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)

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

Atomic profile imaging of ceramic oxide surfaces

International Nuclear Information System (INIS)

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

1989-01-01

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

Manufacturing of porous oxide ceramics by replication of plant morphologies

Energy Technology Data Exchange (ETDEWEB)

Sieber, H.; Rambo, C.; Cao, J.; Vogli, E.; Greil, P. [Erlangen-Nuernberg Univ., Erlangen (DE). Dept. of Materials Science (III) Glass and Ceramics

2002-07-01

Biomorphic oxide ceramics of alumina, mullite and zirconia with a directed pore morphology on the micrometer level were manufactured from bioorganic plant structures by sol-gel processing as well as sol-assisted nano-powder infiltrations. The inherent open porous morphology of natural grown rattan palms was used for vacuum-infiltration with aluminum isopropoxide (Al(OC{sub 3}H{sub 7}){sub 3}), zirconium oxichloride (ZrOCl{sub 2}.8H{sub 2}O) and SiO{sub 2} nano powder. Hydrolysis of the sols by adding HNO{sub 3} and pyrolysis in inert atmosphere at 800 C resulted in the formation of biocarbon/ceramic replica of the original wood morphology. The specimens were sintered in air at temperatures up to 1600 C to yield porous oxide ceramics with an unidirected pore structure similar to the original plant material. Repeated infiltration, hydrolysis and annealing steps were applied to increase the density of the ceramic materials. (orig.)

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

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

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

Science.gov (United States)

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

2009-01-01

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

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

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

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.

Oxide ceramics

International Nuclear Information System (INIS)

Ryshkewitch, E.; Richerson, D.W.

1985-01-01

The book explores single-phase ceramic oxide systems from the standpoint of physical chemistry and technology. This second edition also focuses on advances in technology since publication of the original edition. These include improvements in raw materials and forming and sintering techniques, and the major role that oxide ceramics have had in development of advanced products and processes. The text is divided into five major sections: general fundamentals of oxide ceramics, advances in aluminum oxide technology, advances in zirconia technology, and advances in beryllium oxide technology

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

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.

Production of ceramic formed parts by means of plasma spraying

International Nuclear Information System (INIS)

Kirner, K.

1989-01-01

Open and closed pipes and tubes, nozzles and crucibles, conical parts and other molded articles of ceramic materials such as aluminium oxide, magnesium-aluminium spinel, zirconium oxide, zirconium silicate and special ceramics can be fabricated by spray application to a core which is afterwards removed. Because at the same time these are mainly high temperature materials and high temperature application areas, plasma spraying is preferred. The process and examples of application are described, the advantages and disadvantages are pointed out. (orig.) [de

Optical properties of ytterbium-doped yttrium oxide ceramics

Energy Technology Data Exchange (ETDEWEB)

Solomonov, V.I.; Maksimov, R.N. [Institute of Electrophysics UrB RAS, Amundsena 106, 620016 Ekaterinburg (Russian Federation); Ural Federal University Named After the First President of Russia B.N. Yeltsin, Mira 19, 620002 Ekaterinburg (Russian Federation); Osipov, V.V.; Shitov, V.A.; Lipchak, A.I. [Institute of Electrophysics UrB RAS, Amundsena 106, 620016 Ekaterinburg (Russian Federation)

2017-05-15

Ytterbium-doped yttrium oxide (Yb:Y{sub 2}O{sub 3}) transparent ceramics with different sintering additives (Lu{sub 2}O{sub 3}, Sc{sub 2}O{sub 3}, CeO{sub 2}, ZrO{sub 2}, or HfO{sub 2}) were fabricated using nanopowders produced by laser ablation. Transmission and photoluminescence spectra of the obtained ceramics were investigated at room temperature. Highest in-line transmittance was over 80% at the wavelength of 1060 nm for 2 mm thick Yb:Y{sub 2}O{sub 3} ceramics with zirconium and hafnium. Divalent Yb ions with the ground state electron configuration 4f{sup 13}6s were revealed. The absorption and emission bands caused by s <-> s transitions of these ions were observed in the IR spectral range of Yb{sup 3+} ions. The superposition of both Yb{sup 3+} and Yb{sup 2+} emission bands leads to an effective broadening of the whole luminescence band. (copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

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

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.

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

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

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

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)

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.

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.

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.

Fundamental studies of ceramic/metal interfacial reactions at elevated temperatures.

Energy Technology Data Exchange (ETDEWEB)

McDeavitt, S. M.; Billings, G. W.; Indacochea, J. E.

2000-12-14

This work characterizes the interfaces resulting from exposing oxide and non-oxide ceramic substrates to zirconium metal and stainless steel-zirconium containing alloys. The ceramic/metal systems together were preheated at about 600 C and then the temperatures were increased to the test maximum temperature, which exceeded 1800 C, in an atmosphere of high purity argon. Metal samples were placed onto ceramic substrates, and the system was heated to elevated temperatures past the melting point of the metallic specimen. After a short stay at the peak temperature, the system was cooled to room temperature and examined. The chemical changes across the interface and other microstructural developments were analyzed with energy dispersive spectroscopy (EDS). This paper reports on the condition of the interfaces in the different systems studied and describes possible mechanisms influencing the microstructure.

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

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.

Dispersion toughened silicon carbon ceramics

Science.gov (United States)

Wei, G.C.

1984-01-01

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

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.

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.

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.

Thermodynamic analysis of thermal plasma process of composite zirconium carbide and silicon carbide production from zircon concentrates

International Nuclear Information System (INIS)

Kostic, Z.G.; Stefanovic, P.Lj.; Pavlovic; Pavlovic, Z.N.; Zivkovic, N.V.

2000-01-01

Improved zirconium ceramics and composites have been invented in an effort to obtain better resistance to ablation at high temperature. These ceramics are suitable for use as thermal protection materials on the exterior surfaces of spacecraft, and in laboratory and industrial environments that include flows of hot oxidizing gases. Results of thermodynamic consideration of the process for composite zirconium carbide and silicon carbide ultrafine powder production from ZrSiO 4 in argon thermal plasma and propane-butane gas as reactive quenching reagents are presented in the paper. (author)

High temperature strengthening of zirconium-toughened ceramics

International Nuclear Information System (INIS)

Claussen, N.

1986-01-01

Transformation-toughened (i.e. ZrO/sub 2/-toughened) ceramics represent a new class of high performance ceramics with spectacular strength properties at low and intermediate temperatures. However, at temperatures above about 700 0 C, most of these tough oxide-base ceramics can no longer be used as load-bearing engineering parts because of characteristic deficiencies. The aim of the present paper is to provide and discuss microstructural design strategies which may enable ZrO/sub 2/-toughened ceramics to be applied at higher temperatures. From the various strategies suggested, three appear to show good prospects, namely (a) the prevention of glassy intergranular films, (b) the addition of hard high modulus particles and (c) whikser or fibre reinforcement. Experimental approaches are presented from some ZrO/sub 2/-toughened ceramics, elg. tetragonal ZrO/sub 2/ polycrystals and ZrO/sub 2/-toughened cordierite, spinel and mullite

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)

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

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

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.

Transmission of Er:YAG laser through different dental ceramics.

Science.gov (United States)

Sari, Tugrul; Tuncel, Ilkin; Usumez, Aslihan; Gutknecht, Norbert

2014-01-01

The aim of this study was to determine the erbium-doped yttrium aluminum garnet (Er:YAG) laser transmission ratio through different dental ceramics with different thicknesses. Laser debonding procedure of adhesively luted all-ceramic restorations is based on the transmission of laser energy through the ceramic and the ablation of resin cement, because of the transmitted laser energy. Five different dental ceramics were evaluated in this study: sintered zirconium-oxide core ceramic, monolithic zirconium-oxide ceramic, feldspathic ceramic, leucite-reinforced glass ceramic, and lithium disilicate-reinforced glass ceramic. Two ceramic discs with different thicknesses (0.5 and 1 mm) were fabricated for each group. Ceramic discs were placed between the sensor membrane of the laser power meter and the tip of the contact handpiece of an Er:YAG laser device with the aid of a custom- made acrylic holder. The transmission ratio of Er:YAG laser energy (500 mJ, 2 Hz, 1 W, 1000 μs) through different ceramic discs was measured with the power meter. Ten measurements were made for each group and the results were analyzed with two way analysis of variance (ANOVA) and Tukey honestly significant difference (HSD) tests. The highest transmission ratio was determined for lithium disilicate-reinforced ceramic with 0.5 mm thickness (88%) and the lowest was determined for feldspathic ceramic with 1 mm thickness (44%). The differences among the different ceramics and between the different thicknesses were significant (pCeramic type and thickness should be taken into consideration to adjust the laser irradiation parameters during laser debonding of adhesively luted all-ceramic restorations.

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...

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

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

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.

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

Dense high temperature ceramic oxide superconductors

Science.gov (United States)

Landingham, Richard L.

1993-01-01

Dense superconducting ceramic oxide articles of manufacture and methods for producing these articles are described. Generally these articles are produced by first processing these superconducting oxides by ceramic processing techniques to optimize materials properties, followed by reestablishing the superconducting state in a desired portion of the ceramic oxide composite.

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

Shear Bond Strength of Orthodontic Brackets Bonded to Zirconium Crowns.

Science.gov (United States)

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

2017-06-01

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

MAX Phase Modified SiC Composites for Ceramic-Metal Hybrid Cladding Tubes

International Nuclear Information System (INIS)

Jung, Yang-Il; Kim, Sun-Han; Park, Dong-Jun; Park, Jeong-Hwan; Park, Jeong-Yong; Kim, Hyun-Gil; Koo, Yang-Hyun

2015-01-01

A metal-ceramic hybrid cladding consists of an inner zirconium tube, and an outer SiC fiber-matrix SiC ceramic composite with surface coating as shown in Fig. 1 (left-hand side). The inner zirconium allows the matrix to remain fully sealed even if the ceramic matrix cracks through. The outer SiC composite can increase the safety margin by taking the merits of the SiC itself. In addition, the outermost layer prevents the dissolution of SiC during normal operation. On the other hand, a ceramic-metal hybrid cladding consists of an outer zirconium tube, and an inner SiC ceramic composite as shown in Fig. 1 (right-hand side). The outer zirconium protects the fuel rod from a corrosion during reactor operation, as in the present fuel claddings. The inner SiC composite, additionally, is designed to resist the severe oxidation under a postulated accident condition of a high-temperature steam environment. Reaction-bonded SiC was fabricated by modifying the matrix as the MAX phase. The formation of Ti 3 SiC 2 was investigated depending on the compositions of the preform and melt. In most cases, TiSi 2 was the preferential phase because of its lowest melting point in the Ti-Si-C system. The evidence of Ti 3 SiC 2 was the connection with the pressurizing

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.

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.

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.

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

Niobia and tantala codoped orthorhombic zirconia ceramics

International Nuclear Information System (INIS)

Hoeftberger, M.; Gritzner, G.

1995-01-01

During recent studies it was found that codoping of zirconia with niobia and tantala yielded very corrosion resistant, orthorhombic zirconia ceramics. The powders for those novel ceramics were made via the sol-gel technique by hydrolysis of the respective metal propoxides; a method which required dry-box techniques during the preparation of the alkoxides. In these studies the authors investigated the fabrication of precursor material from aqueous solutions. The preparation of aqueous solutions of salts of zirconium, niobium and tantalum is hampered by rapid hydrolysis. Premature hydrolysis of the chlorides and oxichlorides of niobium, tantalum and zirconium can be, however, prevented in aqueous solutions of oxalic acid. Thus the authors investigated the coprecipitation of hydroxides as precursors by reacting oxalic acid solutions of the respective cations with aqueous ammonia. In addition they studied the effects of calcination and of hydrothermal conversion of the hydroxides to oxides on the powder characteristics and on the mechanical properties of the niobia and tantala codoped zirconia ceramics

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)

Tough hybrid ceramic-based material with high strength

International Nuclear Information System (INIS)

Guo, Shuqi; Kagawa, Yutaka; Nishimura, Toshiyuki

2012-01-01

This study describes a tough and strong hybrid ceramic material consisting of platelet-like zirconium compounds and metal. A mixture of boron carbide and excess zirconium powder was heated to 1900 °C using a liquid-phase reaction sintering technique to produce a platelet-like ZrB 2 -based hybrid ceramic bonded by a thin zirconium layer. The platelet-like ZrB 2 grains were randomly present in the as-sintered hybrid ceramic. Relative to non-hybrid ceramics, the fracture toughness and flexural strength of the hybrid ceramic increased by approximately 2-fold.

Use of the azeotropic distillation technique in the synthesis of zirconium post ceramics

International Nuclear Information System (INIS)

Ussui, V.; Lazar, D.R.R.; Menezes, F.; Menezes, C.A.B.; Paschoal, J.O.A.

1996-01-01

The azeotropic distillation technique has been used for treatment of coprecipitated zirconium and yttrium hydroxides, in order to synthesize weak agglomerated powders. Experiments were performed by preparing suspensions of this precipitate with organic solvents as toluene, isopropanol, butanol and ethanol, which were submitted to the distillation, to remove all the liquid phase. The obtained powders after drying and calcination, have been characterized by granulometric distribution and specific surface area determination. The densities of the ceramic bodies, obtained by pressing and sintering at 1500 deg C during 1 hour, have also been evaluated. (author)

High-Temperature Ceramic Matrix Composite with High Corrosion Resistance

Science.gov (United States)

2010-06-02

description of high temperature oxidation processes of composite ceramic materials of ZrB2 - SiC and ZrB2-SiC-Zr(Mo)Si2 systems up to high (~1300 °C...analysis was applied using MІN-7 mineralogical microscope and a set of standard immersion liquids with the known values of refraction coefficients...2.0 V) corresponds to the simultaneous formation of ZrO2 zirconium dioxide of monoclinic modification and Zr(OH)4 zirconium hydroxide which is

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

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.

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.

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

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

Glass ceramic toughened with tetragonal zirconia

Science.gov (United States)

Keefer, Keith D.; Michalske, Terry A.

1986-01-01

A phase transformation-toughened glass ceramic and a process for making it are disclosed. A mixture of particulate network-forming oxide, network-modifying oxide, and zirconium oxide is heated to yield a homogeneous melt, and this melt is then heat-treated to precipitate an appreciable quantity of tetragonal zirconia, which is retained at ambient temperature to form a phase transformation-toughened glass ceramic. Nucleating agents and stabilizing agents may be added to the mixture to facilitate processing and improve the ceramic's properties. Preferably, the mixture is first melted at a temperature from 1200.degree. to 1700.degree. C. and is then heat-treated at a temperature within the range of 800.degree. to 1200.degree. C. in order to precipitate tetragonal ZrO.sub.2. The composition, as well as the length and temperature of the heat-treatment, must be carefully controlled to prevent solution of the precipitated tetragonal zirconia and subsequent conversion to the monoclinic phase.

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.

Study on application of zirconium dioxide for upgrading quality of pouring cups used in continuous steel casting technology

International Nuclear Information System (INIS)

Pham Ba Kien; Vu Thanh Quang and Ngo Van Tuyen

2004-01-01

This theme studies on technology of zirconium oxide powder stabilized by calcium and testing production of steel pouring cup made of the stabilized dioxide zirconium ceramic. As a product of the theme, the steel pouring cup has had the following main characteristics: heat resistance > 1700 o C, density of 4.7 g/cm 3 , apparent sponge degree of 1.63%, compressibility of 3300 kg/cm 2 . The quality of the cup has been tested and highly evaluated during the actual production. (author)

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)

Spectrophotometric titration of zirconium in siliceous materials

International Nuclear Information System (INIS)

Sugawara, K.F.; Su, Y.-S.; Strzegowski, W.R.

1978-01-01

An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1 to 5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. (author)

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.

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)

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

Institute of Scientific and Technical Information of China (English)

无

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.

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)

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.

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

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

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

Ceramic component for M.H.D electrode

International Nuclear Information System (INIS)

Marchant, D.D.; Bates, J.L.

1980-01-01

A ceramic component which exhibits electrical conductivity down to near room temperatures has the formula: Hfsub(x)Insub(y)Asub(z)O 2 where x = 0.1 to 0.4, y = 0.3 to 0.6, z = 0.1 to 0.4 and A is a rare earth or yttrium. The rare earth may be Yb, Tb, Pr or Ce. The component is suitable for use in the fabrication of MHD electrodes or as the current lead-out portion of a composite electrode with other ceramic components. An MHD electrode comprises a cap of a known ceramic, e.g. stabilised zirconium or hafnium oxide or terbium stabilised hafnium, a current lead-out ceramic according to the invention, and a copper frame. (author)

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

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.

Survival of anterior cantilevered all-ceramic resin-bonded fixed dental prostheses made from zirconia ceramic.

Science.gov (United States)

Sasse, Martin; Kern, Matthias

2014-06-01

This study evaluated the clinical outcome of all-ceramic resin-bonded fixed dental prostheses (RBFDPs) with a cantilevered single-retainer design made from zirconia ceramic. Forty-two anterior RBFDPs with a cantilevered single-retainer design were made from yttrium oxide-stabilized zirconium oxide ceramic. RBFDPs were inserted using Panavia 21 TC as luting agent after air-abrasion of the ceramic bonding surface. During a mean observation time of 61.8 months two debondings occurred. Both RBFDPs were rebonded using Panavia 21 TC and are still in function. A caries lesion was detected at one abutment tooth during recall and was treated with a composite filling. Therefore, the overall six-year failure-free rate according to Kaplan-Meier was 91.1%. If only debonding was defined as failure the survival rate increased to 95.2%. Since all RBFDPs are still in function the overall survival rate was 100% after six years. Cantilevered zirconia ceramic RBFDPs showed promising results within the observation period. Single-retainer resin-bonded fixed dental prostheses made from zirconia ceramic show very good mid-term clinical survival rates. They should therefore be considered as a viable treatment alternative for the replacement of single missing anterior teeth especially as compared to an implant therapy. Copyright © 2014 Elsevier Ltd. All rights reserved.

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

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.

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.)

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.)

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.

High temperature synthesis of ceramic composition by directed reaction of molten titanium or zirconium with boron carbide

International Nuclear Information System (INIS)

Johnson, W.B.

1990-01-01

Alternative methods of producing ceramics and ceramic composites include sintering, hot pressing and more recently hot isostatic pressing (HIP) and self-propagating high temperature synthesis (SHS). Though each of these techniques has its advantages, each suffers from several restrictions as well. Sintering may require long times at high temperatures and for most materials requires sintering aids to get full density. These additives can, and generally do, change (often degrade) the properties of the ceramic. Hot pressing and hot isostatic pressing are convenient methods to quickly prepare samples of some materials to full density, but generally are expensive and may damage some types of reinforcements during densification. This paper focuses on the preparation and processing of composites prepared by the directed reaction of molten titanium or zirconium with boron carbide. Advantages and disadvantages of this approach when compared to traditional methods are discussed, with reference to specific examples. Examples of microstructure are properties of these materials are reported

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

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.

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.

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.

Mechanical fatigue degradation of ceramics versus resin composites for dental restorations.

Science.gov (United States)

Belli, Renan; Geinzer, Eva; Muschweck, Anna; Petschelt, Anselm; Lohbauer, Ulrich

2014-04-01

For posterior partial restorations an overlap of indication exists where either ceramic or resin-based composite materials can be successfully applied. The aim of this study was to compare the fatigue resistance of modern dental ceramic materials versus dental resin composites in order to address such conflicts. Bar specimens of five ceramic materials and resin composites were produced according to ISO 4049 and stored for 14 days in distilled water at 37°C. The following ceramic materials were selected for testing: a high-strength zirconium dioxide (e.max ZirCAD, Ivoclar), a machinable lithium disilicate (e.max CAD, Ivoclar), a pressable lithium disilicate ceramic (e-max Press, Ivoclar), a fluorapatite-based glass-ceramic (e.max Ceram, Ivoclar), and a machinable color-graded feldspathic porcelain (Trilux Forte, Vita). The composite materials selected were: an indirect machinable composite (Lava Ultimate, 3M ESPE) and four direct composites with varying filler nature (Clearfil Majesty Posterior, Kuraray; GrandioSO, Voco; Tetric EvoCeram, Ivoclar-Vivadent; and CeramX Duo, Dentsply). Fifteen specimens were tested in water for initial strength (σin) in 4-point bending. Using the same test set-up, the residual flexural fatigue strength (σff) was determined using the staircase approach after 10(4) cycles at 0.5 Hz (n=25). Weibull parameters σ0 and m were calculated for the σin specimens, whereas the σff and strength loss in percentage were obtained from the fatigue experiment. The zirconium oxide ceramic showed the highest σin and σff (768 and 440 MPa, respectively). Although both lithium disilicate ceramics were similar in the static test, the pressable version showed a significantly higher fatigue resistance after cyclic loading. Both the fluorapatite-based and the feldspathic porcelain showed equivalent initial and cyclic fatigue properties. From the composites, the highest filled direct material Clearfil Majesty Posterior showed superior fatigue performance

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

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.

