13. Magnetic Iron Oxide Nanowires Formed by Reactive Dewetting.

    Science.gov (United States)

    Bennett, Roger A; Etman, Haitham A; Hicks, Hannah; Richards, Leah; Wu, Chen; Castell, Martin R; Dhesi, Sarnjeet S; Maccherozzi, Francesco

    2018-04-11

    The growth and reactive dewetting of ultrathin films of iron oxides supported on Re(0001) surfaces have been imaged in situ in real time. Initial growth forms a nonmagnetic stable FeO (wüstite like) layer in a commensurate network upon which high aspect ratio nanowires of several microns in length but less than 40 nm in width can be fabricated. The nanowires are closely aligned with the substrate crystallography and imaging by X-ray magnetic circular dichroism shows that each contain a single magnetic domain. The driving force for dewetting appears to be the minimization of strain energy of the Fe 3 O 4 crystallites and follows the Tersoff and Tromp model in which strain is minimized at constant height by extending in one epitaxially matched direction. Such wires are promising in spintronic applications and we predict that the growth will also occur on other hexagonal substrates.

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

    Science.gov (United States)

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

    2016-09-02

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2003-07-01

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

  16. When do oxide precipitates form during consolidation of oxide dispersion strengthened steels?

    Energy Technology Data Exchange (ETDEWEB)

    Deschamps, A., E-mail: alexis.deschamps@grenoble-inp.fr [Univ. Grenoble Alpes, SIMAP, F-38000 Grenoble (France); CNRS, SIMAP, F-38000 Grenoble (France); De Geuser, F. [Univ. Grenoble Alpes, SIMAP, F-38000 Grenoble (France); CNRS, SIMAP, F-38000 Grenoble (France); Malaplate, J.; Sornin, D. [DEN, DANS, DMN, Service de Recherches Métallurgiques Appliquées, CEA, Université Paris-Saclay, 91191 Gif-Sur-Yvette (France)

    2016-12-15

    The processing of oxide dispersion strengthened (ODS) steels involves ball milling, where the oxide forming species are driven in solid solution. Precipitation of the nanometre-scale oxides occurs during subsequent annealing and consolidation. This paper reports in-situ Small-Angle X-ray Scattering measurements of the formation of these precipitates during heating of cold-compressed as-milled powders. Clusters are already initially present, and precipitation starts at 300 °C. The maximum precipitate density is achieved at 600 °C, followed by very slow coarsening at higher temperature. These results open the way to understand the coupled evolution of precipitation and crystalline defects during heating and consolidation of ODS steels.

  17. Review of Fabrication Methods, Physical Properties, and Applications of Nanostructured Copper Oxides Formed via Electrochemical Oxidation

    Directory of Open Access Journals (Sweden)

    Wojciech J. Stepniowski

    2018-05-01

    Full Text Available Typically, anodic oxidation of metals results in the formation of hexagonally arranged nanoporous or nanotubular oxide, with a specific oxidation state of the transition metal. Recently, the majority of transition metals have been anodized; however, the formation of copper oxides by electrochemical oxidation is yet unexplored and offers numerous, unique properties and applications. Nanowires formed by copper electrochemical oxidation are crystalline and composed of cuprous (CuO or cupric oxide (Cu2O, bringing varied physical and chemical properties to the nanostructured morphology and different band gaps: 1.44 and 2.22 eV, respectively. According to its Pourbaix (potential-pH diagram, the passivity of copper occurs at ambient and alkaline pH. In order to grow oxide nanostructures on copper, alkaline electrolytes like NaOH and KOH are used. To date, no systemic study has yet been reported on the influence of the operating conditions, such as the type of electrolyte, its temperature, and applied potential, on the morphology of the grown nanostructures. However, the numerous reports gathered in this paper will provide a certain view on the matter. After passivation, the formed nanostructures can be also post-treated. Post-treatments employ calcinations or chemical reactions, including the chemical reduction of the grown oxides. Nanostructures made of CuO or Cu2O have a broad range of potential applications. On one hand, with the use of surface morphology, the wetting contact angle is tuned. On the other hand, the chemical composition (pure Cu2O and high surface area make such materials attractive for renewable energy harvesting, including water splitting. While compared to other fabrication techniques, self-organized anodization is a facile, easy to scale-up, time-efficient approach, providing high-aspect ratio one-dimensional (1D nanostructures. Despite these advantages, there are still numerous challenges that have to be faced, including the

  18. Characteristics of oxide scale formed on Cu-bearing austenitic stainless steel during early stages of high temperature oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Swaminathan, Srinivasan, E-mail: swaminathan@kist.re.kr [Metallurgy & Materials Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); High Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seongbuk-gu, Seoul 136 791 (Korea, Republic of); Krishna, Nanda Gopala [Metallurgy & Materials Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); Kim, Dong-Ik, E-mail: dongikkim@kist.re.kr [High Temperature Energy Materials Research Center, Korea Institute of Science and Technology, Seongbuk-gu, Seoul 136 791 (Korea, Republic of)

    2015-10-30

    Highlights: • Initial oxidation characteristics of Cu-bearing austenitic stainless steel at 650 °C were studied. • Strong segregation and oxidation of Mn and Nb were found in the entire oxide scale. • Surface coverage by metallic Cu-rich precipitates increases with exposure time. • Chemical heterogeneity of oxide scale revealed initial oxidation to be non-selective. • Fe-Cr and Mn-Cr mixed oxides were realized along with binary oxides of Fe, Cr and Mn. - Abstract: Oxide scale evolution on Cu-bearing austenitic stainless steel 304H at 650 °C, in ambient air, for exposure times 100, 300, 500 and 1000 h, has been investigated. Surface morphology and chemistry of the oxide scale grown were examined using SEM/EDX and XPS. The oxidation kinetics was determined by measuring the weight change using an electronic balance. At the initial stage, up to 500 h of exposure time, the oxidation rate was rapid due to surface reactions governed primarily by oxygen ingress, and then, dropped to a low rate after prolonged oxidation for 1000 h. The diffusion of reactants through the initially formed oxide scale limits the oxidation rate at longer times, thus, the progress of reaction followed the parabolic kinetics. The formed oxide scale was enriched significantly with segregation and subsequent oxidation of Nb, and finely dispersed metallic Cu particles. Within the time frame of oxidation, the oxide scale was mainly composed of mixed oxides such as FeCr{sub 2}O{sub 4} and MnCr{sub 2}O{sub 4} along with the binary oxides of Fe, Cr and Mn. Moreover, the precipitation fraction of Cu-rich particles on the oxide scale increased markedly with increase of exposure times. The chemical heterogeneity of oxide scale suggests that the oxidation occurred in a non-selective manner.

  19. 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.

  20. Method of forming oxide coatings. [for solar collector heating panels

    Science.gov (United States)

    Mcdonald, G. E. (Inventor)

    1983-01-01

    This invention is concerned with an improved plating process for covering a substrate with a black metal oxide film. The invention is particularly directed to making a heating panel for a solar collector. A compound is electrodeposited from an aqueous solution containing cobalt metal salts onto a metal substrate. This compound is converted during plating into a black, highly absorbing oxide coating which contains hydrated oxides. This is achieved by the inclusion of an oxidizing agent in the plating bath. The inclusion of an oxidizing agent in the plating bath is contrary to standard electroplating practice. The hydrated oxides are converted to oxides by treatment in a hot bath, such as boiling water. An oxidizing agent may be added to the hot liquid treating bath.

  1. 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

  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. 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

  4. Ultra-low power thin film transistors with gate oxide formed by nitric acid oxidation method

    International Nuclear Information System (INIS)

    Kobayashi, H.; Kim, W. B.; Matsumoto, T.

    2011-01-01

    We have developed a low temperature fabrication method of SiO 2 /Si structure by use of nitric acid, i.e., nitric acid oxidation of Si (NAOS) method, and applied it to thin film transistors (TFT). A silicon dioxide (SiO 2 ) layer formed by the NAOS method at room temperature possesses 1.8 nm thickness, and its leakage current density is as low as that of thermally grown SiO 2 layer with the same thickness formed at ∼900 deg C. The fabricated TFTs possess an ultra-thin NAOS SiO 2 /CVD SiO 2 stack gate dielectric structure. The ultrathin NAOS SiO 2 layer effectively blocks a gate leakage current, and thus, the thickness of the gate oxide layer can be decreased from 80 to 20 nm. The thin gate oxide layer enables to decrease the operation voltage to 2 V (cf. the conventional operation voltage of TFTs with 80 nm gate oxide: 12 V) because of the low threshold voltages, i.e., -0.5 V for P-ch TFTs and 0.5 V for N-ch TFTs, and thus the consumed power decreases to 1/36 of that of the conventional TFTs. The drain current increases rapidly with the gate voltage, and the sub-threshold voltage is ∼80 mV/dec. The low sub-threshold swing is attributable to the thin gate oxide thickness and low interface state density of the NAOS SiO 2 layer. (authors)

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

    International Nuclear Information System (INIS)

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

    2014-01-01

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

  6. 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)

  7. Environmentally Friendly Zirconium Oxide Pretreatment

    Science.gov (United States)

    2013-05-01

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

  8. 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

  9. XPS studies of the oxide formed on pure Ti

    International Nuclear Information System (INIS)

    Cremery, P.; David, D.; Beranger, G.; Oviedo, C.; Garcia, E.A.

    1980-01-01

    The XPS technique was used to study titanium samples oxidized at 200 ton of pure oxigen at different times and temperatures with the aim of producing variable oxide thicknesses. The thicknesses of different oxigen layers were determined by the nuclear reaction O 16 (d,p) O 17 *. (author) [pt

  10. Determination of the stability of the uranyl ion sipped in {tau}-hydrogen phosphate of zirconium in sodic form; Determinacion de la estabilidad del ion uranilo sorbido en {tau}-hidrogenofosfato de zirconio en forma sodica

    Energy Technology Data Exchange (ETDEWEB)

    Ordonez R, E.; Fernandez V, S.M. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico); Drot, R.; Simoni, E. [Universite de Paris-Sud-XI, Institut de Physique Nucleaire d' Orsay, Groupe de radiochimie, Bat. 100, 91406 Orsay (France)]. e-mail: edo@nuclear.inin.mx

    2005-07-01

    The stability of the uranyl sipped in the zirconium {tau}-hydrogen phosphate in sodic form ({tau}-NaZrP), was carried out characterizing the complexes formed by Laser spectroscopy in the visible region and by X-ray photoelectron spectroscopy. The material was prepared by a new synthesis technique working in nitrogen atmosphere and to low temperatures. The sorption of the uranyl ion was made in acid media with concentrations of 10{sup -4} and 10{sup -5} of uranyl nitrate and with ion forces of 0.1 and 0.5 M of NaClO{sub 4}. The spectra of induced fluorescence with laser (TRLFS) show that the uranyl is fixed in very acid media in three well differentiated species, to pH less acid, the specie of long half life disappears and are only those of short half life. The results of the binding energy obtained by XPS indicate that the binding energy of the uranyl confer it a stable character to the complex formed in the {tau}-NaZP, that makes to this material appropriate to retain to the uranyl in solution to high ion forces and in acid media. (Author)

  11. 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

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

    Science.gov (United States)

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

    2018-02-01

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

  13. 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.)