Electrostatic Assembly Preparation of High-Toughness Zirconium Diboride-Based Ceramic Composites with Enhanced Thermal Shock Resistance Performance.

Science.gov (United States)

Zhang, Baoxi; Zhang, Xinghong; Hong, Changqing; Qiu, Yunfeng; Zhang, Jia; Han, Jiecai; Hu, PingAn

2016-05-11

The central problem of using ceramic as a structural material is its brittleness, which associated with rigid covalent or ionic bonds. Whiskers or fibers of strong ceramics such as silicon carbide (SiC) or silicon nitride (Si3N4) are widely embedded in a ceramic matrix to improve the strength and toughness. The incorporation of these insulating fillers can impede the thermal flow in ceramic matrix, thus decrease its thermal shock resistance that is required in some practical applications. Here we demonstrate that the toughness and thermal shock resistance of zirconium diboride (ZrB2)/SiC composites can be improved simultaneously by introducing graphene into composites via electrostatic assembly and subsequent sintering treatment. The incorporated graphene creates weak interfaces of grain boundaries (GBs) and optimal thermal conductance paths inside composites. In comparison to pristine ZrB2-SiC composites, the toughness of (2.0%) ZrB2-SiC/graphene composites exhibited a 61% increasing (from 4.3 to 6.93 MPa·m(1/2)) after spark plasma sintering (SPS); the retained strength after thermal shock increased as high as 74.8% at 400 °C and 304.4% at 500 °C. Present work presents an important guideline for producing high-toughness ceramic-based composites with enhanced thermal shock properties.

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)

Fracture properties and heat resistance of ceramics consisting of microspheres of stabilized zirconium dioxide

International Nuclear Information System (INIS)

Krasulin, Yu.L.; Barinov, S.M.; Ivanov, A.B.; Timofeev, V.N.; Grevtsev, S.N.; Ivanov, D.A.

1980-01-01

Determined were effective specific fracture work, critical coefficient of stress intensity in the upper point of the fracture, strength and heat resistance during heat changes (20-1300 deg C) of the material produced by sintering stabilized zirconium dioxide microspheres. Dependence of these characteristics on granulometric composition of microspheres was determined. It was ascertained that the additional introduction of large microspheres into the bulk of small microspheres increased the metal fracture work. Specific work of material fracture progress exceeded specific work of fracture motion initiation. High value of fracture work together with high strength permits to use the material formed of microspheres as structural ceramics

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.

Flash sintering of ceramic materials

Science.gov (United States)

Dancer, C. E. J.

2016-10-01

During flash sintering, ceramic materials can sinter to high density in a matter of seconds while subjected to electric field and elevated temperature. This process, which occurs at lower furnace temperatures and in shorter times than both conventional ceramic sintering and field-assisted methods such as spark plasma sintering, has the potential to radically reduce the power consumption required for the densification of ceramic materials. This paper reviews the experimental work on flash sintering methods carried out to date, and compares the properties of the materials obtained to those produced by conventional sintering. The flash sintering process is described for oxides of zirconium, yttrium, aluminium, tin, zinc, and titanium; silicon and boron carbide, zirconium diboride, materials for solid oxide fuel applications, ferroelectric materials, and composite materials. While experimental observations have been made on a wide range of materials, understanding of the underlying mechanisms responsible for the onset and latter stages of flash sintering is still elusive. Elements of the proposed theories to explain the observed behaviour include extensive Joule heating throughout the material causing thermal runaway, arrested by the current limitation in the power supply, and the formation of defect avalanches which rapidly and dramatically increase the sample conductivity. Undoubtedly, the flash sintering process is affected by the electric field strength, furnace temperature and current density limit, but also by microstructural features such as the presence of second phase particles or dopants and the particle size in the starting material. While further experimental work and modelling is still required to attain a full understanding capable of predicting the success of the flash sintering process in different materials, the technique non-etheless holds great potential for exceptional control of the ceramic sintering process.

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.

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

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

Planar ceramic membrane assembly and oxidation reactor system

Science.gov (United States)

Carolan, Michael Francis; Dyer, legal representative, Kathryn Beverly; Wilson, Merrill Anderson; Ohm, Ted R.; Kneidel, Kurt E.; Peterson, David; Chen, Christopher M.; Rackers, Keith Gerard; Dyer, deceased, Paul Nigel

2007-10-09

Planar ceramic membrane assembly comprising a dense layer of mixed-conducting multi-component metal oxide material, wherein the dense layer has a first side and a second side, a porous layer of mixed-conducting multi-component metal oxide material in contact with the first side of the dense layer, and a ceramic channeled support layer in contact with the second side of the dense layer. The planar ceramic membrane assembly can be used in a ceramic wafer assembly comprising a planar ceramic channeled support layer having a first side and a second side; a first dense layer of mixed-conducting multi-component metal oxide material having an inner side and an outer side, wherein the inner side is in contact with the first side of the ceramic channeled support layer; a first outer support layer comprising porous mixed-conducting multi-component metal oxide material and having an inner side and an outer side, wherein the inner side is in contact with the outer side of the first dense layer; a second dense layer of mixed-conducting multi-component metal oxide material having an inner side and an outer side, wherein the inner side is in contact with the second side of the ceramic channeled layer; and a second outer support layer comprising porous mixed-conducting multi-component metal oxide material and having an inner side and an outer side, wherein the inner side is in contact with the outer side of the second dense layer.

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

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.

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.

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

Reactive Spark Plasma Sintering and Mechanical Properties of Zirconium Diboride–Titanium Diboride Ultrahigh Temperature Ceramic Solid Solutions

Directory of Open Access Journals (Sweden)

Karthiselva N. S.

2016-09-01

Full Text Available Ultrahigh temperature ceramics (UHTCs such as diborides of zirconium, hafnium tantalum and their composites are considered to be the candidate materials for thermal protection systems of hypersonic vehicles due to their exceptional combination of physical, chemical and mechanical properties. A composite of ZrB2-TiB2 is expected to have better properties. In this study, an attempt has been made to fabricate ZrB2-TiB2 ceramics using mechanically activated elemental powders followed by reactive spark plasma sintering (RSPS at 1400 °C. Microstructure and phase analysis was carried out using X-ray diffractometer (XRD and electron microscopy to understand microstructure evolution. Fracture toughness and hardness were evaluated using indentation methods. Nanoindentation was used to measure elastic modulus. Compressive strength of the composites has been reported.

Structural characterization of clays commercially used in red ceramics

International Nuclear Information System (INIS)

Brito, E.M.; Moura, J.K.L.; Souza, R.B.; Brandim, A.S.

2014-01-01

The use of clays hills being an alternative to clay floodplain, due to environmental protection laws. The research project aims at the morphological and chemical characterization of hills clays used industrially for the production of ceramic tiles and blocks. Therefore, two types of methods were known commercially in the region of Teresina-PI through diffraction of X-rays (X-DR), scanning electron microscopy (SEM) and energy dispersive spectrometry X-ray (EDS). It can be observed that the samples have a high percentage of quartz, hematite still having in its constitution aluminum oxide, zirconium oxide and titanium oxide. The results show that the clays are clays and montmorillonites may be used for the production of ceramic tiles and blocks, but as the proportion of using the same will be focusing the next job. (author)

Microwave processing of ceramic oxide filaments

Energy Technology Data Exchange (ETDEWEB)

Vogt, G.J.; Katz, J.D. [Los Alamos National Laboratory, NM (United States)

1995-05-01

The objective of the microwave filament processing project is to develop microwave techniques at 2.45 GHZ to manufacture continuous ceramic oxide filaments. Microwave processing uses the volumetric absorption of microwave power in oxide filament tows to drive off process solvents, to burn out organic binders, and to sinter the dried fibers to produce flexible, high-strength ceramic filaments. The technical goal is to advance filament processing technology by microwave heating more rapidly with less energy and at a lower cost than conventional processing, but with the same quality as conventional processing. The manufacturing goal is to collaborate with the 3M Company, a US manufacturer of ceramic oxide filaments, to evaluate the technology using a prototype filament system and to transfer the microwave technology to the 3M Company.

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

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.

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.

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)

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)

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)

Improved dielectric and ferroelectric properties of Mn doped barium zirconium titanate (BZT) ceramics for energy storage applications

Science.gov (United States)

Sangwan, Kanta Maan; Ahlawat, Neetu; Kundu, R. S.; Rani, Suman; Rani, Sunita; Ahlawat, Navneet; Murugavel, Sevi

2018-06-01

Lead free Mn doped barium zirconium titanate ceramic of composition BaZr0.045 (MnxTi1-x)0.955O3 (x = 0.00, 0.01, 0.02) were prepared by solid state reaction method. Tetragonal perovskite structure was confirmed by Rietveld refinement of X-ray diffraction pattern. Analysis of Scanning electron microscope (SEM) micrographs revealed that addition of Mn up to a certain limit accelerates grain growth of BZT ceramic. Static dielectric constant was successfully extended up to high frequencies with an appreciable decrease in dielectric loss about 70% for Mn doped BZT ceramics. The experimental data fitted with Curie Weiss Law and Power Law confirmed first order transition and diffusive behavior of the investigated system. The shifting of Curie temperature (Tc) from 387 K to 402 K indicated tendency for sustained ferroelectricity in doped BZMT ceramics. High value of percentage temperature coefficient of capacitance TCC >10% near Tc was observed for all the compositions and increases with Mn content in pure BZT. At room temperature, BZT modified ceramic corresponding to x = 0.01 composition shows better values of remnant polarization (Pr = 5.718 μC/cm2), saturation polarization (Ps = 14.410 μC/cm2), low coercive field (Ec = 0.612 kV/cm), and highest value of Pr/Ps = 0.396.

In-situ synthesized Ni–Zr intermetallic/ceramic reinforced composite coatings on zirconium substrate by high power diode laser

Energy Technology Data Exchange (ETDEWEB)

Liu, Kun; Li, Yajiang, E-mail: yajli@sdu.edu.cn; Wang, Juan; Ma, Qunshuang

2015-03-05

Highlights: • In-situ synthesized Ni–Zr intermetallics/ceramic reinforced composite coatings. • Si enrichment and Ni replacing site of Si both resulted in forming Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4.} • Microstructure and forming of ZrB{sub 2} depended on affinity of elements and Si/B ratio. - Abstract: Ni–Zr intermetallic/ceramic reinforced composite coatings were in-situ synthesized by laser cladding series of Ni–Cr–B–Si powders on zirconium substrate. Microstructure, phase constituents and microhardness of coatings were investigated by means of optical microscope (OM), scanning electron microscope (SEM), energy dispersive spectrometer (EDS), X-ray diffraction (XRD) and microsclemeter. Results indicated that coatings with metallurgical bonding to substrate consisted of cellular NiZr matrix and massive reinforcements including NiZr{sub 2}, Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4} and ZrB{sub 2}. Morphologies of reinforcements were mainly dominated by temperature gradient and cooling rate from surface to bottom of the coating produced by same powder. In different coatings, microstructure and forming of ZrB{sub 2} mainly depended on affinity of elements and Si/B ratio in different powders. In addition, the mean microhardness of coatings up to 1200–1300 HV{sub 0.2} is nearly 7 times higher than that of R60702 zirconium substrate.

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

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

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

Structural behaviour of nitrogen in oxide ceramics

International Nuclear Information System (INIS)

Ghauri, K.M.

1997-01-01

The solubility of nitrogen in molten oxides has significant consideration for two quite different types of engineering materials. The implication of a knowledge of the role of nitrogen in these oxides for refining high nitrogen steels in obvious but similar nitrogen-bearing oxide melts are of critical importance in the densification of silicon nitride ceramics. Present paper discusses structural behaviour and phase equilibria qualitatively in the light of knowledge available on slag structure through infrared and x-ray diffraction. Nitrogen solubility in glasses and related sialon based ceramics may be of paramount importance to understand the role of nitrogen in these materials as these oxides are similar in composition, structure and characteristics to sintering glasses in nitrogen ceramics. It is quite logical to infer that the same oxide model can be applied in order to massively produce nitrogen alloyed steels which are actively competing to be the materials of the next century. (author)

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.)

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.)

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

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.

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)

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

Science.gov (United States)

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

2015-12-01

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

Lutetium oxide-based transparent ceramic scintillators

Science.gov (United States)

Seeley, Zachary; Cherepy, Nerine; Kuntz, Joshua; Payne, Stephen A.

2016-01-19

In one embodiment, a transparent ceramic of sintered nanoparticles includes gadolinium lutetium oxide doped with europium having a chemical composition (Lu.sub.1-xGd.sub.x).sub.2-YEu.sub.YO.sub.3, where X is any value within a range from about 0.05 to about 0.45 and Y is any value within a range from about 0.01 to about 0.2, and where the transparent ceramic exhibits a transparency characterized by a scatter coefficient of less than about 10%/cm. In another embodiment, a transparent ceramic scintillator of sintered nanoparticles, includes a body of sintered nanoparticles including gadolinium lutetium oxide doped with a rare earth activator (RE) having a chemical composition (Lu.sub.1-xGd.sub.x).sub.2-YRE.sub.YO.sub.3, where RE is selected from the group consisting of: Sm, Eu, Tb, and Dy, where the transparent ceramic exhibits a transparency characterized by a scatter coefficient of less than about 10%/cm.

Structure and short time degradation studies of sodium zirconium phosphate ceramics loaded with simulated fast breeder (FBR) waste

Energy Technology Data Exchange (ETDEWEB)

Ananthanarayanan, A., E-mail: arvinda@barc.gov.in [Process Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Ambashta, R.D., E-mail: aritu@barc.gov.in [Process Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Sudarsan, V. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Ajithkumar, T. [Applied Catalysis Unit, National Chemical Laboratory, Pune 411008 (India); Sen, D.; Mazumder, S. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Wattal, P.K. [Process Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

2017-04-15

Sodium zirconium phosphate (NZP) ceramics have been prepared using conventional sintering and hot isostatic pressing (HIP) routes. The structure of NZP ceramics, prepared using the HIP route, has been compared with conventionally sintered NZP using a combination of X-ray diffraction (XRD) and ({sup 31}P and {sup 23}Na) nuclear magnetic resonance (NMR) spectroscopy techniques. It is observed that NZP with no waste loading is aggressive toward the steel HIP-can during hot isostatic compaction and significant fraction of cations from the steel enter the ceramic material. Waste loaded NZP samples (10 wt% simulated FBR waste) show significantly low can-interaction and primary NZP phase is evident in this material. Upon exposure of can-interacted and waste loaded NZP to boiling water and steam, {sup 31}P NMR does not detect any major modifications in the network structure. However, the {sup 23}Na NMR spectra indicate migration of Na{sup +} ions from the surface and possible re-crystallization. This is corroborated by Small-Angle Neutron Scattering (SANS) data and Scanning Electron Microscopy (SEM) measurements carried out on these samples.

Composition and microstructure of zirconium and hafnium germanates obtained by different chemical routes

International Nuclear Information System (INIS)

Utkin, A.V.; Prokip, V.E.; Baklanova, N.I.

2014-01-01

The phase composition and morphology of zirconium and hafnium germanates synthesized by ceramic and co-precipitation routes were studied. The products were characterized using high-temperature X-ray diffraction analysis (XRD), Raman spectroscopy, scanning electron microscopy (SEM) and thermal (TG/DTA) analysis. To investigate the phase composition and stoichiometry of compounds the unit cell parameters were refined by full-profile Rietveld XRD analysis. The morphology of products and its evolution during high-temperature treatment was examined by SEM analysis. It was stated that there is the strong dependence of the phase composition and morphology of products on the preparation route. The ceramic route requires a multi-stage high-temperature treatment to obtain zirconium and hafnium germanates of 95% purity or more. Also, there are strong diffusion limitations to obtain hafnium germanate Hf 3 GeO 8 by ceramic route. On the contrary, the co-precipitation route leads to the formation of nanocrystalline single phase germanates of stoichiometric composition at a relatively low temperatures (less than 1000 °C). The results of quantitative XRD analysis showed the hafnium germanates are stoichiometric compounds in contrast to zirconium germanates that form a set of solid solutions. This distinction may be related to the difference in the ion radii of Zr and Hf. - Graphical abstract: The phase composition and morphology of zirconium and hafnium germanates synthesized by ceramic and co-precipitation routes were studied. It was stated that there is the strong dependence of the phase composition and morphology of products on the preparation route. Display Omitted - Highlights: • Zr and Hf germanates were synthesized by ceramic and co-precipitation routes. • The morphology of products depends on the synthesis parameters. • Zirconium germanates forms a set of solid solutions. • Hafnium germanates are stoichiometric compounds

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)

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.

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)

Reduction-oxidation Enabled Glass-ceramics to Stainless Steel Bonding Part I: screening of doping oxidants

Energy Technology Data Exchange (ETDEWEB)

Dai, Steve Xunhu [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

2015-09-01

Lithium silicate-based glass-ceramics with high coefficients of thermal expansion, designed to form matched hermetic seals in 304L stainless steel housing, show little evidence of interfacial chemical bonding, despite extensive inter-diffusion at the glass-ceramic-stainless steel (GC-SS) interface. A series of glass-ceramic compositions modified with a variety of oxidants, AgO, FeO, NiO, PbO, SnO, CuO, CoO, MoO₃ and WO₃, are examined for the feasibility of forming bonding oxides through reduction-oxidation (redox) at the GC-SS interface. The oxidants were selected according to their Gibbs free energy to allow for oxidation of Cr/Mn/Si from stainless steel, and yet to prevent a reduction of P2O5 in the glass-ceramic where the P₂O₅ is to form Li₃PO₄ nuclei for growth of high expansion crystalline SiO₂ phases. Other than the CuO and CoO modified glass-ceramics, bonding from interfacial redox reactions were not achieved in the modified glass-ceramics, either because of poor wetting on the stainless steel or a reduction of the oxidants at the surface of glass-ceramic specimens rather than the GC-SS interface.

Ceramic Coatings for Clad (The C³ Project): Advanced Accident-Tolerant Ceramic Coatings for Zr-Alloy Cladding

Energy Technology Data Exchange (ETDEWEB)

Sickafus, Kurt E. [Univ. of Tennessee, Knoxville, TN (United States); Wirth, Brian [Univ. of Tennessee, Knoxville, TN (United States); Miller, Larry [Univ. of Tennessee, Knoxville, TN (United States); Weber, Bill [Univ. of Tennessee, Knoxville, TN (United States); Zhang, Yanwen [Univ. of Tennessee, Knoxville, TN (United States); Patel, Maulik [Univ. of Tennessee, Knoxville, TN (United States); Motta, Arthur [Pennsylvania State Univ., University Park, PA (United States); Wolfe, Doug [Pennsylvania State Univ., University Park, PA (United States); Fratoni, Max [Univ. of California, Berkeley, CA (United States); Raj, Rishi [Univ. of Colorado, Boulder, CO (United States); Plunkett, Kenneth [Univ. of Colorado, Boulder, CO (United States); Was, Gary [Univ. of Michigan, Ann Arbor, MI (United States); Hollis, Kendall [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Nelson, Andy [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Stanek, Chris [Los Alamos National Lab. (LANL), Los Alamos, NM (United States); Comstock, Robert [Westinghouse Electric Corporation, Pittsburgh, PA (United States); Partezana, Jonna [Westinghouse Electric Corporation, Pittsburgh, PA (United States); Whittle, Karl [Univ. of Sheffield (United Kingdom); Preuss, Michael [Univ. of Manchester (United Kingdom); Withers, Philip [Univ. of Manchester (United Kingdom); Wilkinson, Angus [Univ. of Oxford (United Kingdom); Donnelly, Stephen [Univ. of Huddersfield (United Kingdom); Riley, Daniel [Australian Nuclear Science and Technology Organisation, Syndney (Australia)

2017-02-14

The goal of this NEUP-IRP project is to develop a fuel concept based on an advanced ceramic coating for Zr-alloy cladding. The coated cladding must exhibit demonstrably improved performance compared to conventional Zr-alloy clad in the following respects: During normal service, the ceramic coating should decrease cladding oxidation and hydrogen pickup (the latter leads to hydriding and embrittlement). During a reactor transient (e.g., a loss of coolant accident), the ceramic coating must minimize or at least significantly delay oxidation of the Zr-alloy cladding, thus reducing the amount of hydrogen generated and the oxygen ingress into the cladding. The specific objectives of this project are as follows: To produce durable ceramic coatings on Zr-alloy clad using two possible routes: (i) MAX phase ceramic coatings or similar nitride or carbide coatings; and (ii) graded interface architecture (multilayer) ceramic coatings, using, for instance, an oxide such as yttria-stabilized zirconia (YSZ) as the outer protective layer. To characterize the structural and physical properties of the coated clad samples produced in 1. above, especially the corrosion properties under simulated normal and transient reactor operating conditions. To perform computational analyses to assess the effects of such coatings on fuel performance and reactor neutronics, and to perform fuel cycle analyses to assess the economic viability of modifying conventional Zr-alloy cladding with ceramic coatings. This project meets a number of the goals outlined in the NEUP-IRP call for proposals, including: Improve the fuel/cladding system through innovative designs (e.g. coatings/liners for zirconium-based cladding) Reduce or eliminate hydrogen generation Increase resistance to bulk steam oxidation Achievement of our goals and objectives, as defined above, will lead to safer light-water reactor (LWR) nuclear fuel assemblies, due to improved cladding properties and built-in accident resistance, as well as

Structure, dielectric and electrical properties of cerium doped barium zirconium titanate ceramics

International Nuclear Information System (INIS)

Feng Hongjun; Hou Jungang; Qu Yuanfang; Shan Dan; Yao Guohua

2012-01-01

Highlights: ► Rare-earth doped barium zirconate titanate (BZT) ceramics, Ba(Zr 0.25 Ti 0.75 )O 3 + xCeO 2 , (x = 0–1.5 at%) were obtained by a solid state reaction route. ► Morphological analysis on sintered samples by scanning electron microscopy shows that the addition of rare-earth ions affects the growth of the grain and remarkably changes the grain morphology. ► The effect of rare-earth addition to BZT on dielectric and electrical properties is analyzed, demonstrating that the samples with x = 0.4 and x = 0.6 could be semiconducting in air atmosphere. - Abstract: Rare-earth doped barium zirconium titanate (BZT) ceramics, Ba(Zr 0.25 Ti 0.75 )O 3 + xCeO 2 , (x = 0–1.5 at%) were obtained by a solid state reaction route. Perovskite-like single-phase compounds were confirmed from X-ray diffraction data and the lattice parameters were refined by the Rietveld method. It is found that, integrating with the lattice parameters and the distortion of crystal lattice, there is an alternation of substitution preference of cerium ions for the host cations in perovskite lattice. Morphological analysis on sintered samples by scanning electron microscopy shows that the addition of rare-earth ions affects the growth of the grain and remarkably changes the grain morphology. The effect of rare-earth addition to BZT on dielectric and electrical properties is analyzed. High values of dielectric tunability are obtained for cerium doped BZT. Especially, the experimental results on the effect of the contents of rare-earth addition on the resistivity of BZT ceramics were investigated, demonstrating that the samples with x = 0.4 and x = 0.6 could be semiconducting in air atmosphere.

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.

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.

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

Fatigue limit of polycrystalline zirconium oxide ceramics: effect of grinding and low-temperature aging

NARCIS (Netherlands)

Pereira, G.K.R.; Silvestri, T.; Amaral, M.; Rippe, M.P.; Kleverlaan, C.J.; Valandro, L.F.

2016-01-01

The following study aimed to evaluate the effect of grinding and low-temperature aging on the fatigue limit of Y-TZP ceramics for frameworks and monolithic restorations. Disc specimens from each ceramic material, Lava Frame (3M ESPE) and Zirlux FC (Ivoclar Vivadent) were manufactured according to

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

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)

Polymer derived non-oxide ceramics modified with late transition metals.

Science.gov (United States)

Zaheer, Muhammad; Schmalz, Thomas; Motz, Günter; Kempe, Rhett

2012-08-07

This tutorial review highlights the methods for the preparation of metal modified precursor derived ceramics (PDCs) and concentrates on the rare non-oxide systems enhanced with late transition metals. In addition to the main synthetic strategies for modified SiC and SiCN ceramics, an overview of the morphologies, structures and compositions of both, ceramic materials and metal (nano) particles, is presented. Potential magnetic and catalytic applications have been discussed for the so manufactured metal containing non-oxide ceramics.

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.

A comparison of the marginal vertical discrepancies of zirconium and metal ceramic posterior fixed dental prostheses before and after cementation.

Science.gov (United States)

Gonzalo, Esther; Suárez, Maria J; Serrano, Benjamin; Lozano, Jose F L

2009-12-01

increase in the vertical marginal discrepancies of the FDPs and that an internal space of 50 mum provided a high precision of fit of the restorations. The accuracy of fit achieved for the 3 zirconium oxide groups analyzed was within the range of clinical acceptance, and the discrepancies were lower than in the metal ceramic group. Procera Bridge Zirconia showed the lowest vertical discrepancies.

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.

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

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.

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

Determination of zirconium by fluoride ion selective electrode

International Nuclear Information System (INIS)

Mahanty, B.N.; Sonar, V.R.; Gaikwad, R.; Raul, S.; Das, D.K.; Prakash, A.; Afzal, Md.; Panakkal, J.P.

2010-01-01

Full text: Zirconium is used in a wide range of applications including nuclear clad, catalytic converters, surgical appliances, metallurgical furnaces, superconductors, ceramics, lamp filaments, anti corrosive alloys and photographical purposes. Irradiation testing of U-Zr and U-Pu-Zr fuel pins has also demonstrated their feasibility as fuel in liquid metal reactors. Different methods that are employed for the determination of zirconium are spectrophotometry, potentiometry, neutron activation analysis and mass spectrometry. Ion-selective electrode (ISE), selective to zirconium ion has been studied for the direct potentiometric measurements of zirconium ions in various samples. In the present work, an indirect method has been employed for the determination of zirconium in zirconium nitrate sample using fluoride ion selective electrode. This method is based on the addition of known excess amount of fluoride ion to react with the zirconium ion to produce zirconium tetra fluoride at about pH 2-3, followed by determination of residual fluoride ion selective electrode. The residual fluoride ion concentrations were determined from the electrode potential data using calibration plot. Subsequently, zirconium ion concentrations were determined from the concentration of consumed fluoride ions. A precision of about 2% (RSD) with the mean recovery of more than 94% has been achieved for the determination of zirconium at the concentration of 4.40 X 10 -3 moles lit -1

METHOD AND ALLOY FOR BONDING TO ZIRCONIUM

Science.gov (United States)

McCuaig, F.D.; Misch, R.D.

1960-04-19

A brazing alloy can be used for bonding zirconium and its alloys to other metals, ceramics, and cermets, and consists of 6 to 9 wt.% Ni, 6 to 9 wn~.% Cr, Mo, or W, 0 to 7.5 wt.% Fe, and the balance Zr.

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.

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.

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

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.

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

Continuous fiber ceramic composite. Phase I final report, April 1992--April 1993

Energy Technology Data Exchange (ETDEWEB)

Goettler, R.W.

1995-04-01

Babcock and Wilcox assembled a team to develop the Continuous Fiber Ceramic Composite (CFCC) processing technology, identify the industrial applications, generate design and life prediction software, and to begin the necessary steps leading to full commercialization of CFCC components. Following is a summary of Phase I activities on this program. B&W has selected an oxide-oxide composite system for development and optimization in this program. This selection was based on the results of exposure tests in combustion environments typical of the boiler and heat exchanger applications. Aluminum oxide fiber is the selected reinforcement, and both aluminum oxide and zirconium oxide matrices were selected, based on their superior resistance to chemical attack in hostile industrial service.

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.

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.

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

Preparation, microstructural evolution and properties of Ni–Zr intermetallic/Zr–Si ceramic reinforced composite coatings on zirconium alloy by laser cladding

Energy Technology Data Exchange (ETDEWEB)

Liu, Kun; Li, Yajiang, E-mail: yajli@sdu.edu.cn; Wang, Juan; Ma, Qunshuang; Li, Jishuai; Li, Xinyue

2015-10-25

NiZr{sub 2}–ZrSi–Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4}-ZrC intermetallic/ceramic reinforced composite coatings were in situ synthesized by laser cladding the pre-placed Ni–Cr–B–Si powder on zirconium substrate. Microstructure and phase constituents were investigated by X-ray diffraction (XRD), optical microscope (OM), scanning electron microscope (SEM) and energy dispersive spectroscopy (EDS). Microhardness tester and block-on-ring wear tester were employed to measure the hardness distribution and wear resistance of the intermetallic/ceramic reinforced composite coating. Results indicated that the multiphase of reinforcements includes Ni–Zr intermetallic compounds (e.g., NiZr and NiZr{sub 2}) and Zr–Si(C) ceramic phases (e.g., ZiSi, Zr{sub 5}Si{sub 4} and ZrC). Ni–Si clusters transforming to Zr–Si–Ni clusters at high temperature facilitated the forming of Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4} and during the growth of Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4}, the consumption of Zr atoms at the lateral interface of liquid/Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4} resulted into developing Zr-poor zone near Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4}. The microhardness and wear resistance of the coating were significantly improved by various reinforced phases in comparison to zirconium substrate. - Highlights: • NiZr{sub 2}–ZrSi–Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4}-ZrC compostie coating was in-situ synthesized. • Ni–Si clusters transforming resulted into developing Zr-poor zone near Zr{sub 5}(Si{sub x}Ni{sub 1−x}){sub 4}. • Reinforced phases significantly improve wear resistance of the coating.

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.

Manufacturing process for the metal ceramic hybrid fuel cladding tube

International Nuclear Information System (INIS)

Jung, Yang Il; Kim, Sun Han; Park, Jeong Yong

2012-01-01

For application in LWRs with suppressed hydrogen release, a metal-ceramic hybrid cladding tube has been proposed. The cladding consists of an inner zirconium tube and outer SiC fiber matrix SiC ceramic composite. The inner zirconium allows the matrix to remain fully sealed even if the ceramic matrix cracks through. The outer SiC composite can increase the safety margin by taking the merits of the SiC itself. However, it is a challenging task to fabricate the metal-ceramic hybrid tube. Processes such as filament winding, matrix impregnation, and surface costing are additionally required for the existing Zr based fuel cladding tubes. In the current paper, the development of the manufacturing process will be introduced

Manufacturing process for the metal ceramic hybrid fuel cladding tube

Energy Technology Data Exchange (ETDEWEB)

Jung, Yang Il; Kim, Sun Han; Park, Jeong Yong [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

2012-10-15

For application in LWRs with suppressed hydrogen release, a metal-ceramic hybrid cladding tube has been proposed. The cladding consists of an inner zirconium tube and outer SiC fiber matrix SiC ceramic composite. The inner zirconium allows the matrix to remain fully sealed even if the ceramic matrix cracks through. The outer SiC composite can increase the safety margin by taking the merits of the SiC itself. However, it is a challenging task to fabricate the metal-ceramic hybrid tube. Processes such as filament winding, matrix impregnation, and surface costing are additionally required for the existing Zr based fuel cladding tubes. In the current paper, the development of the manufacturing process will be introduced.

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

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

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

Effect of mineralizer lithium fluoride on praseodymium-zirconium-yellow ceramic pigment%矿化剂氟化锂对镨锆黄陶瓷色料的影响

Institute of Scientific and Technical Information of China (English)

董伟霞; 包启富; 顾幸勇; 易玉如

2017-01-01

Due to its stable color and low price, zirconium yellow ceramic pigment has become the favorite of high temperature ceramic pigment market. But the synthesis temperature of zirconium yellow ceramic pigment prepared by the traditional solid phase method is high (>1600℃) , resulting in the too large particle size of pigment and thus poor color performance. Therefore, reducing the synthesis temperature for the decrease in the particle size of the pigment has become a research hotspot. In the paper, zirconium praseodymium yellow pigment precursor is prepared by a solvothermal method using zirconium silicate, tetraethyl orthosilicate and praseodymium oxide as the main raw materials, then added LiF with various concentrations to reduce the synthesis temperature. The yellow pigment was obtained at 1100℃ for 50 min. The colorimeter, particle-size analyzer, ultraviolet visible light spectrum analyzer, scanning electron microscope ( SEM) and X-ray diffract analysis ( XRD) are utilized to characterize the properties and microstructure of the samples. The results show that compared with other samples, the sample with 0. 35% LiF concentration has the higher crystallinity, smaller and more uniform particle size, resulting in the stronger absorption at 400~480 nm for the blue and purple light. Therefore, the sample with 0.35% LiF concentration exhibits a pure yellow hue of L?=84.92, a?=4.70, b?=68.00, which is promising for applicationin ceramic inkjet printing technology in the future.%谱锆黄陶瓷色料由于呈色稳定,价格较低廉已成为高温陶瓷色料市场的宠儿,但传统固相法所制备的谱锆黄陶瓷色料煅烧温度高(>1600℃),导致颜料粒径过大影响呈色性能,因此,降低合成温度减小�

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...

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)

Development of zirconium/magnesium phosphate composites for immobilization of fission products

International Nuclear Information System (INIS)

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

1999-01-01

Novel chemically bonded phosphate ceramics have been investigated for the capture and stabilization of volatile fission-product radionuclides. The authors have used low-temperature processing to fabricate zirconium phosphate and zirconium/magnesium phosphate composites. A zirconium/magnesium phosphate composite has been developed and shown to stabilize ash waste that has been contaminated with a radioactive surrogate of the 137 Cs and 90 Sr species. Excellent retention of cesium in the phosphate matrix system was observed in both short- and long-term leaching tests. The retention factor determined by the USEPA Toxicity Characteristic Leaching Procedure was one order of magnitude better for cesium that for strontium. The effective diffusivity, at room temperature, for cesium and strontium in the waste forms was estimated to be as low as 2.4 x 10 -13 and 1.2 x 10 -11 m 2 /s, respectively. This behavior was attributed to the capture of cesium in the layered zirconium phosphate structure via an intercalation ion-exchange reaction, followed by microencapsulation. However, strontium is believed to be precipitated out in its phosphate form and subsequently microencapsulated in the phosphate ceramic. The performance of these final waste forms, as indicated by the compression strength and the durability in aqueous environments, satisfies the regulatory criteria

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.

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

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.

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.)

Analyses on Silicide Coating for LOCA Resistant Cladding

Energy Technology Data Exchange (ETDEWEB)

Sweidan, Faris B.; Lee, You Ho; Ryu, Ho Jin [KAIST, Daejeon (Korea, Republic of)

2015-10-15

A particular focus of accident-tolerant fuel has been cladding due to the rapid high-temperature oxidation of zirconium-based cladding with the evolution of H2 when steam is a reactant. Some key features of the coated cladding include high-temperature resistance to oxidation, lower processing temperatures, and a high melting point of the coating. Zirconium alloys exhibit a reasonably high melting temperature, so a coating for the cladding is appealing if the coating increases the high-temperature resistance to oxidation. In this case, the cladding is protected from complete oxidation. The cladding coating involves the application of zirconium silicide onto Zr-based cladding. Zirconium silicide coating is expected to produce a glassy layer that becomes more protective at elevated temperature. For this reason, silicide coatings on cladding offer the potential for improved reliability at normal operating temperatures and at the higher transient temperatures encountered during accidents. Although ceramic coatings are brittle and may have weak points to be used as coating materials, several ceramic coatings were successful and showed adherent behavior and high resistance to oxidation. In this study, the oxidation behavior of zirconium silicide and its oxidation kinetics are analyzed. Zirconium silicide is a new suggested material to be used as coatings on existing Zr-based cladding alloys, the aim of this study is to evaluate if zirconium silicide is applicable to be used, so they can be more rapidly developed using existing cladding technology with some modifications. These silicide coatings are an attractive alternative to the use of coatings on zirconium claddings or to the lengthy development of monolithic ceramic or ceramic composite claddings and coatings.

Analyses on Silicide Coating for LOCA Resistant Cladding

International Nuclear Information System (INIS)

Sweidan, Faris B.; Lee, You Ho; Ryu, Ho Jin

2015-01-01

A particular focus of accident-tolerant fuel has been cladding due to the rapid high-temperature oxidation of zirconium-based cladding with the evolution of H2 when steam is a reactant. Some key features of the coated cladding include high-temperature resistance to oxidation, lower processing temperatures, and a high melting point of the coating. Zirconium alloys exhibit a reasonably high melting temperature, so a coating for the cladding is appealing if the coating increases the high-temperature resistance to oxidation. In this case, the cladding is protected from complete oxidation. The cladding coating involves the application of zirconium silicide onto Zr-based cladding. Zirconium silicide coating is expected to produce a glassy layer that becomes more protective at elevated temperature. For this reason, silicide coatings on cladding offer the potential for improved reliability at normal operating temperatures and at the higher transient temperatures encountered during accidents. Although ceramic coatings are brittle and may have weak points to be used as coating materials, several ceramic coatings were successful and showed adherent behavior and high resistance to oxidation. In this study, the oxidation behavior of zirconium silicide and its oxidation kinetics are analyzed. Zirconium silicide is a new suggested material to be used as coatings on existing Zr-based cladding alloys, the aim of this study is to evaluate if zirconium silicide is applicable to be used, so they can be more rapidly developed using existing cladding technology with some modifications. These silicide coatings are an attractive alternative to the use of coatings on zirconium claddings or to the lengthy development of monolithic ceramic or ceramic composite claddings and coatings

Investigation of holmium-doped zirconium oxide ceramic phosphor as an ultraviolet wavelength-discriminating laser beam viewer

Science.gov (United States)

Yamanoi, Kohei; Hori, Tatsuhiro; Minami, Yuki; Empizo, Melvin John F.; Luong, Mui Viet; Shiro, Atsushi; Watanabe, Jun; Iwano, Keisuke; Iwasa, Yuki; Cadatal-Raduban, Marilou; Gabayno, Jacque Lynn; Shimizu, Toshihiko; Sarukura, Nobuhiko; Norimatsu, Takayoshi

2018-01-01

We report the fluorescence spectra of ZrO2 and trivalent Ho-doped ZrO2 ceramics under ultraviolet (UV) excitation at 213, 266, and 355 nm wavelengths. The Ho3+-doped ZrO2 ceramics exhibited varying fluorescence color tones depending on the excitation wavelength used. The different color tones match the fluorescence spectrum characteristics at each excitation wavelength. Our results demonstrate that Ho3+-doped ZrO2 ceramics can discriminate between UV light, specifically the third, fourth, and fifth harmonics of a Nd:YAG laser. It can potentially be used for developing UV laser beam viewers to aid laser alignment.

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.

Synthesis of ZrB{sub 2}-SiC ceramic composites from a single-source precursor

Energy Technology Data Exchange (ETDEWEB)

Arish, Dasan, E-mail: arishd@rediffmail.com [Université of Limoges, SPCTS-CNRS, UMR 7315, Centre Européen de la Céramique (CEC), 12 Rue Atlantis, F-87068, Limoges Cedex (France); Shiju, Chellan [Synthetic Products Division, Corporate R & D Center (CRDC), HLL Lifecare Limited, Thiruvananthapuram, Kerala (India); Joseyphus, Raphael Selwin, E-mail: rsjoseyphus@gmail.com [PG & Research, Department of Chemistry, Mar Ivanios College (Autonomous), Thiruvananthapuram, 695015, Kerala (India); Pushparajan, Joseph [Travancore Titanium Products Ltd., Kochuveli, Thiruvananthapuram, 695021, Kerala (India)

2017-06-15

Preceramic polymer zirconoborosiloxane was synthesized from the reaction with boric acid, diphenyldiethoxysilane and zirconium (IV) propoxide via solventless process. The thermogravimetric analysis of the polymer showed that ceramic yield as decomposition product at 900 °C was 71%. The pyrolysis of zirconoborosiloxane in an argon gas environment was investigated as standard pyrolytic process up to 1650 °C. Microstructure evolution of ceramic phases was made by means of Fourier transform infrared, Raman spectroscopy, X-ray diffraction and scanning electron microscope analysis. The results clearly demonstrated the pyrolysis products at 1650 °C consist of totally non-oxide ceramic phases of β-SiC, ZrB{sub 2} and free carbon. - Highlights: • Preceramic polymer zirconoborosiloxane was synthesized by non-aqueous solventless process. • Non-oxide ZrB{sub 2}-SiC composites could be obtained from the pyrolysed products at 1650 °C. • Free carbon content was identified by Raman spectroscopy.

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.

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.)

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)

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.