  14. Oxidation kinetics of reaction products formed in uranium metal corrosion

    International Nuclear Information System (INIS)

    Totemeier, T. C.

    1998-01-01

    The oxidation behavior of uranium metal ZPPR fuel corrosion products in environments of Ar-4%O 2 and Ar-20%O 2 were studied using thermo-gravimetric analysis (TGA). These tests were performed to extend earlier work in this area specifically, to assess plate-to-plate variations in corrosion product properties and the effect of oxygen concentration on oxidation behavior. The corrosion products from two relatively severely corroded plates were similar, while the products from a relatively intact plate were not reactive. Oxygen concentration strongly affected the burning rate of reactive products, but had little effect on low-temperature oxidation rates

  15. Oxidation kinetics of reaction products formed in uranium metal corrosion.

    Energy Technology Data Exchange (ETDEWEB)

    Totemeier, T. C.

    1998-04-22

    The oxidation behavior of uranium metal ZPPR fuel corrosion products in environments of Ar-4%O{sub 2} and Ar-20%O{sub 2} were studied using thermo-gravimetric analysis (TGA). These tests were performed to extend earlier work in this area specifically, to assess plate-to-plate variations in corrosion product properties and the effect of oxygen concentration on oxidation behavior. The corrosion products from two relatively severely corroded plates were similar, while the products from a relatively intact plate were not reactive. Oxygen concentration strongly affected the burning rate of reactive products, but had little effect on low-temperature oxidation rates.

  16. 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)

  17. Microstructural investigation of the oxide formed on TP 347H FG during long-term steam oxidation

    DEFF Research Database (Denmark)

    Hansson, Anette Nørgaard; Danielsen, Hilmar Kjartansson; Grumsen, Flemming Bjerg

    2010-01-01

    The long-term oxidation behaviour of TP347H FG in ultra supercritical steam conditions was assessed by exposing the steel in test superheater loops in a Danish coal-fired power plant and characterising the oxide layer with reflective light and electron microscopy. Double layered oxide scales formed...... during steam oxidation. TEM investigations reveal that the inner oxide layer consists of particles of metallic Ni/Fe and Fe-Cr spinel in the interior of the former alloy grains and a compact layer of Fe-Cr spinel and Cr2O3 along the former alloy grain boundaries. The morphology suggests that the inner...

  18. 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

  19. Effect of zirconium addition on welding of aluminum grain refined by titanium

    International Nuclear Information System (INIS)

    Zaid, A.I.O.

    2011-01-01

    Aluminum and its alloys solidify in large grains columnar structure which tends to reduce their mechanical behaviour and surface quality. Therefore, they are industrially grain refined by titanium or titanium + boron. Furthermore, aluminum oxidizes in ordinary atmosphere which makes its weldability difficult and weak. Therefore, it is anticipated that the effect of addition of zirconium at a weight percentages of 0.1% (which proved to be an effective grain refiner on the weldability of aluminum grain refined by Ti) is worthwhile investigating. This formed the objective of this research work. In this paper, the effect of zirconium addition at a weight percentage of 0.1%, which corresponds to the peritctic limit on the aluminum-zirconium phase diagram, on the weldability of aluminum grain refined by Ti is investigated. Rolled sheets of commercially pure aluminum, Al grain refined Ti of 3 mm thickness were welded together using Gas Tungsten Arc Welding method (GTAW), formerly known as TIG. A constant air gap was maintained at a constant current level, 30 ampere AC, was used because it removes the oxides of the welding process under the same process parameters. Metallographic examination of weldments of the different combinations of aluminum and its microalloys at the heat affected zone, HAZ, and base metal was carried out and examined for width, porosity, cracks and microhardness. It was found that grain refining of commercially pure aluminum by Ti resulted in enhancement of its weldability. Similarly, addition of zirconium to Al grain refined by Ti resulted in further enhancement of the weldment. Photomicrographs of the HAZ regions are presented and discussed. (author)

  20. 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.

  1. 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.

  2. 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

  3. The synthesis, characterization and properties of zirconium-chelating polymers

    International Nuclear Information System (INIS)

    Van Reenen, A.J.

    1985-12-01

    A series of homo- and copolymers based on the monomers : 2-propenoic acid, 2-methyl-2-propenoic acid, 2-chloro-2-propenoic acid, methylene butanedioic acid, ethenyl acetate and ethylene sulphonic acid have been synthesized and characterized. These polyelectrolytes were used with hydrous zirconium oxide to form novel dynamic membranes on Millipore filter substrates. These desalinating membranes were studied in terms of the chemical structure of the polyelectrolytes with regard to the effect of pH on their formation and performance characteristics. The effect of the charge density on the membranes was related to the membranes' figure of merit. Membrane studies were undertaken at pressures of 6 MPa and flow rates of 3,65 litres per minute. 59 figs., 20 tabs., 94 refs

  4. On the crystalline structures of iron oxides formed during the removal process of iron in water

    International Nuclear Information System (INIS)

    Cho, Bongyeon; Fujita, Kenji; Oda, Katsuro; Ino, Hiromitsu

    1993-01-01

    The iron oxide samples collected from both filtration and batch reactors were analysed by X-ray diffraction and Moessbauer spectroscopy. In the filtration of water containing iron, the oxidized form of iron was determined to be ferrihydrite. In contrast, in the batch experiment without filtration, iron was oxidized to microcrystalline goethite. (orig.)

  5. Raman spectroscopy used for structural investigations of anodically formed ZrO2

    International Nuclear Information System (INIS)

    Koneska, Zagorka; Arsova, Irena

    2003-01-01

    The structure of the oxide formed on Zr(99% + Hf) with anodic oxidation at different potentials in 1 mol/dm 3 H 3 PO 4 and 2 mol/dm 3 KOH solutions were investigated using Raman spectroscopy. Normally the anodic oxides of Zr form only crystals. Under certain circumstances, amorphous anodic ZrO 2 can be observed. Amorphous phase is observed for the anodically formed zirconium oxides in H 3 PO 4 . The oxide formed in KOH at potential of 80 V, where sparks appears on the Zr electrode showed crystalline structure. (Original)

  6. 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

  7. 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

  8. 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.

  9. Zirconium microstructures: uncharted possibilities

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  10. Zirconium elasticity modules

    International Nuclear Information System (INIS)

    Vavra, G.

    1978-01-01

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

  11. 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)

  12. 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

  13. Zirconium carbide coating for corium experiments related to water-cooled and sodium-cooled reactors

    Energy Technology Data Exchange (ETDEWEB)

    Plevacova, K. [CEA, DEN, STRI, LMA, Cadarache, 3108 St. Paul lez Durance (France); Journeau, C., E-mail: christophe.journeau@cea.fr [CEA, DEN, STRI, LMA, Cadarache, 3108 St. Paul lez Durance (France); Piluso, P. [CEA, DEN, STRI, LMA, Cadarache, 3108 St. Paul lez Durance (France); Zhdanov, V.; Baklanov, V. [IAE, National Nuclear Centre, Material Structure Investigation Dept., Krasnoarmeiskaya, 10, Kurchatov City (Kazakhstan); Poirier, J. [CEMHTI, 1D, av. de la Recherche Scientifique, 45071 Orleans Cedex 2 (France)

    2011-07-01

    Since the TMI and Chernobyl accidents the risk of nuclear severe accident is intensively studied for existing and future reactors. In case of a core melt-down accident in a nuclear reactor, a complex melt, called corium, forms. To be able to perform experiments with prototypic corium materials at high temperature, a coating which resists to different corium melts related to Generation I and II Water Reactors and Generation IV sodium fast reactor was researched in our experimental platforms both in IAE NNC in Kazakhstan and in CEA in France. Zirconium carbide was selected as protective coating for graphite crucibles used in our induction furnaces: VCG-135 and VITI. The method of coating application, called reactive wetting, was developed. Zirconium carbide revealed to resist well to the (U{sub x}, Zr{sub y})O{sub 2-z} water reactor corium. It has also the advantage not to bring new elements to this chemical system. The coating was then tested with sodium fast reactor corium melts containing steel or absorbers. Undesirable interactions were observed between the coating and these materials, leading to the carburization of the corium ingots. Concerning the resistance of the coating to oxide melts without ZrO{sub 2}, the zirconium carbide coating keeps its role of protective barrier with UO{sub 2}-Al{sub 2}O{sub 3} below 2000 deg. C but does not resist to a UO{sub 2}-Eu{sub 2}O{sub 3} mixture.

  14. 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)

  15. ENTIRELY AQUEOUS SOLUTION-GEL ROUTE FOR THE PREPARATION OF ZIRCONIUM CARBIDE, HAFNIUM CARBIDE AND THEIR TERNARY CARBIDE POWDERS

    Directory of Open Access Journals (Sweden)

    Zhang Changrui

    2016-07-01

    Full Text Available An entirely aqueous solution-gel route has been developed for the synthesis of zirconium carbide, hafnium carbide and their ternary carbide powders. Zirconium oxychloride (ZrOCl₂.8H₂O, malic acid (MA and ethylene glycol (EG were dissolved in water to form the aqueous zirconium carbide precursor. Afterwards, this aqueous precursor was gelled and transformed into zirconium carbide at a relatively low temperature (1200 °C for achieving an intimate mixing of the intermediate products. Hafnium and the ternary carbide powders were also synthesized via the same aqueous route. All the zirconium, hafnium and ternary carbide powders exhibited a particle size of ∼100 nm.

  16. Direct Reaction of Amides with Nitric Oxide To Form Diazeniumdiolates

    Science.gov (United States)

    2015-01-01

    We report the apparently unprecedented direct reaction of nitric oxide (NO) with amides to generate ions of structure R(C=O)NH–N(O)=NO–, with examples including R = Me (1a) or 3-pyridyl (1b). The sodium salts of both released NO in pH 7.4 buffer, with 37 °C half-lives of 1–3 min. As NO-releasing drug candidates, diazeniumdiolated amides would have the advantage of generating only 1 equiv of base on hydrolyzing exhaustively to NO, in contrast to their amine counterparts, which generate 2 equiv of base. PMID:25210948

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

    International Nuclear Information System (INIS)

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

    2016-01-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2016-10-15

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

  19. The oxidation kinetics for sublimates formed during niobium electron-beam remelting

    International Nuclear Information System (INIS)

    Chumarev, V.M.; Gulyaeva, R.I.; Mar'evich, V.P.; Upolovnikova, A.G.; Udoeva, L.Yu.

    2003-01-01

    The oxidation of sublimates of Nb-Al electron beam remelting is investigated under conditions of isothermal and continuous heating in the air. It is stated that basic oxidation products are niobium and aluminium oxides, as well as aluminium niobates of variable composition of Al 2 O 3 · mNb 2 O 5 . The more aluminium enriched sublimates possess an increased resistance to oxidation. Formed in sublimates NbAl 3 intermetallic compound features the highest heat resistance. Oxidation parameters are determined by the method of nonisothermic kinetics. It is noted that the running processes exhibit a multistage nature and are limited by internal diffusion [ru

  20. Plutonium transport for the oxide form. Air and road accidentology

    International Nuclear Information System (INIS)

    Degrange, J.P.; Hubert, P.; Pages, P.

    1989-07-01

    The aim of the study is to define the probability of accident that can be applied to a packaging for plutonium oxide transport. The analysis is designed essentially for packagings of few tons with impact resistance corresponding to a speed of 10 m/s but can be used for packagings with a resistance corresponding to IAEA tests. This work is based on analysis and processing of 2 accident files: one on road accidents, the other on air accidents. Computer codes are developed, from one hand, to obtain stress indicator distribution by Monte Carlo methods and on the other hand to link these distributions to itinerary parameters. Previous similar studies are examined and compared to figures obtained here and explained as far as possible [fr

  1. 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

  2. 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.

  3. 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

  4. Influence of rare earth additions on the oxidation resistance of chromia forming alloys

    International Nuclear Information System (INIS)

    Pillis, Marina Fuser

    1995-01-01

    The addition of rare earths to alloys, either in elemental form or as surface coatings reduces the oxidation rate of chromia forming alloys. The rare earths either act as nucleation sites for surface oxides or get incorporates into the surface oxide and diffuse to oxide grain boundaries. If the latter occurs, a change in the defect structure close to the grain boundaries, probably takes place. In this manner, the rare earths inhibits the movement of chromium ions to the oxide/gas interface. The influence of rare earth additions to AISI 316, AISI 316L and Ni-20 Cr on their oxidation behavior has been studied., AISI 316+Ce, AISI 316+Y, Ni-20 Cr and Ni-20 Cr-2 Al-1 Ce were prepared by melting and AISI 316L, AISI 316L+Ce O 2 and AISI 316L+Y 2 O 3 by powder compaction. The effect of superficial deposits of rare earth oxides was also studied. The alloys were coated with rare earth oxides by high temperature conversion of the respective rare earth nitrates. Isothermal oxidation tests were carried out at 900-1100 deg C and the cyclic oxidation tests consisted of 6 cycles of 2 hours each at 900 deg C, followed by cooling to room temperature. All the tests were carried out in air. Oxidation behavior was evaluated gravimetrically. Scanning electron microscopy was used to study surface morphology. Energy dispersive analysis and X-ray diffraction techniques were used to identify oxide constituents. Overall, it has been observed that with the addition of rare earths, oxidation resistance increases by decreasing oxidation rates and increasing oxide adhesion. Addition of rare earths to AISI 316 prepared by melting resulted in rapid formation of a chromium rich oxide layered near the metal/oxide interface which reduced overall oxidation rate. The addition of Ce O 2 to AISI 316L was found to improve oxidation behavior after 10 hours at 1100 deg C and also inhibit the formation of volatile Cr O 3 . The isothermal oxidation behavior of rare earth oxide covered Ni-20 Cr at 900 deg C

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

    Science.gov (United States)

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

    2017-06-01

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

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

    Energy Technology Data Exchange (ETDEWEB)

    Katunar, Maria R, E-mail: mkatunar@fi.mdp.edu.ar [INTEMA, Universidad Nacional de Mar del Plata-CONICET, Juan B. Justo, 4302, B7608FDQ, Mar del Plata (Argentina); Gomez Sanchez, Andrea [INTEMA, Universidad Nacional de Mar del Plata-CONICET, Juan B. Justo, 4302, B7608FDQ, Mar del Plata (Argentina); Santos Coquillat, Ana [Instituto de Estudios Biofuncionales, Universidad Complutense de Madrid, Madrid, España (Spain); Civantos, Ana [Instituto de Ciencia y Tecnología de Polímeros, CSIC, Madrid (Spain); Martinez Campos, Enrique [Instituto de Estudios Biofuncionales, Universidad Complutense de Madrid, Madrid, España (Spain); Ballarre, Josefina; Vico, Tamara [INTEMA, Universidad Nacional de Mar del Plata-CONICET, Juan B. Justo, 4302, B7608FDQ, Mar del Plata (Argentina); Baca, Matias [Traumatologia y Ortopedia, Hospital Interzonal General de Agudos “Oscar Alende”, Mar del Plata (Argentina); Ramos, Viviana [Instituto de Ciencia y Tecnología de Polímeros, CSIC, Madrid (Spain); Cere, Silvia [INTEMA, Universidad Nacional de Mar del Plata-CONICET, Juan B. Justo, 4302, B7608FDQ, Mar del Plata (Argentina)

    2017-06-01

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

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  8. 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)

  9. 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.

  10. Characterization of low-temperature microwave loss of thin aluminum oxide formed by plasma oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Deng, Chunqing, E-mail: cdeng@uwaterloo.ca; Otto, M.; Lupascu, A., E-mail: alupascu@uwaterloo.ca [Institute for Quantum Computing, Department of Physics and Astronomy, and Waterloo Institute for Nanotechnology, University of Waterloo, Waterloo, Ontario N2L 3G1 (Canada)

    2014-01-27

    We report on the characterization of microwave loss of thin aluminum oxide films at low temperatures using superconducting lumped resonators. The oxide films are fabricated using plasma oxidation of aluminum and have a thickness of 5 nm. We measure the dielectric loss versus microwave power for resonators with frequencies in the GHz range at temperatures from 54 to 303 mK. The power and temperature dependence of the loss are consistent with the tunneling two-level system theory. These results are relevant to understanding decoherence in superconducting quantum devices. The obtained oxide films are thin and robust, making them suitable for capacitors in compact microwave resonators.

  11. Influence of rare earth oxides in the oxidation of chromia forming alloys

    International Nuclear Information System (INIS)

    Ramanathan, L.V.

    1989-01-01

    The influence of superficial application of rare earth oxides such as CeO sub(2), La sub(2)O sub(3), Nd sub(2)O sub(3), Sm sub(2)O sub(3), and Gd sub(2)O sub (3) to AISI 304 and 310 stainless steels, on their isothermal oxidation behavior at 900 sup(0) and 1000 sup(0)C, and cyclic oxidation behavior between 20 sup(0) and 1000 sup(0)C has been studied. The application of rare earth oxides (REO) has been found to increase the oxidation resistance at AISI 304. No significant improvements in oxidation resistance of AISI 310 were noted. The oxidation resistance of AISI 304 was highest in the presence of CeO sub(2) on its surface. The other REO in decreasing order of influence on oxidation resistance are La sub(2)O sub(3), Nd sub(2)O sub(3), Sm sub(2)O sub(3) and Gd sub(2)O sub(3). SEM investigations of the oxide scale morphology revealed that the improved resistance is probably due to the formation of a thin layer of fine grained compact Cr sub(2)O sub(3) and the higher adhesion of the scale to its increased plasticity. (author)

  12. 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/ .

  13. 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

  14. Microstructure and protection characteristics of the naturally formed oxide films on Mg–xZn alloys

    International Nuclear Information System (INIS)

    Song, Yingwei; Han, En-Hou; Dong, Kaihui; Shan, Dayong; Yim, Chang Dong; You, Bong Sun

    2013-01-01

    Highlights: •The oxide films on Mg–xZn alloys consist of similar chemical composition. •The higher Zn content results in the thicker but higher defect of the oxide films. •The oxide films exhibit different protection performance under various potentials. -- Abstract: The naturally formed oxide films on Mg–2Zn and Mg–5Zn alloys were investigated by atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and electrochemical measurements. The oxide films on the both alloys present a similar chemical composition, consisting of surface layer of basic magnesium carbonate and MgO following with MgO and ZnO, but the oxide film on Mg–5Zn is thicker and contains more defects. The protection performance of the oxide film on Mg–5Zn is worse under open circuit potential but better in a suitable anodic potential scope compared with that on Mg–2Zn alloy

  15. Infrared absorption study of ammonium uranates and uranium oxide powders formed during their thermal decomposition

    International Nuclear Information System (INIS)

    Rofail, N.H.; ELfekey, S.A.

    1992-01-01

    Ammonium uranates (AU) were precipitated from a nuclear-pure uranyl nitrate solution using different precipitating agents. IR spectra of the obtained uranates and oxides formed during their thermal decomposition have been studied. The results indicated that the precipitating agent, mode of stirring, washing and calcining temperature are important factors for a specific oxide formation.4 FIG., 3 TAB

  16. Distribution of antimony in the oxide layer formed by potentiostatic oxidation of Pb-Sb alloy

    Energy Technology Data Exchange (ETDEWEB)

    Arifuku, F.; Yoneyama, H.; Tamura, H.

    1979-09-01

    The distribution of antimony within the oxide films on Pb-Sb alloy prepared by potentiostatic oxidation in H/sub 2/SO/sub 4/ solutions was examined by SIMS. The study of oxide films prepared by applying different potentials for three hours showed that two types of film were obtained depending on whether the potential was more negative or more positive than 1.5 V. Antimony profiles were obtained for films at several stages in the initial growth. It was found that antimony was retained in the oxide film at 1.5 V during both nucleation and two- or three-dimensional growth of PbO/sub 2/ and at 1.6 V during the lateral overlaps of three-dimensional centers of PbO/sub 2/. Relationships between the antimony distribution profiles and the oxide film growth are discussed. 8 figures, 1 table.