Properties and clinical application of zirconia bioceramics in medicine

Directory of Open Access Journals (Sweden)

Čedomir Oblak

2014-01-01

Full Text Available Background: A group of inorganic non-metal biomaterials, that are commonly used in clinical medicine to replace or repair tissues, can be classified as a bioceramics. This group includes bioactive glasses, glass-ceramics, hydroxy-apatite and some other calcium phosphates. In addition, some bio-inert engineering ceramics materials have become increasingly utilised, aluminum oxide, zirconium oxide and their composites being the most popular. With the developement of yttria stabilized tetragonal zirconium oxide ceramics (Y-TZP medical community received a high strength biomaterial that is currently a material of choice for the manufacturing of medical devices. Y-TZP ceramics is becoming also increasingly used in dental medicine, where frameworks are manufactured by the use of computer-assisted technology.Conclusions: The article describes the basic properties of zirconia oxide ceramics important for the use in clinical medicine; high strength and fracture toughness, biocompatibility and negligible radiation. The ageing issue of this particular material, which is attributable to the thermo-dynamical instability of tetragonal zirconium oxide in hydrothermal conditions, is also discussed. When exposed to an aqueous environment over long periods of time, the surface of the Y-TZP ceramic will start transforming spontaneously into the monoclinic structure. The mechanism leading to the t-m transformation is temperature-dependent and is accompanied by extensive micro-cracking, which ultimately leads to strength degradation. The degradation might influence the clinical success rate of medical devices and therefore Y-TZP femoral heads are no longer made of pure zirconium oxide. Composites of zirconium and aluminium oxides are used instead, that are currently the strongest ceramic materials used in clinical medicine. In this work the clinical application of zirconia oxide ceramics in dental medicine is also presented. Conventional porcelain fused to metal

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.

Microstructure of lead zirconium titanate (PZT) by electron microscopy

International Nuclear Information System (INIS)

Bursill, L.A.; Peng JuLin

1989-01-01

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

Ceramic media amended with metal oxide for the capture of viruses in drinking water.

Science.gov (United States)

Brown, J; Sobsey, M D

2009-04-01

Ceramic materials that can adsorb and/or inactivate viruses in water may find widespread application in low-tech drinking-water treatment technologies in developing countries, where porous ceramic filters and ceramic granular media filters are increasingly promoted for that purpose. We examined the adsorption and subsequent inactivation of bacteriophages MS2 and (phiX-174 on five ceramic media in batch adsorption studies to determine media suitability for use in a ceramic water filter application. The media examined were a kaolinitic ceramic medium and four kaolinitic ceramic media amended with iron or aluminium oxides that had been incorporated into the kaolinitic clays before firing. Batch adsorption tests indicate increased sorption and inactivation of surrogate viruses by media amended with Fe and Al oxide, with FeOOH-amended ceramic inactivating all bacteriophages up to 8 log10. Unmodified ceramic was a poor adsorbent of bacteriophages at less than 1 log10 adsorption-inactivation and high recovery of sorbed phages. These studies suggest that contact with ceramic media, modified with electropositive Fe or Al oxides, can reduce bacteriophages in waters to a greater extent than unmodified ceramic.

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

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

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

Chemical composition and morphology of oxidic ceramics at filtration of steel deoxidised by aluminium

Directory of Open Access Journals (Sweden)

J. Bažan

2009-10-01

Full Text Available Composition and morphology of filter ceramics were investigated during filtration of steel deoxidised by aluminium. Filtration was realized with use of filters based on oxidic ceramics Cr2O3, TiO2, SiO2, ZrO2, Al2O3, 3Al2O3•2SiO2 and MgO•Al2O3. It was established that change of interphase (coating occurs during filtration of steel on the surface of capillaries of ceramics, where content of basic oxidic component decreases. Loss of oxidic component in the coating is replaced by increase of oxides of manganese and iron and it is great extent inversely proportional to the value of Gibbs’ energy of oxide, which forms this initial basis of ceramics.

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.

Progress in the characterisation of structural oxide/oxide ceramic matrix composites fabricated by electrophoretic deposition (EPD)

Czech Academy of Sciences Publication Activity Database

Stoll, E.; Mahr, P.; Kruger, H. G.; Kern, H.; Dlouhý, Ivo; Boccaccini, A. R.

2006-01-01

Roč. 8, č. 4 (2006), s. 282-285 ISSN 1438-1656 R&D Projects: GA ČR(CZ) GA106/05/0495 Institutional research plan: CEZ:AV0Z20410507 Keywords : electorphoretic deposition * oxid/oxid ceramic matrix composites * flexural strength Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 1.402, year: 2006 http://www3.interscience.wiley.com/cgi-bin/jissue/112579545

Effect of Prior Exposure at Elevated Temperatures on Tensile Properties and Stress-Strain Behavior of Three Oxide/Oxide Ceramic Matrix Composites

Science.gov (United States)

2015-03-26

observations on the fracture surface using an optical microscope and SEM. 4 II. Background 2.1 Ceramics Ceramics are inorganic and nonmetallic... The original uses for ceramic were primarily decorative, until more utilitarian purposes were discovered. Pottery was developed around 9,000...OF THREE OXIDE/OXIDE CERAMIC MATRIX COMPOSITES THESIS Christopher J. Hull, Captain, USAF AFIT-ENY-MS-15-M-228 DEPARTMENT OF THE AIR FORCE

"A New Class of Creep Resistant Oxide/Oxide Ceramic Matrix Composites"

Energy Technology Data Exchange (ETDEWEB)

Dr. Mohit Jain, Dr. Ganesh Skandan, Prof. Roger Cannon, Rutgers University

2007-03-30

Despite recent progress in the development of SiC-SiC ceramic matrix composites (CMCs), their application in industrial gas turbines for distributed energy (DE) systems has been limited. The poor oxidation resistance of the non-oxide ceramics warrants the use of envrionmental barrier coatings (EBCs), which in turn lead to issues pertaining to life expectancy of the coatings. On the other hand, oxide/oxide CMCs are potential replacements, but their use has been limited until now due to the poor creep resistance at high temperatures, particularly above 1200 oC: the lack of a creep resistant matrix has been a major limiting factor. Using yttrium aluminum garnet (YAG) as the matrix material system, we have advanced the state-of-the-art in oxide/oxide CMCs by introducing innovations in both the structure and composition of the matrix material, thereby leading to high temperature matrix creep properties not achieved until now. An array of YAG-based powders with a unique set of particle characteristics were produced in-house and sintered to full density and compressive creep data was obtained. Aided in part by the composition and the microstructure, the creep rates were found to be two orders of magnitude smaller than the most creep resistant oxide fiber available commercially. Even after accounting for porosity and a smaller matrix grain size in a practical CMC component, the YAG-based matrix material was found to creep slower than the most creep resistant oxide fiber available commercially.

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)

Fatigue limit of polycrystalline zirconium oxide ceramics: Effect of grinding and low-temperature aging.

Science.gov (United States)

Pereira, G K R; Silvestri, T; Amaral, M; Rippe, M P; Kleverlaan, C J; Valandro, L F

2016-08-01

The following study aimed to evaluate the effect of grinding and low-temperature aging on the fatigue limit of Y-TZP ceramics for frameworks and monolithic restorations. Disc specimens from each ceramic material, Lava Frame (3M ESPE) and Zirlux FC (Ivoclar Vivadent) were manufactured according to ISO:6872-2008 and assigned in accordance with two factors: (1) "surface treatment"-without treatment (as-sintered, Ctrl), grinding with coarse diamond bur (181µm; Grinding); and (2) "low-temperature aging (LTD)" - presence and absence. Grinding was performed using a contra-angle handpiece under constant water-cooling. LTD was simulated in an autoclave at 134°C under 2-bar pressure for 20h. Mean flexural fatigue limits (20,000 cycles) were determined under sinusoidal loading using stair case approach. For Lava ceramic, it was observed a statistical increase after grinding procedure and different behavior after LTD stimuli (Ctrl

The Effect of adding pore formers on the microstructure of NiO-YSZ ceramic composite

International Nuclear Information System (INIS)

Silva, F.S.; Santos, F.S.; Medeiros, L.M.; Yoshito, W.K.; Lazar, D.R.R.; Ussui, V.

2011-01-01

The ceramic composite of nickel oxide (NiO) with zirconium stabilized with 8 mol% yttria (8-YSZ) is the most employed material for use as anode for solid oxide fuel cells (SOFC). The nickel oxide in the composite is reduced to metallic nickel and this result in a 15% of porosity although the porosity needed to a proper function of an anode is about 30%, demanding the use of a pore former. In this work, NiO-YSZ composite powders were synthesized by a combustion process with urea as fuel, and the effect of the addition of carbon black and corn and rice starch as pore former were investigated. Powders were pressed as cylindrical pellets, sintered at 1350 °C for 60 minutes and density were measured by an immersion method and microstructure were observed by scanning electron microscopy. Results showed that ceramic composite has homogeneous microstructure and pores have different morphology and size depending on the kind of the pore former employed. (author)

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)

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)

The use of metal alkoxides in the preparation of ceramic powders

International Nuclear Information System (INIS)

Chetcuti, A.M.; Woolfrey, J.L.

1982-01-01

The production of fine, chemically homogeneous and highly reactive powder is particularly desirable where the synthesis and fabrication of multicomponent ceramic systems, such as SYNROC, are concerned. To produce good sinterable material, a preparation technique that allows intimate mixing of all reacting species is desirable. Traditional routes for preparing fine powders have involved ball-milling metal oxides and spray-drying or flash-drying the resulting oxide slurries. The hydrolysis of metal alkoxides has been investigated as a technique to produce fine powders. The preparation of SYNROC B powder from alkoxides involves hydrolysing a mixture of titanium and zirconium alkoxides. The precipitated product is then blended with Al 3 + , Ba 2 + and Ca 2 + nitrate solution

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)

Plasma spraying of zirconium carbide – hafnium carbide – tungsten cermets

Czech Academy of Sciences Publication Activity Database

Brožek, Vlastimil; Ctibor, Pavel; Cheong, D.-I.; Yang, S.-H.

2009-01-01

Roč. 9, č. 1 (2009), s. 49-64 ISSN 1335-8987 Institutional research plan: CEZ:AV0Z20430508 Keywords : Plasma spraying * cermet coatings * microhardness * zirconium carbide * hafnium carbide * tungsten * water stabilized plasma Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass

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.

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

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

Oxygen transport by oxygen potential gradient in dense ceramic oxide membranes

Energy Technology Data Exchange (ETDEWEB)

Maiya, P.S.; Balachandran, U.; Dusek, J.T.; Mieville, R.L. [Argonne National Lab., IL (United States). Energy Technology Div.; Kleefisch, M.S.; Udovich, C.A. [Amoco Exploration/Production, Naperville, IL (United States)

1996-05-01

Numerous studies have been conducted in recent years on the partial oxidation of methane to synthesis gas (syngas: CO + H{sub 2}) with air as the oxidant. In partial oxidation, a mixed-oxide ceramic membrane selectively transports oxygen from the air; this transport is driven by the oxygen potential gradient. Of the several ceramic materials the authors have tested, a mixed oxide based on the Sr-Fe-Co-O system has been found to be very attractive. Extensive oxygen permeability data have been obtained for this material in methane conversion experiments carried out in a reactor. The data have been analyzed by a transport equation based on the phenomenological theory of diffusion under oxygen potential gradients. Thermodynamic calculations were used to estimate the driving force for the transport of oxygen ions. The results show that the transport equation deduced from the literature describes the permeability data reasonably well and can be used to determine the diffusion coefficients and the associated activation energy of oxygen ions in the ceramic membrane material.

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

Nano-oxides to improve the surface properties of ceramic tiles

International Nuclear Information System (INIS)

Rambaldi, E.; Tucci, A.; Esposito, L.; Naldi, D.; Timellini, G.

2010-01-01

The aim of the present work is to realise ceramic tiles with superior surface mechanical characteristics and chemical resistance, by the addition of nano-oxides, such as zirconia and alumina, since such advanced ceramics oxides are well known for their excellent mechanical properties and good resistance to chemical etching. In order to avoid any dangerousness, the nanoparticles were used in form of aqueous suspension and they were sprayed, by airbrush, directly onto the dried ceramic support, before firing. To observe the distribution of the nanoparticles and to optimise the surface treatment, SEM-EDS analyses were carried out on the fired samples. XRD analysis was conducted to assess the phases evolution of the different materials during the firing step. The surface mechanical characteristics of the samples have been evaluated by Vickers hardness and scratch test. In addition, also chemical resistance tests were performed. Microstructural observations allowed to understand how alumina and zirconia nanoparticles acted to improve the surface performances of the modified ceramic tiles. (Author) 20 refs.

Production of superconducting ceramic oxides by coprecipitation

International Nuclear Information System (INIS)

Bizaio, L.R.; Lima, M.A.F. de; Figueiredo Jardim, R.de; Pinheiro, E.A.; Galembeck, F.

1988-01-01

An alternative method for production of ceramic oxides is described. The method consist in the coprecipitation reaction of metallic ions with oxalic acid. The obtainment samples present additional phases characterized by X-rays and optical microscopy. (C.G.C.) [pt

Development of low-expansion ceramics with strength retention to elevated temperatures. Final report

Energy Technology Data Exchange (ETDEWEB)

Hirschfeld, D.A.; Brown, J.J. Jr. [Virginia Polytechnic Inst. and State Univ., Blacksburg, VA (United States)

1994-09-01

The development of advanced engines has resulted in the need for new ceramic compositions which exhibit thermo-mechanical properties suitable for the engine environment, e.g., low thermal expansion, stability to 1,200 C, and thermal shock resistance. To meet these goals, a two phase research program was instituted. In the first phase, new oxide ceramics were identified in the AlPO{sub 4}-{beta}-eucryptite, {beta}-cristobalite, mullite and zircon systems. This research focused on screening and property characterization of ceramics in the four systems. The most promising compositions in the AlPO{sub 4}-{beta}-eucryptite and zircon systems were then further evaluated and developed in the second phase with the goal of being ready for prototype testing in actual engines. Of the compositions, calcium magnesium zirconium phosphate (zircon system) exhibits the most desirable properties and is presently being developed for commercialization.

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

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.

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

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

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.)

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.

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.

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

Preparation and Microstructure of Porous ZrB2 Ceramics Using Reactive Spark Plasma Sintering Method

Institute of Scientific and Technical Information of China (English)

YUAN Huiping; LI Junguo; SHEN Qiang; ZHANG Lianmeng

2015-01-01

Zirconium oxide (ZrO2) and boron carbide (B4C) were added to ZrB2 raw powders to prepare ZrB2 porous ceramics by reactive spark plasma sintering (RSPS). The reactions between ZrO2 and B4C which produce ZrB2 and gas (such as CO and B2O3) result in pore formation. X-Ray Diffraction results indicated that the products phase was ZrB2 and the reaction was completed after the RSPS process. The porosity could be controlled by changing the ratio of synthesized ZrB2 to raw ZrB2 powders. The porosity of porous ceramics with 20 wt% and 40 wt% synthsized ZrB2 are 0.185 and 0.222, respectivly. And dense ZrB2-SiC ceramic with a porosity of 0.057 was prepared under the same conditions for comparison. The pores were homogeneously distributed within the microstructure of the porous ceramics. The results indicate a promising method for preparing porous ZrB2-based ceramics.

TECHNOLOGICAL PECULIARITIES OF THERMAL BARRIER COATINGS BASED ON ZIRCONIUM DIOXIDE

Directory of Open Access Journals (Sweden)

V. V. Okovity

2016-01-01

Full Text Available A technology for formation of thermal barrier coatings (TBC based on zirconium dioxide has been developed in the paper. The paper investigates structures of phase composition and thermal stability of such developed coatings. Investigation results pertaining to formation of an oxide system ZrO2 – Y2O3, while using plasma spraying and subsequent high-energy processing, which allows to increase resistance of a thermal barrier coating to thermal cycling heat resistance of the coating at temperature of 1100 °C. This leads to longer protection of bottom layer against high-temperature exposure. The methodology is based on complex metallographic, X-ray diffraction and electron microscopy investigations of structural elements in composite plasma coatings of the ZrO2 – Y2O system. Resistance of plasma coatings (Мe – Cr – Al – Y/ZrO2 – Y2O3-type, used as TBC to protect gas turbine engine blades under conditions of frequent thermal cyclings is limited by cleavage of an outer ceramic layer. Structural and electron microprobe investigations have shown that as a result of thermal cycling an outer atmosphere due to porous structure of the ceramic coating layer, migrates to the surface of lower metal coating, causing its oxidation. As a result, the metal-ceramic Al2O3 layer is formed at a metal-ceramic interface and it changes a stress state of the coating that causes a reduction of protective properties. Thus, a high heat resistance of thermal barrier coatings depends on processes occurring at the interface between metal and ceramic coating layers. A laser impact on samples with TBC leads to changes in the structure of the oxide layer of ZrO2 – Y2O3. In this case its initial surface characterized by considerable relief is significantly flattened due to processing and the coating is fractured and it is separated in fragments. As the oxide coating has low thermal conductivity, and the time of laser exposure is about 10–3 sec, a heat flux

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

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.

Reduction-oxidation Enabled Glass-ceramics to Stainless Steel Bonding Part II interfacial bonding analysis

Energy Technology Data Exchange (ETDEWEB)

Dai, Steve Xunhu [Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

2015-09-01

Among glass-ceramic compositions modified with a variety of oxidants (AgO, FeO, NiO, PbO, SnO, CuO, CoO, MoO₃ and WO₃) only CuO and CoO doped glass-ceramics showed existence of bonding oxides through reduction-oxidation (redox) at the GC-SS interface. The CuO-modified glass-ceramics demonstrate the formation of a continuous layer of strong bonding Cr₂O₃ at the interface in low partial oxygen (PO₂) atmosphere. However, in a local reducing atmosphere, the CuO is preferentially reduced at the surface of glass-ceramic rather than the GC-SS interface for redox. The CoO-modified glass-ceramics demonstrate improved GC-SS bonding. But the low mobility of Co⁺⁺ ions in the GC limited the amount of CoO that can diffuse to and participate in redox at the interface.

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

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

Processing of porous zirconia ceramics by direct consolidation with starch

International Nuclear Information System (INIS)

Garrido, Liliana B; Albano, Maria P

2008-01-01

Porous ceramics are used especially for those environments with high temperatures, heavy wear and in a corrosive medium. Zirconium-based materials are useful for such applications as sensors, filters, support for catalytic reactions, porous components for sofc and in biomedical applications. A conventional method for producing porous ceramics consists of the addition and later decomposition by calcination (pyrolisis) of different organic materials that act as pore formers. Several wet processing possibilities have been developed. Among these is a technique of direct consolidation with starch. This process begins with the preparation of an aqueous suspension of the ceramic with the dispersants needed to stabilize it, to which the starch is added. After casting in a waterproof mold, the suspension thermally hardens into the desired shape. The dry compacts undergo the sintering cycle to obtain pieces almost in their final form. This study aims to optimize the processing of porous zirconium ceramics using starch as a pore and binder forming agent. Zirconium with 3% yttrium molar stabilized in tetragonal phase was used. The aqueous suspensions (52-55% vol) of the zirconium-starch mixtures with different compositions were stabilized with a commercial solution of ammonium polyacrylate as a dispersant and were hardened in plastic molds at 90 o C for 30 min. The influence of added volume of starch on the physical characteristics of the pieces in green state was established while maintaining the temperature, the gelling time and the conditions of constant drying. The sintering was carried out at 1000-1500 o C-2h. The characteristics of the sintered product were evaluated by measuring density, volumetric contraction, intrusion of Hg and the evolution of the crystalline phases by X-ray diffraction (XRD) and scanning electron microscopy (SEM). The microstructural properties of ceramic (pore volume, the relation between open and closed porosity, size distribution, morphology of

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)

Piezoelectric displacement in ceramics

International Nuclear Information System (INIS)

Stewart, M.; Cain, M.; Gee, M.

1999-01-01

This Good Practice Guide is intended to aid a user to perform displacement measurements on piezoelectric ceramic materials such as PZT (lead zirconium titanate) in either monolithic or multilayer form. The various measurement issues that the user must consider are addressed, and good measurement practise is described for the four most suitable methods. (author)

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

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)

Anisotropy oxidation of textured ZrB₂–MoSi₂ ceramics

DEFF Research Database (Denmark)

Liu, Hai-Tao; Zou, Ji; Ni, De Wei

2012-01-01

Oxidation behavior of hot forged textured ZrB2–20vol% MoSi2 ceramics with platelet ZrB2 grains was investigated at 1500°C for exposure time from 0.5 to 12h. Compared to untextured ceramics, the textured ceramics showed obvious anisotropic oxidation behavior and the surface normal to the hot forgi...