  17. Oxidation of triclosan by permanganate (Mn(VII)): importance of ligands and in situ formed manganese oxides.

    Science.gov (United States)

    Jiang, Jin; Pang, Su-Yan; Ma, Jun

    2009-11-01

    Experiments were conducted to examine permanganate (Mn(VII); KMnO(4)) oxidation of the widely used biocide triclosan (one phenolic derivative) in aqueous solution at pH values of 5-9. Under slightly acidic conditions, the reactions displayed autocatalysis, suggesting the catalytic role of in situ formed MnO(2). This was further supported by the promoting effects of the addition of preformed MnO(2) colloids on Mn(VII) oxidations of triclosan and two other selected phenolics (i.e., phenol and 2,4-dichlorophenol), as well as p-nitrophenol which otherwise showed negligible reactivity toward Mn(VII) and MnO(2) colloids, respectively. Surprisingly, phosphate buffer significantly enhanced Mn(VII) oxidation of triclosan, as well as phenol and 2,4-dichlorophenol over a wide pH range. Further, several other selected ligands (i.e., pyrophosphate, EDTA, and humic acid) also exerted oxidation enhancement, supporting a scenario where highly active aqueous manganese intermediates (Mn(INT)(aq)) formed in situ upon Mn(VII) reduction might be stabilized to a certain extent in the presence of ligands and subsequently involved in further oxidation of target phenolics, whereas without stabilizing agents Mn(INT)(aq) autodecomposes or disproportionates spontaneously. The effectiveness of Mn(VII) for the oxidative removal of triclosan in natural water and wastewater was confirmed. Their background matrices were also found to accelerate Mn(VII) oxidation of phenolics.

  18. 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...

  19. 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)

  20. 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.

  1. Process for forming a homogeneous oxide solid phase of catalytically active material

    Science.gov (United States)

    Perry, Dale L.; Russo, Richard E.; Mao, Xianglei

    1995-01-01

    A process is disclosed for forming a homogeneous oxide solid phase reaction product of catalytically active material comprising one or more alkali metals, one or more alkaline earth metals, and one or more Group VIII transition metals. The process comprises reacting together one or more alkali metal oxides and/or salts, one or more alkaline earth metal oxides and/or salts, one or more Group VIII transition metal oxides and/or salts, capable of forming a catalytically active reaction product, in the optional presence of an additional source of oxygen, using a laser beam to ablate from a target such metal compound reactants in the form of a vapor in a deposition chamber, resulting in the deposition, on a heated substrate in the chamber, of the desired oxide phase reaction product. The resulting product may be formed in variable, but reproducible, stoichiometric ratios. The homogeneous oxide solid phase product is useful as a catalyst, and can be produced in many physical forms, including thin films, particulate forms, coatings on catalyst support structures, and coatings on structures used in reaction apparatus in which the reaction product of the invention will serve as a catalyst.

  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. 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

  4. 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%.

  5. Local electrical properties of thermally grown oxide films formed on duplex stainless steel surfaces

    Science.gov (United States)

    Guo, L. Q.; Yang, B. J.; He, J. Y.; Qiao, L. J.

    2018-06-01

    The local electrical properties of thermally grown oxide films formed on ferrite and austenite surfaces of duplex stainless steel at different temperatures were investigated by Current sensing atomic force microscopy, X-ray Photoelectron Spectroscopy (XPS) and Auger Electron Spectroscopy (AES). The current maps and XPS/AES analyses show that the oxide films covering austenite and ferrite surfaces formed at different temperatures exhibit different local electrical characteristics, thickness and composition. The dependence of electrical conductivity of oxide films covering austenite and ferrite surface on the formation temperature is attributed to the film thickness and semiconducting structures, which is intrinsically related to thermodynamics and kinetics process of film grown at different temperature. This is well elucidated by corresponding semiconductor band structures of oxide films formed on austenite and ferrite phases at different temperature.

  6. 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

  7. Minimalistic Liquid-Assisted Route to Highly Crystalline α-Zirconium Phosphate.

    Science.gov (United States)

    Cheng, Yu; Wang, Xiaodong Tony; Jaenicke, Stephan; Chuah, Gaik-Khuan

    2017-08-24

    Zirconium phosphates have potential applications in areas of ion exchange, catalysis, photochemistry, and biotechnology. However, synthesis methodologies to form crystalline α-zirconium phosphate (Zr(HPO 4 ) 2 ⋅H 2 O) typically involve the use of excess phosphoric acid, addition of HF or oxalic acid and long reflux times or hydrothermal conditions. A minimalistic sustainable route to its synthesis has been developed by using only zirconium oxychloride and concentrated phosphoric acid to form highly crystalline α-zirconium phosphate within hours. The morphology can be changed from platelets to rod-shaped particles by fluoride addition. By varying the temperature and time, α-zirconium phosphate with particle sizes from nanometers to microns can be obtained. Key features of this minimal solvent synthesis are the excellent yields obtained with high atom economy under mild conditions and ease of scalability. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. A Novel Investigation of the Formation of Titanium Oxide Nanotubes on Thermally Formed Oxide of Ti-6Al-4V.

    Science.gov (United States)

    Butt, Arman; Hamlekhan, Azhang; Patel, Sweetu; Royhman, Dmitry; Sukotjo, Cortino; Mathew, Mathew T; Shokuhfar, Tolou; Takoudis, Christos

    2015-10-01

    Traditionally, titanium oxide (TiO2) nanotubes (TNTs) are anodized on Ti-6Al-4V alloy (Ti-V) surfaces with native TiO2 (amorphous TiO2); subsequent heat treatment of anodized surfaces has been observed to enhance cellular response. As-is bulk Ti-V, however, is often subjected to heat treatment, such as thermal oxidation (TO), to improve its mechanical properties. Thermal oxidation treatment of Ti-V at temperatures greater than 200°C and 400°C initiates the formation of anatase and rutile TiO2, respectively, which can affect TNT formation. This study aims at understanding the TNT formation mechanism on Ti-V surfaces with TO-formed TiO2 compared with that on as-is Ti-V surfaces with native oxide. Thermal oxidation-formed TiO2 can affect TNT formation and surface wettability because TO-formed TiO2 is expected to be part of the TNT structure. Surface characterization was carried out with field emission scanning electron microscopy, energy dispersive x-ray spectroscopy, water contact angle measurements, and white light interferometry. The TNTs were formed on control and 300°C and 600°C TO-treated Ti-V samples, and significant differences in TNT lengths and surface morphology were observed. No difference in elemental composition was found. Thermal oxidation and TO/anodization treatments produced hydrophilic surfaces, while hydrophobic behavior was observed over time (aging) for all samples. Reduced hydrophobic behavior was observed for TO/anodized samples when compared with control, control/anodized, and TO-treated samples. A method for improved surface wettability and TNT morphology is therefore discussed for possible applications in effective osseointegration of dental and orthopedic implants.

  9. Nitrous oxide-forming codenitrification catalyzed by cytochrome P450nor.

    Science.gov (United States)

    Su, Fei; Takaya, Naoki; Shoun, Hirofumi

    2004-02-01

    Intact cells of the denitrifying fungus Fusarium oxysporum were previously shown to catalyze codenitrification to form a hybrid nitrous oxide (N2O) species from nitrite and other nitrogen compounds such as azide and ammonia. Here we show that cytochrome P450nor can catalyze the codenitrification reaction to form N2O from nitric oxide (NO) but not nitrite, and azide or ammonia. The results show that the direct substrate of the codenitrification by intact cells should not be nitrite but NO, which is formed from nitrite by the reaction of a dissimilatory nitrite reductase.

  10. 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.

  11. 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)

  12. Tunnel Oxides Formed by Field-Induced Anodisation for Passivated Contacts of Silicon Solar Cells

    Directory of Open Access Journals (Sweden)

    Jingnan Tong

    2018-02-01

    Full Text Available Tunnel silicon oxides form a critical component for passivated contacts for silicon solar cells. They need to be sufficiently thin to allow carriers to tunnel through and to be uniform both in thickness and stoichiometry across the silicon wafer surface, to ensure uniform and low recombination velocities if high conversion efficiencies are to be achieved. This paper reports on the formation of ultra-thin silicon oxide layers by field-induced anodisation (FIA, a process that ensures uniform oxide thickness by passing the anodisation current perpendicularly through the wafer to the silicon surface that is anodised. Spectroscopical analyses show that the FIA oxides contain a lower fraction of Si-rich sub-oxides compared to wet-chemical oxides, resulting in lower recombination velocities at the silicon and oxide interface. This property along with its low temperature formation highlights the potential for FIA to be used to form low-cost tunnel oxide layers for passivated contacts of silicon solar cells.

  13. Semiconducting properties of oxide and passive films formed on AISI 304 stainless steel and Alloy 600

    Directory of Open Access Journals (Sweden)

    Ferreira M. G. S.

    2002-01-01

    Full Text Available The semiconducting properties of passive films formed on AISI 304 stainless steel and Alloy 600 in borate buffer solution were studied by capacitance (Mott-Schottky approach and photocurrent measurements. Oxide films formed on 304 stainless steel in air at 350 ºC have also been studied. The results obtained show that, in all cases the electronic structure of the films is comparable to that of a p-n heterojunction in which the space charges developed at the metal-film and film-electrolyte interfaces have also to be considered. This is in accordance with analytical results showing that the oxide films are in all cases composed of an inner region rich in chromium oxide and an outer region rich in iron oxide.

  14. XPS and SEM studies of chromium oxide films chemically formed on stainless steel 316 L

    International Nuclear Information System (INIS)

    Stefanov, P.; Marinova, T.

    2000-01-01

    The structure and composition of chromium oxide films formed on stainless steel by immersion in a chromium electrolyte have been studied by SEM and XPS. Cr 2 O 3 crystallites in the range 30-150 nm are fully developed and cover the whole surface. The chemical composition in the depth and the thickness of the oxide layer have been determined by XPS sputter profiles. The oxide film can be described within the framework of a double layer consisting of a thin outer hydrated layer and an inner layer of Cr 2 O 3 . (orig.)

  15. Dissolution of various metal oxides in different forms in dilute organic complexants

    International Nuclear Information System (INIS)

    Srinivasan, M.P.; Chandramohan, P.; Velmurugan, S.; Narasimhan, S.V.; Ranganathan, S.