Oxidation behaviour of Zr-Ce alloys. Kinetic and microstructure aspects

International Nuclear Information System (INIS)

Rouillon, Ludovic

1996-01-01

As Zircaloy alloys are used for fuel rods in pressurized water nuclear reactors, this research thesis aims at studying and improving corrosion resistance of zirconium alloys while maintaining their mechanical properties. It more precisely deals with the kinetic and microstructure aspects of the external corrosion of the cladding by the coolant. In the case of Zircaloys, this corrosion is characterized by a kinetic transition from an initially parabolic to a linear regime. This research aims at intervening on this transition by elaborating zirconium alloys containing an element which stabilizes zirconia, in this case cerium. After having reported a bibliographical study on sheath oxidation, on parameters which influence sheath oxidation kinetics, on zirconia stabilization by doping elements, on the interest of lanthanide oxides, the author reports a feasibility study on the use of cerium (choice and preparation, sintered ceramic characterization, annealing of stabilized zirconia), reports a metallurgical study of Zr-Ce alloys, reports the study of the oxidation behaviour of these alloys (in autoclave, in presence of oxygen, under oxygen and then water) and the characterization of the microstructures of the oxide layers. He finally discusses the relationship between microstructure and oxidation kinetics, the role of cerium in the oxidation process, and the role of water in the oxidation process [fr

Dielectric silicone elastomers with mixed ceramic nanoparticles

International Nuclear Information System (INIS)

Stiubianu, George; Bele, Adrian; Cazacu, Maria; Racles, Carmen; Vlad, Stelian; Ignat, Mircea

2015-01-01

Highlights: • Composite ceramics nanoparticles (MCN) with zirconium dioxide and lead zirconate. • Dielectric elastomer films wDith PDMS matrix and MCN as dielectric filler. • Hydrophobic character—water resistant and good flexibility specific to siloxanes. • Increased value of dielectric constant with the content of MCN in dielectric films. • Increased energy output from uniaxial deformation of the dielectric elastomer films. - Abstract: A ceramic material consisting in a zirconium dioxide-lead zirconate mixture has been obtained by precipitation method, its composition being proved by wide angle X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The average diameter of the ceramic particles ranged between 50 and 100 nm, as revealed by transmission electron microscopy images. These were surface treated and used as filler for a high molecular mass polydimethylsiloxane-α,ω-diol (Mn = 450,000) prepared in laboratory, the resulted composites being further processed as films and crosslinked. A condensation procedure, unusual for polydimethylsiloxane having such high molecular mass, with a trifunctional silane was approached for the crosslinking. The effect of filler content on electrical and mechanical properties of the resulted materials was studied and it was found that the dielectric permittivity of nanocomposites increased in line with the concentration of ceramic nanoparticles

Dielectric silicone elastomers with mixed ceramic nanoparticles

Energy Technology Data Exchange (ETDEWEB)

Stiubianu, George, E-mail: george.stiubianu@icmpp.ro [“Petru Poni” Institute of Macromolecular Chemistry, Aleea Gr. Ghica Voda 41A, Iasi 700487 (Romania); Bele, Adrian; Cazacu, Maria; Racles, Carmen; Vlad, Stelian [“Petru Poni” Institute of Macromolecular Chemistry, Aleea Gr. Ghica Voda 41A, Iasi 700487 (Romania); Ignat, Mircea [National R& D Institute for Electrical Engineering ICPE-CA Bucharest, Splaiul Unirii 313, District 3, Bucharest 030138 (Romania)

2015-11-15

Highlights: • Composite ceramics nanoparticles (MCN) with zirconium dioxide and lead zirconate. • Dielectric elastomer films wDith PDMS matrix and MCN as dielectric filler. • Hydrophobic character—water resistant and good flexibility specific to siloxanes. • Increased value of dielectric constant with the content of MCN in dielectric films. • Increased energy output from uniaxial deformation of the dielectric elastomer films. - Abstract: A ceramic material consisting in a zirconium dioxide-lead zirconate mixture has been obtained by precipitation method, its composition being proved by wide angle X-ray powder diffraction and energy-dispersive X-ray spectroscopy. The average diameter of the ceramic particles ranged between 50 and 100 nm, as revealed by transmission electron microscopy images. These were surface treated and used as filler for a high molecular mass polydimethylsiloxane-α,ω-diol (Mn = 450,000) prepared in laboratory, the resulted composites being further processed as films and crosslinked. A condensation procedure, unusual for polydimethylsiloxane having such high molecular mass, with a trifunctional silane was approached for the crosslinking. The effect of filler content on electrical and mechanical properties of the resulted materials was studied and it was found that the dielectric permittivity of nanocomposites increased in line with the concentration of ceramic nanoparticles.

Kinetics of the oxidation of Ba2YCu3O/sub x/ ceramics

International Nuclear Information System (INIS)

O'Bryan, H.M.; Gallagher, P.K.

1988-01-01

The kinetics of the oxidation of dense and porous samples of Ba 2 YCu 3 O/sub x/ ceramic have been determined by gravimetric analysis at 400--700 0 C. At 600 0 C and above, the rate decreases as the thickness of the oxidized layer increases. At 500 0 C and below, the kinetics show a linear relation that indicates that the oxidized layer does not protect the ceramic. Dilatometric, microscopic, and high-temperature x-ray data suggest that fractures in the oxide layer at the lower temperatures are caused by the large volume decrease that accompanies the change in oxygen stoichiometry

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.

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)

Encapsulation of sacrificial silicon containing particles for SH oxide ceramics via a boehmite precursor route

NARCIS (Netherlands)

Carabat, A.L.; Van der Zwaag, S.; Sloof, W.G.

2013-01-01

Easy crack propagation in oxide ceramic coatings limits their application in high temperature environment (e.g. such as engines and gas turbine components) [1]. In order to overcome this problem, incorporation of sacrificial particles into an oxide ceramic coating may be a viable option. Particles

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

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)

Investigation of the thermophysical properties of oxide ceramic materials at liquid-helium temperatures

International Nuclear Information System (INIS)

Taranov, A. V.; Khazanov, E. N.

2008-01-01

The main regularities in the transport of thermal phonons in oxide ceramic materials are investigated at liquid-helium temperatures. The dependences of the thermophysical characteristics of ceramic materials on their structural parameters (such as the grain size R, the grain boundary thickness d, and the structure of grain boundaries) are analyzed. It is demonstrated that, in dense coarse-grained ceramic materials with qR>>1 (where q is the phonon wave vector), the grain boundaries and the grain size are the main factors responsible for the thermophysical characteristics of the material at liquid-helium temperatures. A comparative analysis of the thermophysical characteristics of optically transparent ceramic materials based on the Y 3 Al 5 O 12 (YAG) and Y 2 O 3 cubic oxides synthesized under different technological conditions is performed using the proposed criterion

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.

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.

passive and active measurements for some ceramic samples

International Nuclear Information System (INIS)

Hassan, M.F.; Said, S.A.; Ali, M.A.; Szegedi, S.

2004-01-01

passive measurements for an imported natural ore (zirconium silicate) used in ceramic industries were carried out to identify its radioactivity . this work was done for ceramic quality control purposes. accurate gamma spectrometers with 30% and 70% detector efficiencies were used in the measurements. the 235 U, 238 U and 232 Th radioactivity were determined . for the sake of comparison already manufactured different ceramic samples were investigated applying fast neutrons activation analysis (FNAA) and X-Ray florescence (XRF) techniques. the obtained results were discussed with the tabulated international radioactivity levels for building materials

Synthesis and characterization of nickel oxide doped barium strontium titanate ceramics

Energy Technology Data Exchange (ETDEWEB)

Banerjee, M. [Dept. of Electrical Engineering, Bengal Institute of Technology Kolkata (India); Mukherjee, S. [Dept. of Metallurgical Engineering, Jadavpur University, Kolkata (India); Maitra, S. [Govt. College of Engg. and Ceramic Technology, Kolkata (India)

2012-01-15

Barium strontium titanate (BST) ceramics (Ba{sub 0.6}Sr{sub 0.4})TiO{sub 3} were synthesized by solid state sintering using barium carbonate, strontium carbonate and rutile as the precursor materials. The samples were doped with nickel oxide in different proportions. Different phases present in the sintered samples were determined from X-ray diffraction investigation and the distribution of different phases in the microstructure was assessed from scanning electron microscopy study. It was observed that the dielectric properties of BST were modified significantly with nickel oxide doping. These ceramics held promise for applications in tuned circuits. (author)

Structural and functional characterization of barium zirconium titanate / epoxy composites

Directory of Open Access Journals (Sweden)

Filiberto González Garcia

2011-12-01

Full Text Available The dielectric behavior of composite materials (barium zirconium titanate / epoxy system was analyzed as a function of ceramic concentration. Structure and morphologic behavior of the composites was investigated by X-ray Diffraction (XRD, Fourier transformed infrared spectroscopy (FT-IR, Raman spectroscopy, field emission scanning electron microscopy (FE-SEM and transmission electron microscopy (TEM analyses. Composites were prepared by mixing the components and pouring them into suitable moulds. It was demonstrated that the amount of inorganic phase affects the morphology of the presented composites. XRD revealed the presence of a single phase while Raman scattering confirmed structural transitions as a function of ceramic concentration. Changes in the ceramic concentration affected Raman modes and the distribution of particles along into in epoxy matrix. Dielectric permittivity and dielectric losses were influenced by filler concentration.

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

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

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

Method of depositing thin films of high temperature Bi-Sr-Ca-Cu-O-based ceramic oxide superconductors

International Nuclear Information System (INIS)

Budd, K.D.

1991-01-01

This patent describes a method. It comprises preparing a liquid precursor of a Bi-Sr-Ca-Cu-O- based ceramic oxide superconductor phase, wherein the liquid precursor comprises an alkoxyalkanol, copper acrylate, strontium acrylate, bismuth nitrate, and calcium nitrate, wherein the liquid precursor has a cation ratio sufficient to form the desired stoichiometry in the ceramic oxide superconductor phase when the liquid precursor is heated to a temperature and for a time sufficient to provide the desired ceramic oxide superconductor phase, and wherein the copper acrylate, strontium acrylate, bismuth nitrate, and calcium nitrate are mutually soluble in the alkoxyalkanol; applying the liquid precursor to a substrate, wherein the substrate is one of an oxide ceramic, a metal selected from the group consisting of Ag and Ni, and Si; and heating the substrate in an oxygen-containing atmosphere with the liquid precursor applied thereon to a temperature and for a time sufficient to form a thin film comprising at least one Bi-Sr- Ca-Cu-O-based high temperature ceramic oxide superconductor phase

Laser-joined Al{sub 2}O{sub 3} and ZrO{sub 2} ceramics for high-temperature applications

Energy Technology Data Exchange (ETDEWEB)

Boerner, Floriana-Dana, E-mail: floriana.boerner@tu-dresden.d [Dresden University of Technology (TU Dresden), Institute of Power Engineering, Chair of Hydrogen Technology and Nuclear Power Engineering, George-Baehr-Str. 3, D-01062 Dresden (Germany); Lippmann, Wolfgang, E-mail: wolfgang.lippmann@tu-dresden.d [Dresden University of Technology (TU Dresden), Institute of Power Engineering, Chair of Hydrogen Technology and Nuclear Power Engineering, George-Baehr-Str. 3, D-01062 Dresden (Germany); Hurtado, Antonio, E-mail: antonio.hurtado@tu-dresden.d [Dresden University of Technology (TU Dresden), Institute of Power Engineering, Chair of Hydrogen Technology and Nuclear Power Engineering, George-Baehr-Str. 3, D-01062 Dresden (Germany)

2010-10-01

A laser process is presented that has been specially developed for joining oxide ceramics such as zirconium oxide (ZrO{sub 2}) and aluminium oxide (Al{sub 2}O{sub 3}). It details, by way of example, the design of the laser process applied for to producing both Al{sub 2}O{sub 3}-Al{sub 2}O{sub 3} and ZrO{sub 2}-ZrO{sub 2} joints using siliceous glasses as fillers. The heat source used was a continuous wave diode laser with a wavelength range of 808-1010 nm. Glasses of the SiO{sub 2}-Al{sub 2}O{sub 3}-B{sub 2}O{sub 3}-MeO system were developed as high-temperature resistant brazing fillers whose expansion coefficients, in particular, were optimally adapted to those of the ceramics to be joined. Specially designed measuring devices help to determine both the temperature-dependent emission coefficients and the synchronously determined proportions of reflection and transmission. The glass-ceramic joints produced are free from gas inclusions and macroscopic defects and exhibit a homogenous structure. The average strength values achieved were 158 MPa for the Al{sub 2}O{sub 3} system and 190 MPa for the ZrO{sub 2} system, respectively.

Surface oxidation of porous ZrB2-SiC ceramic composites by continuous-wave ytterbium fibre laser

International Nuclear Information System (INIS)

Mahmod, Dayang Salyani Abang; Glandut, Nicolas; Khan, Amir Azam; Labbe, Jean-Claude

2015-01-01

Highlights: • Surface oxidation of ZrB 2 -SiC ceramic composites by Yb-fibre laser. • Round spiral laser pattern created for the surface oxidation. • Presence of laser-formed oxide scale and unaffected beneath regions. • Crazed but uncracked surface oxide. • A dense glassy SiO 2 -rich layer exhibited enhances oxidation resistance. - Abstract: Surface treatment of ceramic substrates by a laser beam can allow to incorporate interesting properties to these ceramics. In the present work, surface oxidation of ca. 30% porous ZrB 2 -SiC ceramic composites by using an ytterbium fibre laser was conducted. Oxidation of ceramic substrates through this process under ambient conditions has certain advantages compared to the classical oxidation method. A particular spiral laser pattern was created in order to produce an oxidized structure on ZrB 2 -SiC porous substrates. The laser parameters were as follows i.e., laser power of 50, 60 and 70 W, a beam diameter of 1.25 mm, velocity of 2 mm/s, acceleration and deceleration of 1 mm/s 2 . The microstructural and morphological changes in the laser-treated region was examined using scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. At laser power of 70 W, the sample exhibits uniform oxidation. It revealed that the very porous bulk beneath remained unaffected and unoxidized because this laser-formed oxide scale protects the substrate from oxidation. The presence of oxidized and unaffected regions indicated a high degree of heat localization. The dense glassy SiO 2 -rich layer prevents the inward oxygen diffusion into the inner bulk hence enhances the oxidation resistance.

Occupational exposure to natural radioactivity in the zirconium mineral manufacturing industries

International Nuclear Information System (INIS)

Ballesteros, L.; Zarza, I.; Ortiz, J.; Serradell, V.

2006-01-01

The spanish 'Real Decatur 783/2001', published as result of the adaptation of the European Council directive 96/29/EURATOM (B.S.S. directive), regulates in Spain the use of natural radioactive substances. This decree establishes the need to study and control those activities in which significant increases of the exposure of workers or members of the public could take place. One of these natural radioactive substances are zirconium minerals. They are widely employed in some industrial activities, such as the production of zirconia and zirconium chemicals, glazed ceramic products manufacture, refractories, foundry sands (including investment casting) and zirconium mineral manufacturing. Its major end uses are fine ceramics where it acts as an opacifier in glazes and enamels and also as an additive in special glass (i.e. TV glass). This paper provides a description of a measurement campaign carried out to estimate the risk of occupational exposure to natural radioactivity in the zirconium mineral manufacturing industries. Zirconium raw sands have generally a granular size of 100 to 200 μm, which may be reduced to around 2 μm for use in ceramics and paint applications by milling to flour. These sands contain varying concentrations of natural radionuclides: 232 Th, 235 U, and mostly 238 U, together with their progenies. The first part of the study is to identify situations and areas where worker s are exposed to radiation. Five pathways of exposure were found: inhalation of dust, ingestion of dust, inhalation of radon, skin contamination and external irradiation. Samples from raw materials and from the environment at the work areas are performed; both where the zircon sands are unloaded and stored and at the milling area. Secondly, collected samples are analysed to evaluate activities on those natural radionuclides. Gamma spectrometry analysis is performed for the whole of the samples. For this purpose, a Ge-HP detector (high purity Ge detectors) is used. Dust samples

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.

Ablation-resistant carbide Zr0.8Ti0.2C0.74B0.26 for oxidizing environments up to 3,000 °C

Science.gov (United States)

Zeng, Yi; Wang, Dini; Xiong, Xiang; Zhang, Xun; Withers, Philip J.; Sun, Wei; Smith, Matthew; Bai, Mingwen; Xiao, Ping

2017-06-01

Ultra-high temperature ceramics are desirable for applications in the hypersonic vehicle, rockets, re-entry spacecraft and defence sectors, but few materials can currently satisfy the associated high temperature ablation requirements. Here we design and fabricate a carbide (Zr0.8Ti0.2C0.74B0.26) coating by reactive melt infiltration and pack cementation onto a C/C composite. It displays superior ablation resistance at temperatures from 2,000-3,000 °C, compared to existing ultra-high temperature ceramics (for example, a rate of material loss over 12 times better than conventional zirconium carbide at 2,500 °C). The carbide is a substitutional solid solution of Zr-Ti containing carbon vacancies that are randomly occupied by boron atoms. The sealing ability of the ceramic's oxides, slow oxygen diffusion and a dense and gradient distribution of ceramic result in much slower loss of protective oxide layers formed during ablation than other ceramic systems, leading to the superior ablation resistance.

Assessment of full ceramic solid oxide fuel cells based on modified strontium titanates

DEFF Research Database (Denmark)

Holtappels, Peter; Ramos, Tania; Sudireddy, Bhaskar Reddy

2014-01-01

stimulated the development for full ceramic anodes based on strontium titanates. Furthermore, the Ni-cermet is primarily a hydrogen oxidation electrode and efficiency losses might occur when operating on carbon containing fuels. In the European project SCOTAS-SOFC full ceramic cells comprising CGO...

Zirconium titanate: stability and thermal expansion; Titanato de circonio: estabilidad termodinamica y expansion termica

Energy Technology Data Exchange (ETDEWEB)

Lopez-Lopez, E.; Moreno, R.; Baudin, C.

2011-07-01

Zirconium titanate is a well known compound in the field of electro ceramics, although it has also been used in catalyst and sensors applications. The crystallographic thermal expansion anisotropy of this compound makes it a potential candidate as constituent of structural components. In general, to assure the structural integrity and microstructural homogeneity of a ceramic piece, relatively low cooling rates from the fabrication temperature are required. This requirement is essential for zirconium titanate because thermal expansion as well as phase distribution is affected by small variations in the composition and cooling rate. This work reviews the available data on the phase equilibrium relationships in the systems ZrO{sub 2}-TiO{sub 2} and ZrO{sub 2}-TiO{sub 2}-Y{sub 2}O{sub 3}. The main discrepancies as well as the possible origins of them are discussed. Additionally, the crystallographic thermal expansion data in the current literature are reviewed. (Author) 56 refs.

Synthesis and characterization of a polyborosilazane/Cp2ZrCl2 hybrid precursor for the Si-B-C-N-Zr multinary ceramic.

Science.gov (United States)

Long, Xin; Shao, Changwei; Wang, Hao; Wang, Jun

2015-09-21

A novel zirconium-contained polyborosilazane (PBSZ-Zr) was synthesized by chemical modification of a liquid polyborosilazane (LPBSZ) with Cp2ZrCl2. A Si-B-C-N-Zr multinary ceramic was prepared via pyrolysis of PBSZ-Zr. The properties and the ceramization process of PBSZ-Zr, as well as the microstructural development and properties of the derived SiBCN-Zr ceramic, were well studied. The active Si-H and N-H groups in LPBSZ react with Zr-Cl in Cp2ZrCl2 to form PBSZ-Zr polymers. The Zr content of the SiBCN-Zr ceramic was 3.39 wt% when the weight ratio of Cp2ZrCl2 to LPBSZ was 20 : 100. The SiBCN-Zr ceramic remains amorphous when pyrolyzed below 1600 °C, but the crystal phases of Zr2CN, ZrC, BN, SiC, and Si3N4 were detected from a 1600 °C treated sample. Due to the low activity of free carbon at the interface of the SiBCN-Zr ceramic, the oxidation resistance of the SiBCN-Zr ceramic under air was improved compared with the SiBCN ceramic.

Highly porous ceramic oxide aerogels having improved flexibility

Science.gov (United States)

Meador, Mary Ann B. (Inventor); Nguyen, Baochau N. (Inventor); Guo, Haiquan (Inventor)

2012-01-01

Ceramic oxide aerogels having improved flexibility are disclosed. Preferred embodiments exhibit high modulus and other strength properties despite their improved flexibility. The gels may be polymer cross-linked via organic polymer chains to further improve strength properties, without substantially detracting from the improved flexibility. Methods of making such aerogels are also disclosed.