    2002-01-01

    The dissolution of iron containing metal oxides is of importance in various power plant industries from the point of crud and scale removal for efficient operation and better performance of plant. The removal of these oxides has to be accomplished with minimum corrosion to the structural material, with minimum cost and removal duration and also with minimum waste generation for easy disposal. Activity build-up due to pick up of 60 Co and fission products occurs on PHT system surfaces of nuclear power plants. The dissolution kinetics of these oxides are influenced by pH, redox potential, chelating strength, concentration and temperature of the solution, constitution of oxides, and the physical form of existence of oxides. In this paper the influence of the existence of different forms of iron oxides on the ability of the dissolution characteristics of the different formulations have been brought out. How the change in dissolution characteristics can be ingenuously used to characterize both qualitatively and quantitatively the mixtures of oxides have been brought out. How the magnetite dissolution behaviour varies for base metal unaided condition in different formulation in static condition, in regenerative mode is also brought out. The OCP values and iron release behaviour for magnetite coated CS surface and magnetite pellet were also described. (authors)

  16. Dissolution of various metal oxides in different forms in dilute organic complexants

    Energy Technology Data Exchange (ETDEWEB)

    Srinivasan, M.P.; Chandramohan, P.; Velmurugan, S.; Narasimhan, S.V. [Water and Steam Chemistry Lab., BARC Facilities, Tamilnadu (India); Ranganathan, S. [Madras Univ. (India). Research Scholar

    2002-07-01

    The dissolution of iron containing metal oxides is of importance in various power plant industries from the point of crud and scale removal for efficient operation and better performance of plant. The removal of these oxides has to be accomplished with minimum corrosion to the structural material, with minimum cost and removal duration and also with minimum waste generation for easy disposal. Activity build-up due to pick up of {sup 60}Co and fission products occurs on PHT system surfaces of nuclear power plants. The dissolution kinetics of these oxides are influenced by pH, redox potential, chelating strength, concentration and temperature of the solution, constitution of oxides, and the physical form of existence of oxides. In this paper the influence of the existence of different forms of iron oxides on the ability of the dissolution characteristics of the different formulations have been brought out. How the change in dissolution characteristics can be ingenuously used to characterize both qualitatively and quantitatively the mixtures of oxides have been brought out. How the magnetite dissolution behaviour varies for base metal unaided condition in different formulation in static condition, in regenerative mode is also brought out. The OCP values and iron release behaviour for magnetite coated CS surface and magnetite pellet were also described. (authors)

  17. Electrochemical characterization of oxide film formed at high temperature on Alloy 690

    Energy Technology Data Exchange (ETDEWEB)

    Abraham, Geogy J., E-mail: gja@barc.gov.in [Materials Science Division, BARC, Mumbai 400 085 (India); Bhambroo, Rajan [Deptt. of Metallurgical Engg. and Mat. Sci., IIT Bombay, Mumbai 400 076 (India); Kain, V. [Materials Science Division, BARC, Mumbai 400 085 (India); Shekhar, R. [CCCM, BARC, Hyderabad 500 062 (India); Dey, G.K. [Materials Science Division, BARC, Mumbai 400 085 (India); Raja, V.S. [Deptt. of Metallurgical Engg. and Mat. Sci., IIT Bombay, Mumbai 400 076 (India)

    2012-02-15

    Highlights: Black-Right-Pointing-Pointer GD-QMS studies of high temperature oxide film formed on Alloy 690. Black-Right-Pointing-Pointer Defect density reduced with increase in temperature. Black-Right-Pointing-Pointer Electrochemical behaviour of oxide film correlated to the Cr-content in oxide. - Abstract: High temperature passivation studies on Alloy 690 were carried out in lithiated water at 250 Degree-Sign C, 275 Degree-Sign C and 300 Degree-Sign C for 72 h. The passive films were characterized by glow discharge-quadrupole mass spectroscopy (GD-QMS) for compositional variation across the depth and micro laser Raman spectroscopy for oxide composition on the surface. The defect density in the oxide films was established from the Mott-Schottky analysis using electrochemical impedance spectroscopy. Electrochemical experiments at room temperature in chloride medium revealed best passivity behaviour by the oxide film formed at 300 Degree-Sign C for 72 h. The electrochemical studies were correlated to the chromium (and oxygen) content of the oxide films. Autoclaving at 300 Degree-Sign C resulted in the best passive film formation on Alloy 690 in lithiated water.

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

    Directory of Open Access Journals (Sweden)

    Nakane K.

    2013-01-01

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

  19. 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...

  20. 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.

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

    International Nuclear Information System (INIS)

    Ratanalert, N.

    1985-01-01

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

  2. Method of fabricating zirconium metal for use in composite type fuel cans

    International Nuclear Information System (INIS)

    Imahashi, Hiromichi; Inagaki, Masatoshi; Akabori, Kimihiko; Tada, Naofumi; Yasuda, Tetsuro.

    1985-01-01

    Purpose: To mass produce zirconium metal for fuel cans with less radiation hardening. Method: Zirconium sponges as raw material are inserted in a hearth mold and a procedure of melting the zirconium sponges portionwise by using a melting furnace having electron beams as a heat source while moving the hearth is repeated at least for once. Then, the rod-like ingot after melting is melted again in a vacuum or inert gas atmosphere into an ingot of a low oxygen density capable of fabrication. A composite fuel can billet is formed by using the thus obtained zirconium ingot and a zircalloy, and a predetermined composite type fuel can is manufactured by way of hot extrusion and pipe drawing fabrication. The raw material usable herein is zirconium sponge with an oxygen density of 400 ppm or higher and the content of impurity other than oxygen is between 1000 - 5000 ppm in total, or the molten material thereof. (Kamimura, M.)

  3. 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.

  4. 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)

  5. 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

  6. 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)

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

    International Nuclear Information System (INIS)

    Dittmer, G.; Niemann, U.

    1987-01-01

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

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

    International Nuclear Information System (INIS)

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

    1978-01-01

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

  9. 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

  10. 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.

  11. 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

  12. Transparent indium-tin oxide/indium-gallium-zinc oxide Schottky diodes formed by gradient oxygen doping

    Science.gov (United States)

    Ho, Szuheng; Yu, Hyeonggeun; So, Franky

    2017-11-01

    Amorphous InGaZnO (a-IGZO) is promising for transparent electronics due to its high carrier mobility and optical transparency. However, most metal/a-IGZO junctions are ohmic due to the Fermi-level pinning at the interface, restricting their device applications. Here, we report that indium-tin oxide/a-IGZO Schottky diodes can be formed by gradient oxygen doping in the a-IGZO layer that would otherwise form an ohmic contact. Making use of back-to-back a-IGZO Schottky junctions, a transparent IGZO permeable metal-base transistor is also demonstrated with a high common-base gain.

  13. Study on the CMP characteristics of a copper passivity layer formed by dipping in an oxidizer

    International Nuclear Information System (INIS)

    Choi, Youn-Ok; Lee, Woo-Sun; Choi, Gwon-Woo; Lee, Kang-Yeon; Kim, Nam-Oh

    2011-01-01

    Copper has been the material for ultra-large-scale integrated circuits owing to its excellent electromigration resistance and low electrical resistance. The polishing mechanism of metal chemical mechanical polishing (CMP) has been reported to be a repeated process of passive oxide layer formation through the use of on oxidizer and then the abrasion action of the slurry. However, because copper is softer and more sensitive to corrosion than tungsten, the slurry composition and the polishing mechanism during the copper CMP process may be more complicated. In a general Cu-CMP process, a mixture of an alumina-based slurry and an oxidizer in proper proportion is used in order to form a passive oxide layer such as CuO and CuO 2 . However, a conventional CMP process consumes an unnecessary amount of slurry to formed the passive layer. Therefore, in this paper, we propose a new method. The copper samples were oxidized by dipping in an oxidizer for an appropriate time to minimize the consumption of slurry before the CMP process. Then, we performed the CMP process. In order to compare the polishing characteristics of the copper thin film, we discuss the CMP removal rate and non-uniformity, as well as the microstructure of the surface and a layer cross-section based on a scanning.

  14. 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

  15. Formation of zirconium nitride via mechanochemical decomposition of zircon

    International Nuclear Information System (INIS)

    Puclin, T.; Kaczmarek, W.A.

    1996-01-01

    In this paper we report some results of the mechanochemical reduction of zircon, and for the first time subsequent reaction with nitrogen to form zirconium nitride (ZrN). This process can be described by the equation: 3ZrSiO 4 + 8Al + 1.5N 2 = 4Al 2 O 3 + 3ZrN + 3Si. Milling was carried out in three steps: 1) low speed grinding of Al+ZrSiO 4 in vacuum, 2) high speed milling to effect the reduction, and 3) continued milling after the addition of nitrogen. Powders produced were examined by X-ray diffraction. The first step showed no reaction occurred during low speed grinding. The second step proved to be a slow reaction without the 'ignition' often seen in other mechanochemical reduction works. The final step was also gradual, and did not always go to full nitridation over the duration of the experiment, giving a product of composition ZrN 0.6 to ZrN l.0 . This is quite acceptable as transition metal nitrides are often non-stoichiometric. These results show that the formation of a useful hard material such as ZrN can be formed from a raw mineral by two stage mechanochemical processing. Further investigations are currently being undertaken to eliminate Fe contamination and produce pure ceramic oxide-nitride composites

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

    Science.gov (United States)

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

    2018-02-01

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

  17. Spectro-electrochemical and DFT study of tenoxicam metabolites formed by electrochemical oxidation

    International Nuclear Information System (INIS)

    Ramírez-Silva, M.T.; Guzmán-Hernández, D.S.; Galano, A.; Rojas-Hernández, A.; Corona-Avendaño, S.; Romero-Romo, M.; Palomar-Pardavé, M.

    2013-01-01

    Highlights: • Tenoxicam deprotonation and electrochemical oxidation were studied. • Both spectro-electrochemical and theoretical DFT studies were considered. • It was found that the ampholitic species of tenoxicam is a zwitterion. • Electrochemical oxidation of tenoxicam yields two non-electroactive products. • The nature of these fragments was further confirmed by a chromatography study. -- Abstract: From experimental (spectro-electrochemical) and theoretical (DFT) studies, the mechanisms of tenoxicam deprotonation and electrochemical oxidation were assessed. From these studies, new insights on the nature of the ampholitic species involved during tenoxicam's deprotonation in aqueous solution are presented; see scheme A. Moreover, it is shown that, after the analysis of two different reaction schemes that involve up to 10 different molecules and 12 reaction paths, the electrochemical oxidation of tenoxicam, yields two non-electroactive products that are predominately formed by its fragmentation, after the loss of two electrons. The nature of these fragments was further confirmed by a chromatography study

  18. Luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid

    International Nuclear Information System (INIS)

    Stojadinovic, S.; Vasilic, R.; Petkovic, M.; Nedic, Z.; Kasalica, B.; Belca, I.; Zekovic, Lj.

    2010-01-01

    In this paper, we have investigated luminescence properties of oxide films formed by anodization of aluminum in 12-tungstophosphoric acid. For the first time we have measured weak luminescence during anodization of aluminum in this electrolyte (so-called galvanoluminescence GL) and showed that there are wide GL bands in the visible region of the spectrum and observed two dominant spectral peaks. The first one is at about 425 nm, and the second one shifts with anodization voltage. As the anodization voltage approaches the breakdown voltage, a large number of sparks appear superimposed on the anodic GL. Several intensive band peaks were observed under breakdown caused by electron transitions in W, P, Al, O, H atoms. Furthermore, photoluminescence (PL) of anodic oxide films and anodic-spark formed oxide coatings were performed. In both cases wide PL bands in the range from 320 nm to 600 nm were observed.

  19. Comparison of Oxidative Stresses Mediated by Different Crystalline Forms and Surface Modification of Titanium Dioxide Nanoparticles

    Directory of Open Access Journals (Sweden)

    Karim Samy El-Said

    2015-01-01

    Full Text Available Titanium dioxide nanoparticles (TiO2 NPs are manufactured worldwide for use in a wide range of applications. There are two common crystalline forms of TiO2 anatase and rutile with different physical and chemical characteristics. We previously demonstrated that an increased DNA damage response is mediated by anatase crystalline form compared to rutile. In the present study, we conjugated TiO2 NPs with polyethylene glycol (PEG in order to reduce the genotoxicity and we evaluated some oxidative stress parameters to obtain information on the cellular mechanisms of DNA damage that operate in response to TiO2 NPs different crystalline forms exposure in hepatocarcinoma cell lines (HepG2. Our results indicated a significant increase in oxidative stress mediated by the anatase form of TiO2 NPs compared to rutile form. On the other hand, PEG modified TiO2 NPs showed a significant decrease in oxidative stress as compared to TiO2 NPs. These data suggested that the genotoxic potential of TiO2 NPs varies with crystalline form and surface modification.

  20. 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

  1. Niobium oxide nanocolumns formed via anodic alumina with modulated pore diameters

    Science.gov (United States)

    Pligovka, A.; Zakhlebayeva, A.; Lazavenka, A.

    2018-03-01

    Niobium oxide nanocolumns with modulated diameters were formed for the first time. An Al/Nb bilayer specimen was prepared by successive sputter-deposition of 300 nm niobium layer and 1200 nm aluminum layer onto silicon wafer. Regular anodic alumina matrix with modulated pore diameters was formed by sequential anodization of initial specimen in tartaric acid at 180 V, and in oxalic acid at 37 V. Further potentiodynamic reanodization of the specimen up to 400 V causes the simultaneous growth of 440 nm continuous niobium oxide layer beneath the alumina film and two types of an array of oxide nanocolumns (thick – with 100 nm width and 630 nm high and thin – with 25 nm width and 170 nm high), which are the filling of the alumina pores. The morphology of the formed anodic niobium oxide nanocolumns with modulated diameters was determined by field emission scanning electron microscopy. The formed nanostructures can be used for perspective devices of nano- and optoelectronics such as photonic crystals.

  2. 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

  3. [Apatite-forming ability of pure titanium implant after micro-arc oxidation treatment].

    Science.gov (United States)

    Tian, Zhihui; Zhang, Yu; Wang, Lichao; Nan, Kaihui

    2013-10-01

    To investigate the apatite forming ability of pure titanium implant after micro-arc oxidation treatment in simulated body fluid (SBF) and obtain implants with calcium phosphate (Ca-P) layers. The implants were immersed in (SBF) after micro-arc oxidation treatment for different time lengths, and their apatite forming ability and the morphology and constituents of the Ca-P layers formed on the sample surface were analyzed using X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy, and energy dispersive electron probe. After immersion in SBF, large quantities of Ca-P layers were induced on the surface of the samples. The Ca-P layers were composed of octacalcium phosphate and carbonated hydroxyapatite, and the crystals showed a plate-like morphology with an oriented growth. The implants with micro-arc oxidation treatment show good apatite forming ability on the surface with rich calcium and phosphorus elements. The formed layers are composed of bone-like apatite including octacalcium phosphate and carbonated hydroxyapatite.

  4. Clean forming of stainless steel and titanium products by lubricious oxides

    DEFF Research Database (Denmark)

    Heikkilä, Irma; Wadman, Boel; Thoors, Håkan

    2012-01-01

    to industrial forming processes. Preliminary evaluations show a beneficial influence of two oxides types, on stainless steel and on titanium. More work is needed to test the lubricating effect in other forming operations and to analyse the sustainability aspects for products manufactured with this alternative......Big social benefits can be attained through increased use of stainless steel or titanium in new sheet metal applications. Unfortunately, forming of these materials is often a challenging and costly operation, that can lead to environmental and health problems when solving the technical limitations...

  5. 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

  6. Oxidation resistant chromium coating on Zircaloy-4 for accident tolerant fuel cladding

    International Nuclear Information System (INIS)

    Park, Jung-Hwan; Kim, Eui-Jung; Jung, Yang-Il; Park, Dong-Jun; Kim, Hyun-Gil; Park, Jeong-Yong; Koo, Yang-Hyun

    2015-01-01

    The attributes of such a fuel are approved reaction kinetics with steam, a slower hydrogen generation rate, and good cladding thermo-mechanical properties. Many researchers have tried to modify zirconium alloys to improve their oxidation resistance in the early stages of the ATF development. Corrosion resistant coating on cladding is one of the candidate technologies to improve the oxidation resistance of zirconium cladding. By applying coating technology to zirconium cladding, it is easy to obtain corrosion resistance without a change in the base materials. Among the surface coating methods, arc ion plating (AIP) is a coating technology to improve the adhesion owing to good throwing power, and a dense deposit (Fig. 1). Owing to these advantages, AIP has been widely used to efficiently form protective coatings on cutting tools, dies, bearings, etc. In this study, The AIP technique for the protection of zirconium claddings from the oxidation in a high-temperature steam environment was studied. The homogeneous Cr film with a high adhesive ability to the cladding was deposited by AIP and acted as a protection layer to enhance the corrosion resistance of the zirconium cladding. It was concluded that the AIP technology is effective for coating a protective layer on claddings

  7. Oxidation resistant chromium coating on Zircaloy-4 for accident tolerant fuel cladding

    Energy Technology Data Exchange (ETDEWEB)

    Park, Jung-Hwan; Kim, Eui-Jung; Jung, Yang-Il; Park, Dong-Jun; Kim, Hyun-Gil; Park, Jeong-Yong; Koo, Yang-Hyun [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2015-05-15

    The attributes of such a fuel are approved reaction kinetics with steam, a slower hydrogen generation rate, and good cladding thermo-mechanical properties. Many researchers have tried to modify zirconium alloys to improve their oxidation resistance in the early stages of the ATF development. Corrosion resistant coating on cladding is one of the candidate technologies to improve the oxidation resistance of zirconium cladding. By applying coating technology to zirconium cladding, it is easy to obtain corrosion resistance without a change in the base materials. Among the surface coating methods, arc ion plating (AIP) is a coating technology to improve the adhesion owing to good throwing power, and a dense deposit (Fig. 1). Owing to these advantages, AIP has been widely used to efficiently form protective coatings on cutting tools, dies, bearings, etc. In this study, The AIP technique for the protection of zirconium claddings from the oxidation in a high-temperature steam environment was studied. The homogeneous Cr film with a high adhesive ability to the cladding was deposited by AIP and acted as a protection layer to enhance the corrosion resistance of the zirconium cladding. It was concluded that the AIP technology is effective for coating a protective layer on claddings.

  8. Biochemical characterization of the purple form of Marinobacter hydrocarbonoclasticus nitrous oxide reductase

    Science.gov (United States)

    Dell'Acqua, Simone; Pauleta, Sofia R.; Moura, José J. G.; Moura, Isabel

    2012-01-01

    Nitrous oxide reductase (N2OR) catalyses the final step of the denitrification pathway—the reduction of nitrous oxide to nitrogen. The catalytic centre (CuZ) is a unique tetranuclear copper centre bridged by inorganic sulphur in a tetrahedron arrangement that can have different oxidation states. Previously, Marinobacter hydrocarbonoclasticus N2OR was isolated with the CuZ centre as CuZ*, in the [1Cu2+ : 3Cu+] redox state, which is redox inert and requires prolonged incubation under reductive conditions to be activated. In this work, we report, for the first time, the isolation of N2OR from M. hydrocarbonoclasticus in the ‘purple’ form, in which the CuZ centre is in the oxidized [2Cu2+ : 2Cu+] redox state and is redox active. This form of the enzyme was isolated in the presence of oxygen from a microaerobic culture in the presence of nitrate and also from a strictly anaerobic culture. The purple form of the enzyme was biochemically characterized and was shown to be a redox active species, although it is still catalytically non-competent, as its specific activity is lower than that of the activated fully reduced enzyme and comparable with that of the enzyme with the CuZ centre in either the [1Cu2+ : 3Cu+] redox state or in the redox inactive CuZ* state. PMID:22451106

  9. Oxidized epigallocatechin gallate inhibited lysozyme fibrillation more strongly than the native form

    Directory of Open Access Journals (Sweden)

    Ting-Ting An

    2017-04-01

    Full Text Available Epigallocatechin gallate (EGCG, the most abundant flavanoid in green tea, is currently being evaluated in the clinic due to its benefits in the treatment of amyloid disorders. Its anti-amyloidogenic effect has been attributed to direct interaction of the intact molecule with misfolded polypeptides. In addition, antioxidant activity is also involved in the anti-amyloidogenic role. The detailed molecular mechanism is still unclear and requires further investigation. In the present study, the kinetics of EGCG oxidation and the anti-amyloidogenic effect of the resultant oxidation substances have been examined. The results indicate that EGCG degrades in a medium at pH 8.0 with a half-life less than 2 h. By utilizing lysozyme as an in vitro model, the oxidized EGCG demonstrates a more potent anti-amyloidogenic capacity than the intact molecule, as shown by ThT and ANS fluorescence, TEM determination, and hemolytic assay. The oxidized EGCG also has a stronger disruptive effect on preformed fibrils than the native form. Ascorbic acid eliminates the disruptive role of native EGCG on the fibrils, suggesting that oxidation is a prerequisite in fibril disruption. The results of this work demonstrate that oxidized EGCG plays a more important role than the intact molecule in anti-amyloidogenic activity. These insights into the action of EGCG may provide a novel route to understand the anti-amyloidogenic activity of natural polyphenols.