Deposition of Crystalline Hydroxyapatite Nanoparticles on Y-TZP Ceramic: A Potential Solution to Enhance Bonding Characteristics of Y-TZP Ceramics

Directory of Open Access Journals (Sweden)

Abbas Azari

2017-08-01

Full Text Available Objectives: Many advantages have been attributed to dental zirconia ceramics in terms of mechanical and physical properties; however, the bonding ability of this material to dental structure and/or veneering ceramics has always been a matter of concern. On the other hand, hydroxyapatite (HA shows excellent biocompatibility and good bonding ability to tooth structure, with mechanically unstable and brittle characteristics, that make it clinically unacceptable for use in high stress bearing areas. The main purpose of this study was to introduce two simple yet practical methods to deposit the crystalline HA nanoparticles on zirconia ceramics. Materials and Methods: zirconia blocks were treated with HA via two different deposition methods namely thermal coating and air abrasion. Specimens were analyzed by scanning electron microscopy, energy dispersive spectroscopy (EDS and X-ray diffraction (XRD.Results: In both groups, the deposition techniques used were successfully accomplished, while the substrate showed no structural change. However, thermal coating group showed a uniform deposition of crystalline HA but in air abrasion method, there were dispersed thin islands of HA.Conclusions: Thermal coating method has the potential to significantly alter the surface characteristics of zirconia. The simple yet practical nature of the proposed method may be able to shift the bonding paradigm of dental zirconia ceramics. This latter subject needs to be addressed in future investigations.Keywords: Zirconium Oxide; Hydroxyapatites; Dental Bonding; Microscopy, Electron, Scanning; X-Ray Diffraction; Spectrometry, X-Ray Emission

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

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

Corrosion behaviour of porous chromium carbide/oxide based ceramics in supercritical water

International Nuclear Information System (INIS)

Dong, Z.; Xin, T.; Chen, W.; Zheng, W.; Guzonas, D.

2011-01-01

Porous chromium carbide with a high density of open pores was fabricated by a reactive sintering method. Chromium oxide ceramics were obtained by re-oxidizing the porous chromium carbides formed. Some samples were added with yttria at 5 wt. %, prior to reactive sintering to form porous structures. Corrosion tests in SCW were performed at temperatures ranging from 375 o C to 625 o C with a fixed pressure at around 25∼30 MPa. The results show that chromium carbide is stable in SCW environments at temperatures up to 425 o C, above which disintegration of carbides through oxidation occurs. Porous chromium oxide samples show better corrosion resistance than porous chromium carbide, but disintegrate in SCW at around 625 o C. Among all the samples tested, chromium oxide ceramics with added yttria exhibited much better corrosion resistance compared with the pure chromium carbide/oxides. No evidence of weight change or disintegration of porous chromium oxides with 5 wt % added yttria was observed after exposure at 625 o C in SCW for 600 hours. (author)

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.

Morphological characterization of ceramic fillers made from Indonesian natural sand as restorative dental materials

Science.gov (United States)

Karlina, E.; Susra, S.; Fatmala, Y.; Hartoyo, H. M.; Takarini, V.; Usri, K.; Febrida, R.; Djustiana, N.; Panatarani, C.; Joni, I. M.

2018-02-01

Dental composite as restorative dental materials can be reinforced using ceramic fillers. Homogeneous distribution of filler particles shall improve its mechanical properties. This paper presents the results of the preliminary study on the ZrO2-Al2O3-SiO2 ceramic fillers made from Indonesian natural sand that can increase the mechanical properties of dental composite. The synthesis was done using zirconium silicate sand (ZrSiO4) and aluminium oxide (Al2O3) precursors, which dissolved together with 70:30 weight ratios. Two types of sand were used: (1) manufactured sand (mesh #80) and (2) natural sand (mesh #400). The samples then heated in the furnace at 1100 °C for 8 hours. The morphological characterization was then evaluated using JEOL Scanning Electron Microscope (SEM) for the surface structure that analyze particles size and distribution. Ceramic fillers made from natural sand is homogenous, well distributed with average particle size of 5-10 µm. Comparably, ceramic filler made from the manufactured sand is heterogeneous, poorly distributed and appear as agglomerates with average particle size are 30-50 µm. The results suggest that ceramic fillers made from natural sand demonstrate better character to represent as a functional restorative dental material.

Bond strength between zirconium ceramic and dual resinous cement

Directory of Open Access Journals (Sweden)

João Galan Junior

2010-04-01

Full Text Available Objective: To assess the influence of different surface treatments on the bond strength between the resinous cement Panavia F (Kuraray Co. Ltd., Osaka, Japan and the structure of In-Ceram YZ (Vita Zahnfabrik, Bad Säckingen, Germany. Methods: Fifteen ceramic blocks were assessed: Group 1, finishing with abrasive paper; Group 2, finishing, airborne Al2O3 particle abrasion and silanization; Group 3, finishing, airborne particle abrasion, silicatization and silanization. After treatment, the blocks received cementation of resin composite cylinders with Panavia F (Kuraray Co. Ltd., Osaka, Japan and were submitted to the shear bond strength test in a universal testing machine. Results: The results were statistically analyzed (ANOVA and multiple comparison Student-Newman-Keuls test: Group 1 (9.66 ± 1.67 MPa < Group 2 (16.61 ± 3.38 MPa = Group 3 (19.23 ± 5.69 MPa, with p = 0.007. Conclusion: The structures of the In-Ceram YZ system (Vita Zahnfabrik, Bad Säckingen, Germany associated with Panavia F (Kuraray Co. Ltd., Osaka, Japan require previous etching to achieve greater bond strength between the ceramic and cement, and this treatment may be performed with airborne particle abrasion I or traditional silicatization, both followed by silanization.

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.)

Microcracking in ceramics and acoustic emission

International Nuclear Information System (INIS)

Subbarao, E.C.

1991-01-01

One of the limitations in the use of ceramics in critical applications is due to the presence of microcracks, which may arise from differential thermal expansion and phase changes, among others. Acoustic emission signals occur when there are abrupt microdeformations in a material and thus offer a convenient means of non-destructive detection of microcracking. Examples of a study of acoustic emission from microcracking due to anisotropic thermal expansion in low thermal expansion single phase ceramics such as niobia and sodium zirconium phosphate ceramics and due to phase changes in zirconia and superconducting YBa 2 Cu 3 Osub(7-x) ceramics are presented, together with the case of lead titanate ceramics, which exhibits both a phase change (paraelectric to ferroelectric) and an anisotropic thermal expansion. The role of grain size on the extent of microcracking is illustrated in the case of niobia ceramics. Some indirect evidence of healing of microcracks on heating niobia and lead titanate ceramics is presented from the acoustic emission results. (author). 69 refs., 9 figs

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

Study of aluminium oxide from high-alumina refractory ceramics by ...

Indian Academy of Sciences (India)

Wintec

Keywords. Ceramics; aluminium oxide; X-ray diffraction; scanning electron microscopy; thermolumi- nescence. ... and ruby, consists of a slightly distorted hexagonal O. 2– .... a very complex structure consisting of a broad distribu- .... Imax (a.u.).

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

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.

Surface oxidation of porous ZrB{sub 2}-SiC ceramic composites by continuous-wave ytterbium fibre laser

Energy Technology Data Exchange (ETDEWEB)

Mahmod, Dayang Salyani Abang, E-mail: dygsalyani@gmail.com [Department of Mechanical and Manufacturing Engineering, Faculty of Engineering, Universiti Malaysia Sarawak, 94300 Kota Samarahan, Sarawak (Malaysia); Glandut, Nicolas [SPCTS, UMR 7315, CNRS, University of Limoges, European Ceramic Center, 12 Rue Atlantis, 87068 Limoges (France); Khan, Amir Azam [Department of Mechanical and Manufacturing Engineering, Faculty of Engineering, Universiti Malaysia Sarawak, 94300 Kota Samarahan, Sarawak (Malaysia); Labbe, Jean-Claude [SPCTS, UMR 7315, CNRS, University of Limoges, European Ceramic Center, 12 Rue Atlantis, 87068 Limoges (France)

2015-12-01

Highlights: • Surface oxidation of ZrB{sub 2}-SiC ceramic composites by Yb-fibre laser. • Round spiral laser pattern created for the surface oxidation. • Presence of laser-formed oxide scale and unaffected beneath regions. • Crazed but uncracked surface oxide. • A dense glassy SiO{sub 2}-rich layer exhibited enhances oxidation resistance. - Abstract: Surface treatment of ceramic substrates by a laser beam can allow to incorporate interesting properties to these ceramics. In the present work, surface oxidation of ca. 30% porous ZrB{sub 2}-SiC ceramic composites by using an ytterbium fibre laser was conducted. Oxidation of ceramic substrates through this process under ambient conditions has certain advantages compared to the classical oxidation method. A particular spiral laser pattern was created in order to produce an oxidized structure on ZrB{sub 2}-SiC porous substrates. The laser parameters were as follows i.e., laser power of 50, 60 and 70 W, a beam diameter of 1.25 mm, velocity of 2 mm/s, acceleration and deceleration of 1 mm/s{sup 2}. The microstructural and morphological changes in the laser-treated region was examined using scanning electron microscopy, energy dispersive X-ray spectroscopy, and X-ray diffraction. At laser power of 70 W, the sample exhibits uniform oxidation. It revealed that the very porous bulk beneath remained unaffected and unoxidized because this laser-formed oxide scale protects the substrate from oxidation. The presence of oxidized and unaffected regions indicated a high degree of heat localization. The dense glassy SiO{sub 2}-rich layer prevents the inward oxygen diffusion into the inner bulk hence enhances the oxidation resistance.

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

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

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

Corrosion properties of zirconium-based ceramic coatings for micro-bearing and biomedical applications

Science.gov (United States)

Walkowicz, J.; Zavaleyev, V.; Dobruchowska, E.; Murzynski, D.; Donkov, N.; Zykova, A.; Safonov, V.; Yakovin, S.

2016-03-01

Ceramic oxide ZrO2 and oxynitride ZrON coatings are widely used as protective coatings against diffusion and corrosion. The enhancement of the coatings' mechanical properties, as well as their wear and corrosion resistance, is very important for their tribological performance. In this work, ZrO2 and ZrON coatings were deposited by magnetron sputtering on stainless steel (AISI 316) substrates. The adhesion, hardness and elastic properties were evaluated by standard methods. The surface structure of the deposited coatings was observed by electron scanning microscopy (SEM) and atomic force microscopy (AFM). The composition of the coatings was analyzed by X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS). The corrosion resistance properties were evaluated using the potentiodynamic method. The results show that the corrosion parameters are significantly increased in the cases of both oxynitride and oxide coatings in comparison with the stainless steel (AISI 316) substrates.

Ion irradiation studies of oxide ceramics

International Nuclear Information System (INIS)

Zinkle, S.J.

1988-01-01

This paper presents the initial results of an investigation of the depth-dependent microstructures of three oxide ceramics following ion implantation to moderate doses. The implantations were performed using ion species that occur as cations in the target material; for example, Mg + ions were used for MgO and MgAl 2 O 4 (spinel) irradiations. This minimized chemical effects associated with the implantation and allowed a more direct evaluation to be made of the effects of implanted ions on the microstructure. 11 refs., 14 figs

The effect of environmental factors on selected mechanical properties of zirconium dioxide

Science.gov (United States)

Wirwicki, W.; Andrzejewska, A.; Andryszczyk, M.; Siemianowski, P.

2018-04-01

In many centers around the world, research studies are carried out on the mechanical strength of dental materials and glued joints. A literature review shows the variety of testing techniques related to analyzing the strength and durability of the material itself and the glued joints. In dental ceramics, zirconium dioxide is most often used as a base material, and chemically it consists of 97% ZrO2 and 3% Y2O3. This study was to determine the mechanical properties of zirconium dioxide under different environmental conditions. The material is used for the production of dental crowns and tooth bridges in the CAD/CAM technology. This medium is currently one of the most advanced-generation materials used for prosthetic and implant restorations. They were then subjected to a three-point bending test on the Instron ElektroPlus E3000 durability machine. Storage conditions and time have a positive influence on reducing variation in zirconium resistance for active forces and destructive stresses.

Glass/Ceramic Composites for Sealing Solid Oxide Fuel Cells

Science.gov (United States)

Bansal, Narottam P.; Choi, Sung R.

2007-01-01

A family of glass/ceramic composite materials has been investigated for use as sealants in planar solid oxide fuel cells. These materials are modified versions of a barium calcium aluminosilicate glass developed previously for the same purpose. The composition of the glass in mole percentages is 35BaO + 15CaO + 5Al2O3 + 10B2O3 + 35SiO2. The glass seal was found to be susceptible to cracking during thermal cycling of the fuel cells. The goal in formulating the glass/ ceramic composite materials was to (1) retain the physical and chemical advantages that led to the prior selection of the barium calcium aluminosilicate glass as the sealant while (2) increasing strength and fracture toughness so as to reduce the tendency toward cracking. Each of the composite formulations consists of the glass plus either of two ceramic reinforcements in a proportion between 0 and 30 mole percent. One of the ceramic reinforcements consists of alumina platelets; the other one consists of particles of yttria-stabilized zirconia wherein the yttria content is 3 mole percent (3YSZ). In preparation for experiments, panels of the glass/ceramic composites were hot-pressed and machined into test bars.

Biomechanical testing of zirconium dioxide osteosynthesis system for Le Fort I advancement osteotomy fixation.

Science.gov (United States)

Hingsammer, Lukas; Grillenberger, Markus; Schagerl, Martin; Malek, Michael; Hunger, Stefan

2018-01-01

The following work is the first evaluating the applicability of 3D printed zirconium dioxide ceramic miniplates and screws to stabilize maxillary segments following a Le-Fort I advancement surgery. Conventionally used titanium and individual fabricated zirconium dioxide miniplates were biomechanically tested and compared under an occlusal load of 120N and 500N using 3D finite element analysis. The overall model consisted of 295,477 elements. Under an occlusal load of 500N a safety factor before plastic deformation respectively crack of 2.13 for zirconium dioxide and 4.51 for titanium miniplates has been calculated. From a biomechanical point of view 3D printed ZrO 2 mini-plates and screws are suggested to constitute an appropriate patient specific and metal-free solution for maxillary stabilization after Le Fort I osteotomy. Copyright © 2017 Elsevier Ltd. All rights reserved.

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

Evaluation of Ultra-High Temperature Ceramics for Aeropropulsion Use

Science.gov (United States)

Levine, Stanley R.; Opila, Elizabeth J.; Halbig, Michael C.; Kiser, James D.; Singh, Mrityunjay; Salem, Jonathan A.

2001-01-01

Among the ultra-high temperature ceramics (UHTC) are a group of materials consisting of zirconium diboride or hafnium diboride plus silicon carbide, and in some instances, carbon. These materials offer a good combination of properties that make them candidates for airframe leading edges on sharp-bodied reentry vehicles. These UHTC perform well in the environment for such applications, i.e., air at low pressure. The purpose of this study was to examine three of these materials under conditions more representative of a propulsion environment, i.e., higher oxygen partial pressure and total pressure. Results of strength and fracture toughness measurements, furnace oxidation and high velocity thermal shock exposures are presented for ZrB2 plus 20 volume % SiC, ZrB2 plus 14 volume % SiC plus 30 volume % C, and SCS-9a SiC fiber reinforced ZrB2 plus 20 volume % SiC. The poor oxidation resistance of UHTCs is the predominant factor limiting their applicability to propulsion applications.

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

Environmental Effects on Non-oxide Ceramics

Science.gov (United States)

Jacobson, Nathan S.; Opila, Elizabeth J.

1997-01-01

Non-oxide ceramics such as silicon carbide (SiC) and silicon nitride (Si3N4) are promising materials for a wide range of high temperature applications. These include such diverse applications as components for heat engines, high temperature electronics, and re-entry shields for space vehicles. Table I lists a number of selected applications. Most of the emphasis here will be on SiC and Si3N4. Where appropriate, other non-oxide materials such as aluminum nitride (AlN) and boron nitride (BN) will be discussed. Proposed materials include both monolithic ceramics and composites. Composites are treated in more detail elsewhere in this volume, however, many of the oxidation/corrosion reactions discussed here can be extended to composites. In application these materials will be exposed to a wide variety of environments. Table I also lists reactive components of these environments.It is well-known that SiC and Si3N4 retain their strength to high temperatures. Thus these materials have been proposed for a variety of hot-gas-path components in combustion applications. These include heat exchanger tubes, combustor liners, and porous filters for coal combustion products. All combustion gases contain CO2, CO, H2, H2O, O2, and N2. The exact gas composition is dependent on the fuel to air ratio or equivalence ratio. (Equivalence ratio (EQ) is a fuel-to-air ratio, with total hydrocarbon content normalized to the amount of O2 and defined by EQ=1 for complete combustion to CO2 and H2O). Figure 1 is a plot of equilibrium gas composition vs. equivalence ratio. Note that as a general rule, all combustion atmospheres are about 10% water vapor and 10% CO2. The amounts of CO, H2, and O2 are highly dependent on equivalence ratio.

Determination of copper oxidizing power in superconducting yttrium ceramics

International Nuclear Information System (INIS)

Pontaler, R.P.; Lebed', N.B.

1989-01-01

A new photometric method for determining the formal copper degree of oxidation and oxygen deficiency in superconducting high-temperature oxides containing yttrium, barium and copper is developed. The method is based on oxidation of Co(2) complex with EDTA by Cu(3) ions in acetrate buffer solution with pH 4.2-4.7 and allows one to determine 1-10% of Cu(3). Relative standard deviation when determining Cu(3) makes up 0.03-0.05. Using a qualitative reaction with the application of sodium vanadate hydrochloride solution the absence of peroxide compound in superconducting yttrium ceramics is ascertained

Structural studies of calcium phosphate doped with titanium and zirconium obtained by high-energy mechanical alloying

Energy Technology Data Exchange (ETDEWEB)

Silva, C C; Sombra, A S B [Telecommunications and Materials Science and Engineering Laboratory (LOCEM), Physics Department, Federal University of Ceara, Campus do Pii, Postal Code 6030, 60455-760, Fortaleza-Ceara (Brazil)], E-mail: sombra@fisica.ufc.br

2009-12-15

In this paper, we present a new variation of the solid-state procedure on the synthesis of bioceramics with titanium (CapTi) and zirconium (CapZr), considering that zirconium (ZrO{sub 2}) and titanium oxide (TiO{sub 2}) are strengthening agents, due to their superb force and fracture toughness. The high efficiency of the calcination process opens a new way of producing commercial amounts of nanocrystalline bioceramics. In this work, a new variation of the solid-state procedure method was used to produce nanocrystalline powders of titanium and zirconium, using two different experimental chemical routes: CapTi: Ca(H{sub 2}PO{sub 4}){sub 2}+TiO{sub 2} and CapZr: Ca(H{sub 2}PO{sub 4}){sub 2}+ZrO{sub 2}. The powders were submitted to calcination processes (CapTic and CapZrc) at 800, 900 and 1000 deg. C. The calcium titanium phosphate phase, CaTi{sub 4}P{sub 6}O{sub 24}, was obtained in the CapTic reaction and the calcium zirconium phosphate, CaZr{sub 4}P{sub 6}O{sub 24}, was obtained in the CapZrc reaction. The obtained ceramics were characterized by x-ray powder diffraction (XRD), infrared (IR) spectroscopy, Raman scattering spectroscopy (RSS) and scanning electron microscopy (SEM) analysis. This method was compared with the milling process (CapTim and CapZrm), where in the last process the melting is not necessary and the powder obtained is nanocrystalline. The calcium titanium phosphate phase, CaTi{sub 4}P{sub 6}O{sub 24}, was obtained in the reaction CapTim, but in CapZrm the formation of any calcium phosphate phase even after 15 h of dry mechanical alloying was not observed.

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

A method for the densification of ceramic layers, especially ceramic layers within solid oxide cell (SOC) technology, and products obtained by the method

DEFF Research Database (Denmark)

2013-01-01

A ceramic layer, especially for use in solid oxide cell (SOC) technology, is densified in a method comprising (a) providing a multilayer system by depositing the porous ceramic layer, which is to be densified, onto the selected system of ceramic layers on a support, (b) pre-sintering the resulting......(s) in the porous layer surface and (e) performing a thermal treatment at a temperature T2, where T2 > ?1, to obtain densification of and grain growth in the porous layer formed in step (b). The method makes it possible to obtain dense ceramic layers at temperatures, which are compatible with the other materials...... present in a ceramic multilayer system....

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.

Effects of surface-finishing protocols on the roughness, color change, and translucency of different ceramic systems.

Science.gov (United States)

Akar, Gülcan Coşkun; Pekkan, Gürel; Çal, Ebru; Eskitaşçıoğlu, Gürcan; Özcan, Mutlu

2014-08-01

Surface-finishing protocols have a mechanical impact on ceramic surfaces that could eventually affect surface topography and light scattering. An optimum protocol is needed to avoid damaging the optical properties of ceramics. The purpose of this study was to determine the effects of different surface-finishing protocols on the surface roughness, color change, and translucency of ceramic and metal ceramic restorations. Standardized disk-shaped specimens (1.5 × 10 mm, n=128) were fabricated from 3 different ceramic core materials (aluminum oxide [Al2O3]-AL, zirconium oxide [ZrO2]-ZR, lithium disilicate [Li2Si2O5]-LIT), veneered (V) with dentin ceramics (n=32 per group), and placed in the following groups: ALV, ZRV, and LITV. The metal ceramic group acted as the control (n=32). Four different surface-finishing methods were tested. Airborne-particle abrasion with 50 μm Al2O3, polishing with adjustment kit, polishing with adjustment kit plus diamond polishing paste, and autoglazing (n=8 subgroup) were applied on the veneering ceramics. The specimens were analyzed with a profilometer for surface roughness, and color change and translucency were measured with a clinical spectrophotometer. Statistical analyses were performed with 1-way ANOVA and the Tukey honest significant difference tests (α=.05). Specimens treated with the airborne particle abrasion method showed significantly higher mean profilometer for surface roughness values in all groups (P.05). With the diamond polishing paste method, lower surface roughness values were achieved in the ZRV and metal ceramic groups acted as the control groups. Different surface-finishing methods affected the color change of the ceramic systems, except for ZRV. Surface-finishing protocols significantly affected the translucency values of the ALV, LITV, and metal ceramic groups (Pceramics tested. The airborne-particle abrasion protocol created rougher surfaces and decreased translucency, and color change in zirconia was not

Non-conventional synthesis of ceramic pigments

International Nuclear Information System (INIS)

Dziubak, C.; Rutkowski, R.; Gebel, R.

2003-01-01

A short characterization of traditional methods of homogenization of components, used to produce ceramic pigments, was presented. Efficient and economic methods are searched to prepare raw material sets for ceramic pigments as alternative methods for the traditional way of wet mixing in ball mill or of dry mixing in the mixer of 'Z' type. The results of research of the use of sol-gel method to achieve these aims are presented. At the present stage of research, carried out on the yellow praseodymium and coral-pink iron-zirconium pigments show that traditional methods are better. (author)

Corrosion properties of zirconium-based ceramic coatings for micro-bearing and biomedical applications

International Nuclear Information System (INIS)

Walkowicz, J; Zavaleyev, V; Dobruchowska, E; Murzynski, D; Donkov, N; Zykova, A; Safonov, V; Yakovin, S

2016-01-01

Ceramic oxide ZrO 2 and oxynitride ZrON coatings are widely used as protective coatings against diffusion and corrosion. The enhancement of the coatings' mechanical properties, as well as their wear and corrosion resistance, is very important for their tribological performance. In this work, ZrO 2 and ZrON coatings were deposited by magnetron sputtering on stainless steel (AISI 316) substrates. The adhesion, hardness and elastic properties were evaluated by standard methods. The surface structure of the deposited coatings was observed by electron scanning microscopy (SEM) and atomic force microscopy (AFM). The composition of the coatings was analyzed by X-ray photoelectron spectroscopy (XPS) and energy dispersive X-ray spectroscopy (EDS). The corrosion resistance properties were evaluated using the potentiodynamic method. The results show that the corrosion parameters are significantly increased in the cases of both oxynitride and oxide coatings in comparison with the stainless steel (AISI 316) substrates. (paper)

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.

Ceramic joining

Energy Technology Data Exchange (ETDEWEB)

Loehman, R.E. [Sandia National Lab., Albuquerque, NM (United States)

1996-04-01

This paper describes the relation between reactions at ceramic-metal interfaces and the development of strong interfacial bonds in ceramic joining. Studies on a number of systems are described, including silicon nitrides, aluminium nitrides, mullite, and aluminium oxides. Joints can be weakened by stresses such as thermal expansion mismatch. Ceramic joining is used in a variety of applications such as solid oxide fuel cells.

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

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 �

Oxidation resistant filler metals for direct brazing of structural ceramics

Science.gov (United States)

Moorhead, Arthur J.

1986-01-01

A method of joining ceramics and metals to themselves and to one another is described using essentially pure trinickel aluminide and trinickel aluminide containing small amounts of carbon. This method produces strong joints that can withstand high service temperatures and oxidizing environments.

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.

Passivation of mechanically polished, chemically etched and anodized zirconium in various aqueous solutions: Impedance measurements

International Nuclear Information System (INIS)

Abo-Elenien, G.M.; Abdel-Salam, O.E.

1987-01-01

Zirconium and its alloys are finding increasing applications especially in water-cooled nuclear reactors. Because of the fact that zirconium is electronegative (E 0 = -1.529V) its corrosion resistance in aqueous solutions is largely determined by the existence of a thin oxide film on its surface. The structure and properties of this film depend in the first place on the method of surface pre-treatment. This paper presents an experimental study of the nature of the oxide film on mechanically polished, chemically etched and anodized zirconium. Ac impedance measurements carried out in various acidic, neutral and alkaline solutions show that the film thickness depends on the method of surface pre-treatment and the type of electrolyte solution. The variation of the potential and impedance during anodization of zirconium at low current density indicates that the initial stages of polarization consist of oxide build-up at a rate dependent on the nature of the electrode surface and the electrolyte. Oxygen evolution commences at a stage where oxide thickening starts to decline. The effect of frequency on the measured impedance indicates that the surface reactivity, and hence the corrosion rate, decreases in the following order: mechanically polished > chemically etched > anodized

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

Electric-Loading Enhanced Kinetics in Oxide Ceramics: Pore Migration, Sintering and Grain Growth: Final Report

Energy Technology Data Exchange (ETDEWEB)

Chen, I-Wei [Univ. of Pennsylvania, Philadelphia, PA (United States). Dept. of Materials Science & Engineering

2018-02-02

Solid oxide fuel cells and solid oxide electrolysis cells rely on solid electrolytes in which a large ionic current dominates. This project was initiated to investigate microstructural changes in such devices under electrochemical forces, because nominally insignificant processes may couple to the large ionic current to yield non-equilibrium phenomena that alter the microstructure. Our studies had focused on yttria-stabilized cubic zirconia (YSZ) widely used in these devices. The experiments have revealed enhanced grain growth at higher temperatures, pore and gas bubble migration at all temperatures, and the latter also lead to enhanced sintering of highly porous ceramics into fully dense ceramics at unprecedentedly low temperatures. These results have shed light on kinetic processes that fall completely outside the realm of classical ceramic processing. Other fast-oxygen oxide ceramics closely related to, and often used in conjunction with zirconia ceramics, have also be investigated, as are closely related scientific problems in zirconia ceramics. These include crystal structures, defects, diffusion kinetics, oxygen potentials, low temperature sintering, flash sintering, and coarsening theory, and all have resulted in greater clarity in scientific understanding. The knowledge is leveraged to provide new insight to electrode kinetics and near-electrode mixed conductivity and to new materials. In the following areas, our research has resulted in completely new knowledge that defines the state-of-the-art of the field. (a) Electrical current driven non-equilibrium phenomena, (b) Enhanced grain growth under electrochemically reducing conditions, (c) Development of oxygen potential polarization in electrically loaded electrolyte, (d) Low temperature sintering and grain growth, and (e) Structure, defects and cation kinetics of fluorite-structured oxides. Our research has also contributed to synthesis of new energy-relevant electrochemical materials and new understanding

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

Hydrogen desorption kinetics from zirconium hydride and zirconium metal in vacuum

International Nuclear Information System (INIS)

Hu, Xunxiang; Terrani, Kurt A.; Wirth, Brian D.

2014-01-01

The kinetics of hydrogen desorption from zirconium hydride is important in many nuclear design and safety applications. In this paper, a coordinated experimental and modeling study has been used to explicitly demonstrate the applicability of existing kinetic theories for hydrogen desorption from zirconium hydride and α-zirconium. A static synthesis method was used to produce δ-zirconium hydride, and the crystallographic phases of the zirconium hydride were confirmed by X-ray diffraction (XRD). Three obvious stages, involving δ-zirconium hydride, a two-phase region, and α-zirconium, were observed in the hydrogen desorption spectra of two zirconium hydride specimens with H/Zr ratios of 1.62 and 1.64, respectively, which were obtained using thermal desorption spectroscopy (TDS). A continuous, one-dimensional, two-phase moving boundary model, coupled with the zero- and second-order kinetics of hydrogen desorption from δ-zirconium hydride and α-zirconium, respectively, has been developed to reproduce the TDS experimental results. A comparison of the modeling predictions with the experimental results indicates that a zero-order kinetic model is valid for description of hydrogen flux away from the δ-hydride phase, and that a second-order kinetic model works well for hydrogen desorption from α-Zr if the activation energy of desorption is optimized to be 70% of the value reported in the literature

Effect of yttria addition on the stability of porous chromium oxide ceramics in supercritical water

International Nuclear Information System (INIS)

Dong Ziqiang; Chen Weixing; Zheng Wenyue; Guzonas, Dave

2013-01-01

Porous chromium oxide (Cr 2 O 3 ) ceramics were prepared by oxidizing highly porous chromium carbides that were obtained by a reactive sintering method, and were evaluated at temperatures ranging from 375 °C to 625 °C in supercritical water (SCW) environments with a fixed pressure of 25–30 MPa. Reactive element yttrium was introduced to the porous oxide ceramic by adding various amounts of yttria of 5, 10 and 20 wt.%, respectively, prior to reactive sintering. The exposure in SCW shows that the porous chromium oxide is quite stable in SCW at 375 °C. However, the stability decreased with increasing temperature. It is well known that chromium oxide can be oxidized to soluble chromium (VI) species in SCW when oxygen is present. Adding yttria increases the stability of chromium oxide in SCW environments. However, adding yttria higher than 5 wt.% increased the weight loss of porous chromium oxide samples because of the direct dissociation of Y 2 O 3 in SCW.

Process for making a titanium diboride-chromium diboride-yttrium titanium oxide ceramic composition

Science.gov (United States)

Holcombe, C.E.; Dykes, N.L.

1992-04-28

A ceramic composition is described. The ceramic composition consists essentially of from about 84 to 96 w/o titanium diboride, from about 1 to 9 w/o chromium diboride, and from about 3 to about 15 w/o yttrium-titanium-oxide. A method of making the ceramic composition is also described. The method of making the ceramic composition comprises the following steps: Step 1--A consolidated body containing stoichiometric quantities of titanium diboride and chromium diboride is provided. Step 2--The consolidated body is enclosed in and in contact with a thermally insulated package of yttria granules having a thickness of at least 0.5 inches. Step 3--The consolidated body enclosed in the thermally insulated package of yttria granules is heated in a microwave oven with microwave energy to a temperature equal to or greater than 1,900 degrees centigrade to sinter and uniformly disperse yttria particles having a size range from about 1 to about 12 microns throughout the consolidated body forming a densified body consisting essentially of titanium diboride, chromium diboride, and yttrium-titanium-oxide. The resulting densified body has enhanced fracture toughness and hardness. No Drawings

Experimental Investigations on the Influence of Adhesive Oxides on the Metal-Ceramic Bond

Directory of Open Access Journals (Sweden)

Susanne Enghardt

2015-01-01

Full Text Available The objective of this study was to test the influence of selected base metals, which act as oxide formers, on the metal-ceramic bond of dental veneer systems. Using ion implantation techniques, ions of Al, In and Cu were introduced into near-surface layers of a noble metal alloy containing no base metals. A noble metal alloy with base metals added for oxide formation was used as a reference. Both alloys were coated with a low-temperature fusing dental ceramic. Specimens without ion implantation or with Al2O3 air abrasion were used as controls. The test procedures comprised the Schwickerath shear bond strength test (ISO 9693-1, profile height (surface roughness measurements (ISO 4287; ISO 4288; ISO 25178, scanning electron microscopy (SEM imaging, auger electron spectroscopy (AES and energy dispersive X-ray analysis (EDX. Ion implantation resulted in no increase in bond strength. The highest shear bond strengths were achieved after oxidation in air and air abrasion with Al2O3 (41.5 MPa and 47.8 MPa respectively. There was a positive correlation between shear bond strength and profile height. After air abrasion, a pronounced structuring of the surface occurred compared to ion implantation. The established concentration shifts in alloy and ceramic could be reproduced. However, their positive effects on shear bond strength were not confirmed. The mechanical bond appears to be of greater importance for metal-ceramic bonding.

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...

Optimization of the conditions for producing zirconia by the precipitation of basic zirconium sulfate

International Nuclear Information System (INIS)

Ricci, D.R.; Paschoal, J.O.A.

1988-01-01

The process of precipitation of the basic sulfate from zirconium oxychlorides solutions has been optimized in order to obtain zirconia of high purity as well as suitable for ceramic processing. The main parameters of this study were obtained from the determination of the pH and of the concentration of the initial oxychloride solution, of the sulfate/zirconium molar ratio and of the reaction temperature. The following experimental procedure has been carried out: a) reaction of each precipitate with ammonium hydroxide followed by drying at 150 0 -C / 5 h and calcination at 1000 0 C / 1 h, yielding the final product (zirconia) b) product characterization by means of spectrographic, X - ray fluorescence and diffractometry analyses, determination of grain size distribution and of apparent density, and morphology study by scanning electron microscopy. The yielding of the overall reaction has been determined by chemical analysis and the composition of the basic zirconium sulfate by thermogravimetric analyses. (author) [pt

Core–Shell Electrospun Hollow Aluminum Oxide Ceramic Fibers

Directory of Open Access Journals (Sweden)

Jonathan W. Rajala

2015-10-01

Full Text Available In this work, core–shell electrospinning was employed as a simple method for the fabrication of composite coaxial polymer fibers that became hollow ceramic tubes when calcined at high temperature. The shell polymer solution consisted of polyvinyl pyrollidone (PVP in ethanol mixed with an aluminum acetate solution to act as a ceramic precursor. The core polymer was recycled polystyrene to act as a sacrificial polymer that burned off during calcination. The resulting fibers were analyzed with X-ray diffraction (XRD and energy dispersive spectroscopy (EDS to confirm the presence of gamma-phase aluminum oxide when heated at temperatures above 700 °C. The fiber diameter decreased from 987 ± 19 nm to 382 ± 152 nm after the calcination process due to the polymer material being burned off. The wall thickness of these fibers is estimated to be 100 nm.

[Advantages and disadvantages of applying yttrium stabilized zirconium-dioxide post and core restorations].

Science.gov (United States)

Pétercsák, Anita; Radics, Tünde; Hegedus, Csaba

2014-03-01

Full ceramic restorations are associated with metal free post and core prosthodontics for teeth with seriously destroyed clinical crowns. Using custom made zirconium-dioxide post and cores can be flattering not only to give a good aesthetic result, but also to provide excellent retention. As none of the post systems stands all demands, prudent planning is mandatory. Our paper deals with favourable and unfavourable conditions as well as common causes of failures of post and core restorations. We took morphological, esthetical and functional considerations that can help to achieve the best results. Amongst them individual anatomic constitution, shape, width and length of the root and root canal, shape of the clinical crown, direction and magnitude of chewing forces are the most important factors. To give examples we present two cases of zirconium-dioxide post and core restorations. In our first case the missing clinical crown and a too wide root canal entrance created a questionable prognosis. To minimize adverse effect of the missing ferrule effect we applied custom-made zirconium-dioxide post and core and an additional abutment. After 7 years the restoration is still functioning. The second case represented a much favourable situation with 1,5 mm clinical crown height. The restoration was a custom-made zirconia post and core and a full-ceramic crown as a single tooth restoration. Although in this case we expected a better prognosis, 15 months later the patient showed up with a post fracture for applying extreme forces on the crown.

Reactor vessel using metal oxide ceramic membranes

Science.gov (United States)

Anderson, Marc A.; Zeltner, Walter A.

1992-08-11

A reaction vessel for use in photoelectrochemical reactions includes as its reactive surface a metal oxide porous ceramic membrane of a catalytic metal such as titanium. The reaction vessel includes a light source and a counter electrode. A provision for applying an electrical bias between the membrane and the counter electrode permits the Fermi levels of potential reaction to be favored so that certain reactions may be favored in the vessel. The electrical biasing is also useful for the cleaning of the catalytic membrane.

Corrosion of Ceramic Materials

Science.gov (United States)

Opila, Elizabeth J.; Jacobson, Nathan S.

1999-01-01

Non-oxide ceramics are promising materials for a range of high temperature applications. Selected current and future applications are listed. In all such applications, the ceramics are exposed to high temperature gases. Therefore it is critical to understand the response of these materials to their environment. The variables to be considered here include both the type of ceramic and the environment to which it is exposed. Non-oxide ceramics include borides, nitrides, and carbides. Most high temperature corrosion environments contain oxygen and hence the emphasis of this chapter will be on oxidation processes.

Densification of silicon and zirconium carbides by a new process: spark plasma sintering; Densification des carbures de silicium et de zirconium par un procede innovant: le spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Guillard, F

2006-12-15

Materials research for suitable utilization in 4. generation nuclear plants needs new ways to densify testing components. Two carbides, silicon and zirconium carbide seems to be the most suitable choice due to their mechanical, thermal and neutron-transparency properties against next nuclear plant specifications. Nevertheless one main difficulty remains, which is densifying them even at high temperature. Spark Plasma Sintering a new metal-, ceramic- and composite-sintering process has been used to densify both SiC and ZrC. Understanding bases of mass transport mechanisms in SPS have been studied. Composites and interfaces have been processed and analyzed. This manuscript reports original results on SiC and ZrC ceramics sintered with commercial powder started, without additives. (author)

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

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)

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)

Y-TZP ceramic processing from coprecipitated powders: a comparative study with three commercial dental ceramics.

Science.gov (United States)

Lazar, Dolores R R; Bottino, Marco C; Ozcan, Mutlu; Valandro, Luiz Felipe; Amaral, Regina; Ussui, Valter; Bressiani, Ana H A

2008-12-01

(1) To synthesize 3mol% yttria-stabilized zirconia (3Y-TZP) powders via coprecipitation route, (2) to obtain zirconia ceramic specimens, analyze surface characteristics, and mechanical properties, and (3) to compare the processed material with three reinforced dental ceramics. A coprecipitation route was used to synthesize a 3mol% yttria-stabilized zirconia ceramic processed by uniaxial compaction and pressureless sintering. Commercially available alumina or alumina/zirconia ceramics, namely Procera AllCeram (PA), In-Ceram Zirconia Block (CAZ) and In-Ceram Zirconia (IZ) were chosen for comparison. All specimens (6mmx5mmx5mm) were polished and ultrasonically cleaned. Qualitative phase analysis was performed by XRD and apparent densities were measured on the basis of Archimedes principle. Ceramics were also characterized using SEM, TEM and EDS. The hardness measurements were made employing Vickers hardness test. Fracture toughness (K(IC)) was calculated. Data were analyzed using one-way analysis of variance (ANOVA) and Tukey's test (alpha=0.05). ANOVA revealed that the Vickers hardness (pceramic materials composition. It was confirmed that the PA ceramic was constituted of a rhombohedral alumina matrix, so-called alpha-alumina. Both CAZ and IZ ceramics presented tetragonal zirconia and alpha-alumina mixture of phases. The SEM/EDS analysis confirmed the presence of aluminum in PA ceramic. In the IZ and CAZ ceramics aluminum, zirconium and cerium in grains involved by a second phase containing aluminum, silicon and lanthanum were identified. PA showed significantly higher mean Vickers hardness values (H(V)) (18.4+/-0.5GPa) compared to vitreous CAZ (10.3+/-0.2GPa) and IZ (10.6+/-0.4GPa) ceramics. Experimental Y-TZP showed significantly lower results than that of the other monophased ceramic (PA) (pceramics (pceramic processing conditions led to ceramics with mechanical properties comparable to commercially available reinforced ceramic materials.

Methods for the preparation of ultra-pure anhydrous zirconium tetrafluoride from zirconium tetraborohydride, researches in connection with halide glasses

International Nuclear Information System (INIS)

Tortevois, R.

1990-01-01

The synthesis of ultrapure zirconium tetrafluoride, the main component of fluorozirconate based optical fibers, was successfully attempted from zirconium tetraborohydride. Of the fluorinating agents used, nitrogen trifluoride doesn't react with zirconium tetraborohydride while xenon difluoride reacts too violently and leads to phases which contain boron. The fluorination in a compatible solvent enabled us to minimize the degradation. The best results were obtained with the fluorination of Zr(BH 4 ) 4 dissolved in CFCl 3 at -40 deg C by anhydrous HF. Using several analytical methods such as graphite furnace atomic absorption and proton activation, we analyzed the purity. The degree of transition element impurities is less than the ppm level for ZrF 4 . The dehydration of ZrF 4 ,H 2 O and ZrF 4 ,3H 2 O at room temperature by CIF 3 in gaseous and liquid state was also investigated. At exceptionally low temperature, this process allows oxide and oxyfluoride components to be reduced

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.