  10. Characterization of oxide films formed on steels in a BWR environment

    International Nuclear Information System (INIS)

    Honda, Takashi; Ohashi, Kenya; Kashimura, Eiji; Furutani, Yasumasa

    1988-01-01

    Environmental effects on corrosion bahaviors and properties of oxide films were evaluated for austenitic stainless and carbon steels in high-temperature water simulating a Boiling Water Reactor condition. The existence ratios of Cr and OH - in oxide films formed on stainless steel decreased and those of Fe, Ni and O 2- increased with increases of temperature and dissolved oxygen concentration. Changes of pH in the test region did not affect the composition of these species. These results indicated that Cr tended to combine with OH - , i.e., Cr existed as hydroxides or oxyhydroxides. Further, Fe and Ni tended to form spinel type oxides, which were indentified by XRD. In addition, the corrosion resistance of stainless steel was higher than that of carbon steel in all environments. The protectivity of magnetite films on carbon steel increased with temperature, dissolved oxygen concentration and pH. However, Ni ferrite, formed on stainless steel, further improved the corrosion resistance under such conditions. On the other hand, as the solubility of magnetite increased with decreases in the above mentioned factors, the corrosion resistance of carbon steel decreased. But, even under such conditions Cr, contained in stainless steel, tended to form stable films and suppressed corrosion. (author)

  11. Characterization of coatings formed on AZX magnesium alloys by plasma electrolytic oxidation

    Science.gov (United States)

    Anawati, Anawati; Gumelar, Muhammad Dikdik

    2018-05-01

    Plasma Electrolytic Oxidation (PEO) is an electrochemical anodization process which involves the application of a high voltage to create intense plasma on a metal surface to form a ceramic type of oxide. The resulted coating exhibits high wear resistance and good corrosion barrier which are suitable to enhance the performance of biodegradable Mg alloys. In this work, the role of alloying element Ca in modifying the characteristics of PEO layer formed on AZ61 series magnesium alloys was investigated. PEO treatment was conducted on AZ61, AZX611, and AZX612 alloys in 0.5 M Na3PO4 solution at a constant current of 200 A/m2 at 25°C for 8 min. The resulted coatings were characterized by field emission-scanning electron microscope (FESEM), X-ray diffraction spectroscopy (XRD), and X-ray fluorescence spectroscopy (XRF), as well as hardness test. The presence of alloying element Ca in the AZ61 alloys accelerated the PEO coatings formation without altering the coating properties significantly. The coating formed on AZX specimen was slightly thicker ( 14-17 µm) than that of formed onthe AZ specimens ( 13 µm). Longer exposure time to plasma discharge was the reason for faster thickening of the coating layer on AZX specimen. XRD detected a similar crystalline oxide phase of Mg3(PO4)2 in the oxide formed on all of the specimens. Zn was highly incorporated in the coatings with a concentration in the range 24-30 wt%, as analyzed by XRF. Zn compound might exist in amorphous phases. The microhardness test on the coatings revealed similar average hardness 124 HVon all of the specimens.

  12. Structural features of anodic oxide films formed on aluminum substrate coated with self-assembled microspheres

    International Nuclear Information System (INIS)

    Asoh, Hidetaka; Uchibori, Kota; Ono, Sachiko

    2009-01-01

    The structural features of anodic oxide films formed on an aluminum substrate coated with self-assembled microspheres were investigated by scanning electron microscopy and atomic force microscopy. In the first anodization in neutral solution, the growth of a barrier-type film was partially suppressed in the contact area between the spheres and the underlying aluminum substrate, resulting in the formation of ordered dimple arrays in an anodic oxide film. After the subsequent second anodization in acid solution at a voltage lower than that of the first anodization, nanopores were generated only within each dimple. The nanoporous region could be removed selectively by post-chemical etching using the difference in structural dimensions between the porous region and the surrounding barrier region. The mechanism of anodic oxide growth on the aluminum substrate coated with microspheres through multistep anodization is discussed.

  13. Structural features of anodic oxide films formed on aluminum substrate coated with self-assembled microspheres

    Energy Technology Data Exchange (ETDEWEB)

    Asoh, Hidetaka [Department of Applied Chemistry, Faculty of Engineering, Kogakuin University, 2665-1 Nakano, Hachioji, Tokyo 192-0015 (Japan)], E-mail: asoh@cc.kogakuin.ac.jp; Uchibori, Kota; Ono, Sachiko [Department of Applied Chemistry, Faculty of Engineering, Kogakuin University, 2665-1 Nakano, Hachioji, Tokyo 192-0015 (Japan)

    2009-07-15

    The structural features of anodic oxide films formed on an aluminum substrate coated with self-assembled microspheres were investigated by scanning electron microscopy and atomic force microscopy. In the first anodization in neutral solution, the growth of a barrier-type film was partially suppressed in the contact area between the spheres and the underlying aluminum substrate, resulting in the formation of ordered dimple arrays in an anodic oxide film. After the subsequent second anodization in acid solution at a voltage lower than that of the first anodization, nanopores were generated only within each dimple. The nanoporous region could be removed selectively by post-chemical etching using the difference in structural dimensions between the porous region and the surrounding barrier region. The mechanism of anodic oxide growth on the aluminum substrate coated with microspheres through multistep anodization is discussed.

  14. Oxidative Stability of Marine Phospholipids in the Liposomal Form and Their Applications

    DEFF Research Database (Denmark)

    Lu, Henna Fung Sieng; Nielsen, Nina Skall; Timm-Heinrich, M.

    2011-01-01

    Marine phospholipids (MPL) have attracted a great deal of attention recently as they are considered to have a better bioavailability, a better resistance towards oxidation and a higher content of eicosapentaenoic (EPA) and docosahexaenoic acids (DHA) than oily triglycerides (fish oil) from the same...... source. Due to their tight intermolecular packing conformation at the sn-2 position and their synergism with α-tocopherol present in MPL extracts, they can form stable liposomes which are attractive ingredients for food or feed applications. However, MPL are still susceptible to oxidation as they contain...... large amounts polyunsaturated fatty acids and application of MPL in food and aquaculture industries is therefore a great challenge for researchers. Hence, knowledge on the oxidative stability of MPL and the behavior of MPL in food and feed systems is an important issue. For this reason, this review...

  15. XPS characterization of the anodic oxide film formed on uranium metal in sodium hydroxide solution

    International Nuclear Information System (INIS)

    Fu Xiaoguo; Wang Xiaolin; Guo Huanjun; Wang Qingfu; Zhao Zhengping; Zhong Yongqiang

    2002-01-01

    X-ray photoelectron spectroscopy (XPS) is used to examine the anodic oxide film formed on uranium metal in 0.8 mol/L NaOH solution. The U4f 7/2 fitting spectra suggests that the anodic oxide film is composed of uranium trioxide and a small amount of UO 2+x . Under UHV condition, the U4f peak shifts to the lower binding energy, while a gradual increase in the intensity of U5f peak and the broad of U4f peak are also observed. All of these changes are due to reduction of uranium trioxide in the anodic oxide film. XPS quantitative analysis confirms the occurrence of reduction reaction

  16. 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.

  17. Induced nano-scale self-formed metal-oxide interlayer in amorphous silicon tin oxide thin film transistors.

    Science.gov (United States)

    Liu, Xianzhe; Xu, Hua; Ning, Honglong; Lu, Kuankuan; Zhang, Hongke; Zhang, Xiaochen; Yao, Rihui; Fang, Zhiqiang; Lu, Xubing; Peng, Junbiao

    2018-03-07

    Amorphous Silicon-Tin-Oxide thin film transistors (a-STO TFTs) with Mo source/drain electrodes were fabricated. The introduction of a ~8 nm MoO x interlayer between Mo electrodes and a-STO improved the electron injection in a-STO TFT. Mo adjacent to the a-STO semiconductor mainly gets oxygen atoms from the oxygen-rich surface of a-STO film to form MoO x interlayer. The self-formed MoO x interlayer acting as an efficient interface modification layer could conduce to the stepwise internal transport barrier formation while blocking Mo atoms diffuse into a-STO layer, which would contribute to the formation of ohmic contact between Mo and a-STO film. It can effectively improve device performance, reduce cost and save energy for the realization of large-area display with high resolution in future.

  18. Chemical structure of the adducts formed by the oxidation of benzidine in the presence of phenols

    International Nuclear Information System (INIS)

    Josephy, P.D.; Mason, R.P.; Eling, T.

    1982-01-01

    Bioactivation of carcinogens by peroxidases has received increasing attention since the discovery of the oxidation of carcinogens by prostaglandin hydroperoxidase. Benzidine and 3,5,3',5'-tetramethylbenzidine are oxidized by horseradish peroxidase and prostaglandin synthase to two-electron oxidation products (di-imines). Di-imines readily react with the phenolic anti-oxidant butylated hydroxyanisole to form adducts. In this paper, we have studied the oxidation of benzidine by horseradish peroxidase in the presence of phenolic compounds and characterized the resultant benzidine/phenol adducts. A benzidine/2,6-dimethylphenol adduct was isolated and characterized by mass spectrometry and high field n.m.r. The reaction of [ 14 C]benzidine in the presence of horseradish peroxidase and phenol yielded only the benzidine/phenol adduct. Our results indicate that the benzidine/phenol adducts are analogous to the indoaniline dyes, differing only in substitution of a biphenyl group for a benzene ring. The reaction of benzidine di-imine with endogenous phenols may represent a new pathway for detoxication, removing potentially harmful metabolites of benzidine

  19. The oxidized form of vitamin C, dehydroascorbic acid, regulates neuronal energy metabolism.

    Science.gov (United States)

    Cisternas, Pedro; Silva-Alvarez, Carmen; Martínez, Fernando; Fernandez, Emilio; Ferrada, Luciano; Oyarce, Karina; Salazar, Katterine; Bolaños, Juan P; Nualart, Francisco

    2014-05-01

    Vitamin C is an essential factor for neuronal function and survival, existing in two redox states, ascorbic acid (AA), and its oxidized form, dehydroascorbic acid (DHA). Here, we show uptake of both AA and DHA by primary cultures of rat brain cortical neurons. Moreover, we show that most intracellular AA was rapidly oxidized to DHA. Intracellular DHA induced a rapid and dramatic decrease in reduced glutathione that was immediately followed by a spontaneous recovery. This transient decrease in glutathione oxidation was preceded by an increase in the rate of glucose oxidation through the pentose phosphate pathway (PPP), and a concomitant decrease in glucose oxidation through glycolysis. DHA stimulated the activity of glucose-6-phosphate dehydrogenase, the rate-limiting enzyme of the PPP. Furthermore, we found that DHA stimulated the rate of lactate uptake by neurons in a time- and dose-dependent manner. Thus, DHA is a novel modulator of neuronal energy metabolism by facilitating the utilization of glucose through the PPP for antioxidant purposes. © 2014 International Society for Neurochemistry.

  20. Transmission electron microscopy of coatings formed by plasma electrolytic oxidation of titanium.

    Science.gov (United States)

    Matykina, E; Arrabal, R; Skeldon, P; Thompson, G E

    2009-05-01

    Transmission electron microscopy and supporting film analyses are used to investigate the changes in composition, morphology and structure of coatings formed on titanium during DC plasma electrolytic oxidation in a calcium- and phosphorus-containing electrolyte. The coatings are of potential interest as bioactive surfaces. The initial barrier film, of mixed amorphous and nanocrystalline structure, formed below the sparking voltage of 180 V, incorporates small amounts of phosphorus and calcium species, with phosphorus confined to the outer approximately 63% of the coating thickness. On commencement of sparking, calcium- and phosphorus-rich amorphous material forms at the coating surface, with local heating promoting crystallization in underlying and adjacent anodic titania. The amorphous material thickens with increased treatment time, comprising almost the whole of the approximately 5.7-microm-thick coating formed at 340 V. At this stage, the coating is approximately 4.4 times thicker than the oxidized titanium, with a near-surface composition of about 12 at.% Ti, 58 at.% O, 19 at.% P and 11 at.% Ca. Further, the amount of titanium consumed in forming the coating is similar to that calculated from the anodizing charge, although there may be non-Faradaic contributions to the coating growth.

  1. Collaborative study of the colorimetric determination of zirconium in antiperspirant aerosols

    International Nuclear Information System (INIS)

    Beavin, P. Jr.

    1977-01-01

    A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also added to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average percent recoveries and standard deviations for spiked samples were 99.8-100.2 and 1.69-2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8-97.4 and 3.09-4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average perent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action

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

    Energy Technology Data Exchange (ETDEWEB)

    Davila N, M. L.

    2015-07-01

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

  3. Chemistry, spectroscopy and isotope separation of zirconium and its compounds as revealed by laser diagnostics of laser produced metal beams

    International Nuclear Information System (INIS)

    Hackett, P.A.; Humphries, M.; Rayner, D.M.; Bourne, O.L.; Mitchell, A.

    1986-01-01

    Recent work from the author's laboratory on zirconium beams is reviewed. Zirconium metal beams have been produced by laser vaporization of solid zirconium targets coupled with supersonic expansion of helium gas. The resultant supersonic metal beam is shown to present an ideal environment for various spectroscopic techniques. The state distribution of zirconium atoms in the beam is obtained from low resolution laser induced fluorescence (LIF) studies. High resolution LIF studies give information on the hyperfine splitting in the ground state of the zirconium-91 isotope. Information on the hyperfine splitting in the excited state is obtained from quantum beat spectroscopy. Low resolution 2 color multiphoton ionization spectroscopy using a XeCl laser allows isotope separation of all isotopes of zirconium. These metal beams are highly reactive and can be used to produce novel chemical species. The results of two studies in which a reactant is added to the expansion gas are reported here. Zirconium oxide (ZrO), a molecule observed in the emission spectra of cool stars and in laboratory studies at high temperatures, is produced in a low temperature, collision free environment by adding small quantities of oxygen to the expansion gas. Zirconium fluoride (ZrF), a molecule previously unobserved, is produced by the addition of small quantities of CF/sub 4/

  4. Influence of oxazolidines and zirconium oxalate crosslinkers on the hydrothermal, enzymatic, and thermo mechanical stability of type 1 collagen fiber

    International Nuclear Information System (INIS)

    Haroun, Mahdi A.; Khirstova, Palmina K.; Gasmelseed, Gurashi A.; Covington, Antony D.

    2009-01-01

    Stabilization of type I rat tail tendon (RTT) collagen by crosslink agent oxazolidine and zirconium oxalate was studied to understand the effect on the thermal, enzymatic and mechanical stability of collagen. The results show that both oxazolidine and zirconium oxalate imparts thermal stability to collagen, and oxazolidine exhibits a marked increase in the peak temperature and enthalpy changes when compared to both native and zirconium oxalate tanned RTT. There is a decrease in the peak temperature and the enthalpy changes of oxazolidine tanned RTT fibers after treatment with urea, suggesting the possibility of alterations in the secondary structure of collagen after tanning. Oxazolidine, which forms carbocationic intermediates species in solution, have better crosslinking with collagen as seen from viscometry studies and hence provides better enzymatic stability to collagen than zirconium, which largely forms monomeric species in solution. Zirconium does not seem to change the tensile strength of RTT fibers significantly in wet condition as well as oxazolidine

  5. Influence of oxazolidines and zirconium oxalate crosslinkers on the hydrothermal, enzymatic, and thermo mechanical stability of type 1 collagen fiber

    Energy Technology Data Exchange (ETDEWEB)

    Haroun, Mahdi A. [Department of Chemical and Environmental Engineering, Faculty of Engineering, Universiti Putra Malaysia, 43400 UPM, Serdang (Malaysia)], E-mail: Mahdiupm@hotmail.com; Khirstova, Palmina K. [People' s Hall 11113, P.O. Box 6272, Khartoum (Sudan); Gasmelseed, Gurashi A. [Juba University, Leather Dept. P.O. Box 12327 Khartoum (Sudan); Covington, Antony D. [Leather Centre, University College Northampton, Northampton (United Kingdom)

    2009-02-20

    Stabilization of type I rat tail tendon (RTT) collagen by crosslink agent oxazolidine and zirconium oxalate was studied to understand the effect on the thermal, enzymatic and mechanical stability of collagen. The results show that both oxazolidine and zirconium oxalate imparts thermal stability to collagen, and oxazolidine exhibits a marked increase in the peak temperature and enthalpy changes when compared to both native and zirconium oxalate tanned RTT. There is a decrease in the peak temperature and the enthalpy changes of oxazolidine tanned RTT fibers after treatment with urea, suggesting the possibility of alterations in the secondary structure of collagen after tanning. Oxazolidine, which forms carbocationic intermediates species in solution, have better crosslinking with collagen as seen from viscometry studies and hence provides better enzymatic stability to collagen than zirconium, which largely forms monomeric species in solution. Zirconium does not seem to change the tensile strength of RTT fibers significantly in wet condition as well as oxazolidine.

  6. Interaction of titanium and zirconium hydroxides with aqueous solutions of lead(2) salts

    International Nuclear Information System (INIS)

    Savenko, V.G.; Sakharov, V.V.; Nurgalieva, A.A.; Petrov, K.I.

    1980-01-01

    The mixed phases, characterized by the Pb : Zr 4 ratio are synthesized during the process of geterophase interaction of zirconium hydroxide with solutions of lead nitrate and acetate. The process of the mixed phases thermolysis on the base of amorphous zirconium hydroxides is investigated by the methods of DTA, X-ray phase analysis and IR spectroscopy. The metastable phases are formed during the thermolysis process

  7. Moessbauer spectrometry study and metallography of paramagnetic phases from zirconium-iron system

    International Nuclear Information System (INIS)

    Freitas Brandao Bittencourt, C. de.

    1976-01-01

    Binary alloys of zirconium with 3 to 23% of iron by weight, were made by diffusion at 875 0 C of iron onto thin plates of zirconium. Moessbauer spectroscopy and optic metallography indicated the phases Zr 2 Fe and Zr 4 Fe, the bulk of which probably formed during the diffusion. These phases were confirmed by electron probe microanalysis. Moessbauer spectra showed quadrupole doublets with the same hyperfine interaction parameters in both phases, but with clearly distinct asymmetries. (author)

  8. 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.

  9. Growth behavior of anodic oxide formed by aluminum anodizing in glutaric and its derivative acid electrolytes

    Science.gov (United States)

    Nakajima, Daiki; Kikuchi, Tatsuya; Natsui, Shungo; Suzuki, Ryosuke O.

    2014-12-01

    The growth behavior of anodic oxide films formed via anodizing in glutaric and its derivative acid solutions was investigated based on the acid dissociation constants of electrolytes. High-purity aluminum foils were anodized in glutaric, ketoglutaric, and acetonedicarboxylic acid solutions under various electrochemical conditions. A thin barrier anodic oxide film grew uniformly on the aluminum substrate by glutaric acid anodizing, and further anodizing caused the film to breakdown due to a high electric field. In contrast, an anodic porous alumina film with a submicrometer-scale cell diameter was successfully formed by ketoglutaric acid anodizing at 293 K. However, the increase and decrease in the temperature of the ketoglutaric acid resulted in non-uniform oxide growth and localized pitting corrosion of the aluminum substrate. An anodic porous alumina film could also be fabricated by acetonedicarboxylic acid anodizing due to the relatively low dissociation constants associated with the acid. Acid dissociation constants are an important factor for the fabrication of anodic porous alumina films.

  10. Wet oxidative degradation of cellulosic wastes 5- chemical and thermal properties of the final waste forms

    International Nuclear Information System (INIS)

    Eskander, S.B.; Saleh, H.M.

    2002-01-01

    In this study, the residual solution arising from the wet oxidative degradation of solid organic cellulosic materials, as one of the component of radioactive solid wastes, using hydrogen peroxide as oxidant. Were incorporated into ordinary Portland cement matrix. Leaching as well as thermal characterizations of the final solidified waste forms were evaluated to meet the final disposal requirements. Factors, such as the amount of the residual solution incorporated, types of leachant. Release of different radionuclides and freezing-thaw treatment, that may affect the leaching characterization. Were studied systematically from the data obtained, it was found that the final solid waste from containing 35% residual solution in tap water is higher than that in ground water or sea water. Based on the data obtained from thermal analysis, it could be concluded that incorporating the residual solution form the wet oxidative degradation of cellulosic materials has no negative effect on the hydration of cement materials and consequently on the thermal stability of the final solid waste from during the disposal process

  11. 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)