Development and sintering of alumina based mixed oxide ceramic products for sensor applications in petroleum industries

Energy Technology Data Exchange (ETDEWEB)

Yadava, Y.P.; Muniz, L.B.; Aguiar, L.A.R.; Sanguinetti Ferreira, R.A. [Departamento de Engenharia Mecanica, Universidade Federal de Pernambuco, CEP 50741-530, Recife-PE (Brazil); Albino Aguiar, J. [Departamento de Fisica, Universidade Federal de Pernambuco, CEP 50670-901 Recife-PE (Brazil)

2005-07-01

In petroleum production, different types of sensors are required to monitor temperature, pressure, leakage of inflammable gases, etc. These sensors work in very hostile environmental conditions and frequently suffer from abrasion and corrosion problems. Presently perovskite oxide based ceramic materials are increasingly being used for such purposes, due to their highly inert behavior in hostile environment. In the present work, we have developed and characterized alumina based complex perovskite oxide ceramics, Ba{sub 2}AlSnO{sub 5.5}. These ceramics were prepared by solid state reaction process and produced in the form of circular discs by uniaxial pressure compaction technique. Green ceramic bodies were sintered at different sintering temperatures (1200 to 1500 deg. C) in air atmosphere. Structural and microstructural characteristics of sintered Ba{sub 2}AlMO{sub 5.5} were studied by XRD and SEM techniques. Mechanical properties were tested by Vickers microhardness tests. Ceramics sintered in the temperature range 1300 deg. C 1400 deg. C presented best results in terms of microstructural characteristics and mechanical performance. (authors)

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)

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

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)

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.

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.

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

Densification of silicon and zirconium carbides by a new process: spark plasma sintering

International Nuclear Information System (INIS)

Guillard, F.

2006-12-01

Materials research for suitable utilization in 4. generation nuclear plants needs new ways to densify testing components. Two carbides, silicon and zirconium carbide seems to be the most suitable choice due to their mechanical, thermal and neutron-transparency properties against next nuclear plant specifications. Nevertheless one main difficulty remains, which is densifying them even at high temperature. Spark Plasma Sintering a new metal-, ceramic- and composite-sintering process has been used to densify both SiC and ZrC. Understanding bases of mass transport mechanisms in SPS have been studied. Composites and interfaces have been processed and analyzed. This manuscript reports original results on SiC and ZrC ceramics sintered with commercial powder started, without additives. (author)

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

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.

Industrial ceramics - Properties, forming and applications

International Nuclear Information System (INIS)

Fantozzi, Gilbert; Niepce, Jean-Claude; Bonnefont, Guillaume; Alary, J.A.; Allard, B.; Ayral, A.; Bassat, J.M.; Elissalde, C.; Maglione, M.; Beauvy, M.; Bertrand, G.; Bignon, A.; Billieres, D.; Blanc, J.J.; Blumenfeld, P.; Bonnet, J.P.; Bougoin, M.; Bourgeon, M.; Boussuge, M.; Thorel, A.; Bruzek, C.E.; Cambier, F.; Carrerot, H.; Casabonne, J.M.; Chaix, J.M.; Chevalier, J.; Chopinet, M.H.; Couque, H.; Courtois, C.; Leriche, A.; Dhaler, D.; Denape, J.; Euzen, P.; Ganne, J.P.; Gauffinet, S.; Girard, A.; Gonon, M.; Guizard, C.; Hampshire, S.; Joulin, J.P.; Julbe, A.; Ferrato, M.; Fontaine, M.L.; Lebourgeois, R.; Lopez, J.; Maquet, M.; Marinel, S.; Marrony, M.; Martin, J.F.; Mougin, J.; Pailler, R.; Pate, M.; Petitpas, E.; Pijolat, C.; Pires-Franco, P.; Poirier, C.; Poirier, J.; Pourcel, F.; Potier, A.; Tulliani, J.M.; Viricelle, J.P.; Beauger, A.

2013-01-01

After a general introduction to ceramics (definition, general properties, elaboration, applications, market data), this book address conventional ceramics (elaboration, material types), thermo-structural ceramics (oxide based ceramics, non-oxide ceramics, fields of application, functional coatings), refractory ceramics, long fibre and ceramic matrix composites, carbonaceous materials, ceramics used for filtration, catalysis and the environment, ceramics for biomedical applications, ceramics for electronics and electrical engineering (for capacitors, magnetic, piezoelectric, dielectric ceramics, ceramics for hyper-frequency resonators), electrochemical ceramics, transparent ceramics (forming and sintering), glasses, mineral binders. The last chapter addresses ceramics used in the nuclear energy sector: in nuclear fuels and fissile material, absorbing ceramics and shields, in the management of nuclear wastes, new ceramics for reactors under construction or for future nuclear energy

Microstructural Improvement of Hydroxyapatite-ZrO2 Composite Ceramics via Thermal Precipitation Techniques.

Science.gov (United States)

Sangmala, A.; Limsuwan, P.; Kaewwiset, W.; Naemchanthara, K.

2017-09-01

Hydroxyapatite-ZrO2 composite ceramic were synthesized using a thermal precipitation techniques. The chemical precursors were prepared from di-ammonium hydrogen orthophosphate, calcium oxide (CaO) derived from chicken eggshell, zirconium dioxide (ZrO2) and distilled water. The mixture were heated at the various temperatures from 100 to 700 °C in the furnace with an incremental temperature of 100 °C. The ZrO2 contents in the composite ceramic were varied from 0 to 15 percent weight of CaO. The prepared composites were then annealed at 300, 600 and 700 °C for 4 h in air. The crystal structure, function group and morphology of all samples were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), field emission scanning electron microscopy (FESEM) and universal testing machine (UTM), respectively. The results indicated that the undoped-ZrO2 samples hydroxyapatite phase with a hexagonal structure. However, the hydroxyapatite was transformed to the tri-calcium phosphate after thermal treatment at 700 °C. For the doped-ZrO2 samples, the hydroxyapatite and ZrO2 phases were found. Moreover, the result showed that the compressive strength of hydroxyapatite-ZrO2 composite ceramic increased with increasing the ZrO2 content.

Creep performance of oxide ceramic fiber materials at elevated temperature in air and in steam

Science.gov (United States)

Armani, Clinton J.

Structural aerospace components that operate in severe conditions, such as extreme temperatures and detrimental environments, require structural materials that have superior long-term mechanical properties and that are thermochemically stable over a broad range of service temperatures and environments. Ceramic matrix composites (CMCs) capable of excellent mechanical performance in harsh environments are prime candidates for such applications. Oxide ceramic materials have been used as constituents in CMCs. However, recent studies have shown that high-temperature mechanical performance of oxide-oxide CMCs deteriorate in a steam-rich environment. The degradation of strength at elevated temperature in steam has been attributed to the environmentally assisted subcritical crack growth in the oxide fibers. Furthermore, oxide-oxide CMCs have shown significant increases in steady-state creep rates in steam. The present research investigated the effects of steam on the high-temperature creep and monotonic tension performance of several oxide ceramic materials. Experimental facilities were designed and configured, and experimental methods were developed to explore the influence of steam on the mechanical behaviors of ceramic fiber tows and of ceramic bulk materials under temperatures in the 1100--1300°C range. The effects of steam on creep behavior of Nextel(TM)610 and Nextel(TM)720 fiber tows were examined. Creep rates at elevated temperatures in air and in steam were obtained for both types of fibers. Relationships between creep rates and applied stresses were modeled and underlying creep mechanisms were identified. For both types of fiber tows, a creep life prediction analysis was performed using linear elastic fracture mechanics and a power-law crack velocity model. These results have not been previously reported and have critical design implications for CMC components operating in steam or near the recommended design limits. Predictions were assessed and validated via

Ceramic hot-gas filter

Science.gov (United States)

Connolly, E.S.; Forsythe, G.D.; Domanski, D.M.; Chambers, J.A.; Rajendran, G.P.

1999-05-11

A ceramic hot-gas candle filter is described having a porous support of filament-wound oxide ceramic yarn at least partially surrounded by a porous refractory oxide ceramic matrix, and a membrane layer on at least one surface thereof. The membrane layer may be on the outer surface, the inner surface, or both the outer and inner surface of the porous support. The membrane layer may be formed of an ordered arrangement of circularly wound, continuous filament oxide ceramic yarn, a ceramic filler material which is less permeable than the filament-wound support structure, or some combination of continuous filament and filler material. A particularly effective membrane layer features circularly wound filament with gaps intentionally placed between adjacent windings, and a filler material of ceramic particulates uniformly distributed throughout the gap region. The filter can withstand thermal cycling during back pulse cleaning and is resistant to chemical degradation at high temperatures.

Ceramic hot-gas filter

Science.gov (United States)

Connolly, Elizabeth Sokolinski; Forsythe, George Daniel; Domanski, Daniel Matthew; Chambers, Jeffrey Allen; Rajendran, Govindasamy Paramasivam

1999-01-01

A ceramic hot-gas candle filter having a porous support of filament-wound oxide ceramic yarn at least partially surrounded by a porous refractory oxide ceramic matrix, and a membrane layer on at least one surface thereof. The membrane layer may be on the outer surface, the inner surface, or both the outer and inner surface of the porous support. The membrane layer may be formed of an ordered arrangement of circularly wound, continuous filament oxide ceramic yarn, a ceramic filler material which is less permeable than the filament-wound support structure, or some combination of continuous filament and filler material. A particularly effective membrane layer features circularly wound filament with gaps intentionally placed between adjacent windings, and a filler material of ceramic particulates uniformly distributed throughout the gap region. The filter can withstand thermal cycling during backpulse cleaning and is resistant to chemical degradation at high temperatures.

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

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)

A modified anode/electrolyte structure for a solid oxide electrochemical cell and a method for making said structure

DEFF Research Database (Denmark)

2013-01-01

-stabilised zirconium oxide electrolyte and (c) a metallic and/or a ceramic electrocatalyst in the shape of interlayers incorporated in the interface between the anode and the electrolyte. This assembly is first sintered at a given temperature and then at a lower temperature in reducing gas mixtures. These heat...... treatments resulted in a distribution of the metallic and/or ceramic interlayers in the electrolyte/anode backbone junction taking place. The structure is prepared by (a) depositing a ceramic interlayer onto one side of the electrolyte, (b) optionally applying a metallic interlayer thereon, (c) repeating...... steps (a) and (b), (d) applying a layer of the selected anode backbone onto the electrolyte with applied interlayers, (e) sintering the raw assembly and (f) infiltrating the electrocatalyst precursor into the sintered assembly and heat treating the assembly to incorporate additional electrocatalyst...

Automatic measuring system of zirconium thickness for zirconium liner cladding tubes

International Nuclear Information System (INIS)

Matsui, K.; Yamaguchi, H.; Hiroshima, T.; Sakamoto, T.; Murayama, R.

1985-01-01

An automatic system of pure zirconium liner thickness for zirconium-zircaloy cladding tubes has been successfully developed. The system consists of three parts. (1) An ultrasonic thickness measuring method for mother tubes before cold rolling. (2) An electromagnetic thickness measuring method for the manufactured tubes. (3) An image processing method for the cross sectional view of the manufactured cut tube samples. In Japanese nuclear industry, zirconium-zircaloy cladding tubes have been tested in order to realize load following operation in the atomic power plant. In order to provide for the practical use in the near future, Sumitomo Metal Industries, Ltd. has been studied and established the practical manufacturing process of the zirconium liner cladding tubes. The zirconium-liner cladding tube is a duplex tube comprising an inner layer of pure zirconium bonded to zircaloy metallurgically. The thickness of the pure zirconium is about 10 % of the total wall thickness. Several types of the automatic thickness measuring methods have been investigated instead of the usual microscopic viewing method in which the liner thickness is measured by the microscopic cross sectional view of the cut tube samples

Wettability of zirconium diboride ceramics by Ag, Cu and their alloys with Zr

International Nuclear Information System (INIS)

Muolo, M.L.; Ferrera, E.; Novakovic, R.; Passerone, A.

2003-01-01

Sintered ZrB 2 ceramics, pure and with 4 wt.% Ni as sintering aid, have been tested in contact with liquid Ag, Cu, Ag-Cu and Ag-Cu-Zr. ''Pure'' ZrB 2 ceramics are wetted by Ag-Zr alloys, and ZrB 2 /Ni ceramics also by pure Cu. The wetting behaviour is briefly discussed in terms of existing wetting theories

Microstructure evolution during pressureless sintering of bulk oxide ceramics

Directory of Open Access Journals (Sweden)

Karel Maca

2009-06-01

Full Text Available The author’s experience concerning the infl uence of the choice of different pressureless heating schedules on the fi nal microstructure of oxide ceramic materials is summarized in the paper. Alumina, ceria, strontium titanate, as well as tetragonal (3 mol% Y2O3 and cubic (8 mol% Y2O3 zirconia were cold isostatically pressed or injection moulded and pressureless sintered with different heating schedules – namely with Constant-Rate of Heating with different dwell temperatures (CRH, with Rate-Controlled Sintering (RCS and with Two-Step Sintering (TSS. It was examined whether some of these three sintering schedules, with the same fi nal density achieved, can lead to a decrease of the grain size of sintered ceramics. The results showed that only TSS (and only for selected materials brought significant decrease of the grain size.

Development of iron oxide and titania treated fly ash based ceramic and its bioactivity

Energy Technology Data Exchange (ETDEWEB)

Sultana, Parveen [Physics Department, Jadavpur University, Kolkata-700 032 (India); Das, Sukhen, E-mail: das_sukhen@yahoo.com [Physics Department, Jadavpur University, Kolkata-700 032 (India); Bhattacharya, Alakananda [Physics Department, West Bengal State University, Barasat (India); Basu, Ruma [Physics Department, Jogamaya Devi College, Kolkata-700026 (India); Nandy, Papiya [Centre for Interdisciplinary Research and Education, Kolkata-700 068 (India)

2012-08-01

The increasing accumulation of fly ash from thermal power plants poses a major problem to the environment. The present work reflects the novel utilization of this profusely available industrial waste in the form of an antibacterial hard ceramic material by treating fly ash with ferric oxide (Fe{sub 2}O{sub 3}) and titania (TiO{sub 2}) during sintering process at 1600 Degree-Sign C. The developed material shows more than 90% bacterial reduction against both Gram-positive and Gram-negative bacteria. The mechanism of their antibacterial action was studied by transmission electron microscopy (TEM) image analysis of the bacterial cross-section. The developed ceramic material acquires hardness due to the enhancement of the natural mullite content in the matrix. The mullite content and the crystallinity of mullite have shown their increasing trend with increasing concentration of the metal oxide during sintering process. A maximum of {approx} 37% increase in mullite was obtained for 7% w/w Fe{sub 2}O{sub 3} and TiO{sub 2}. Metal oxide lowered the activation energy of the reaction and enhanced the reaction rate of alumina (Al{sub 2}O{sub 3})-silica (SiO{sub 2}) to form mullite which increases the hardness. The study highlights novel utilization of fly ash as a hard ceramic antibacterial product (bioceramics) for both structural and hygiene applications in an eco-friendly way. - Highlights: Black-Right-Pointing-Pointer A novel antibacterial hard ceramic material by treating fly ash with metal oxide. Black-Right-Pointing-Pointer The material shows excellent antibacterial activity (> 90%) against pathogenic bacteria. Black-Right-Pointing-Pointer Mechanism of antibacterial action by TEM analysis. Black-Right-Pointing-Pointer Enhancement of the concentration of 'natural mullite content' in the material. Black-Right-Pointing-Pointer Hardness induced by enhanced mullite content is an added advantage for prolonged product life.

Structural and electrical properties of Nd ion modified lead zirconate titanate nanopowders and ceramics

International Nuclear Information System (INIS)

Da-Wei, Wang; De-Qing, Zhang; Quan-Liang, Zhao; Hong-Mei, Liu; Zhi-Ying, Wang; Mao-Sheng, Cao; Jie, Yuan

2009-01-01

A modified sol-gel method is used for synthesizing Nd ion doped lead zirconate titanate nanopowders Pb 1–3x/2 Nd x Zr 0.52 Ti 0.48 O 3 (PNZT) in an ethylene glycol system with zirconium nitrate as zirconium source. The results show that it is critical to add lead acetate after the reaction of zirconium nitrate with tetrabutyl titanate in the ethylene glycol system for preparing PNZT with an exact fraction of titanium content. It has been observed that the dopant of excess Nd ions can effectively improve the sintered densification and activity of the PNZT ceramics. Piezoelectric, dielectric and ferroelectric properties of the PNZT ceramics are remarkably enhanced as compared with those of monolithic lead zirconate titanate (PZT). Especially, the supreme values of piezoelectric constant (d 33 ) and dielectric constant ( element of ) for the PNZT are both about two times that of the monolithic PZT and moreover, the remnant polarization (P r ) also increases by 30%. According to the analysis of the structures and properties, we attribute the improvement in electrical properties to the lead vacancies caused by the doping of Nd ions

Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure and method of processing

Science.gov (United States)

Brown, Jr., Jesse J.; Hirschfeld, Deidre A.; Li, Tingkai

1993-12-07

Alkali corrosion resistant coatings and ceramic foams having superfine open cell structure are created using sol-gel processes. The processes have particular application in creating calcium magnesium zirconium phosphate, CMZP, coatings and foams.

Radiochemical neutron activation analysis of zirconium and zirconium-niobium alloys

International Nuclear Information System (INIS)

Tashimova, F.A.; Sadikov, I.I.; Salimov, M.

2004-01-01

Full text: Zirconium and zirconium-niobium alloys are used on nuclear technology, as fuel cladding of nuclear reactors. Their nuclear-physical, mechanical and thermophysical properties are influenced them matrix and impurity composition, therefore determination of matrix and impurity content of these materials is a very important task. Neutron activation analysis is one from multielemental and high sensible techniques that are widely applied in analysis of high purity materials. Investigation of nuclear-physical characteristics of zirconium has shown that instrumental variant NAA is unusable for analysis due to high radioactivity of a matrix. Therefore it is necessary carrying out radiochemical separation of impurity radionuclides from matrix. Study of the literature datum have shown, that zirconium and niobium are very well extracted from muriatic solution with 5% tributyl phosphineoxide (TBPO) solution in toluene and 0,75 M solution of di-2-ethyl hexyl phosphoric acid (HDEHP) in cyclohexanone. Investigation of these elements extraction in these systems has shown that more effective and selective separation of matrix radionuclides is achieved in HDEHP-3M HCI system. This system is also extracted and hafnium, witch is an accompanying element of zirconium and its high content prevented determination of other impurity elements in sample. Therefore we used extraction system HDEHP-3M HCl for analysis of zirconium and zirconium-niobium alloys in chromatographic variant. By measurement of distribution profile of a matrix and of elution curve of determined elements is established, that for effective separation of impurity and matrix radionuclides there is enough chromatographic column with diameter 1 cm and height of a sorbent layer 7 cm, thus volume of elute, necessary for complete elution of determinate elements is 35-40 ml. On the basis of the carried out researches the technique of radiochemical NAA of high purity zirconium and zirconium-niobium alloy, which allows to

Study of the microstructure and the hardness of PZT piezoelectric ceramics types I and III used in electro acoustic transducers; Estudo da microestrutura e da microdureza das ceramicas piezoeletricas tipos PZT I e III utilizadas em transdutores eletroacusticos

Energy Technology Data Exchange (ETDEWEB)

Cabral, Ricardo de Freitas; Itaboray, Lucas Mendes; Santos, Anna Paula de Oliveira [Centro Universitario de Volta Redonda (UNIFOA), Volta Redonda, RJ (Brazil)

2015-12-15

The field of electronic processing of the ceramic piezoelectric type imported powdered led to the production of ceramics with 97% of theoretical density, homogeneous microstructure with great potential for applications in piezoelectric devices such as electro acoustic transducers. However, the production of electronic ceramics National piezoelectric type is not yet able to have as raw material zirconate titanate Lead (PZT) 100% made in Brazil. Thus, this is used for supply of domestic production, the zirconium oxide. In this work, both post PZT types I and III, imported, were uniaxially pressed at 70 MPa and sintered at 1200 and 1250 deg C for 3 hours. Hardness measurements were performed by micro indentation, X-ray diffraction analysis and Scanning Electron Microscopy. The hardness of PZT I was 393 HV. (author)

Natural Radioactivity in Ceramic Materials

International Nuclear Information System (INIS)

Abu Khadra, S.A.; Kamel, N.H.

2005-01-01

Ceramics are one of the most important types of the industrial building materials. The raw materials of the ceramic are made of a mixture of clay, feldspar, silica, talc kaolin minerals together with zirconium silicates (ZrSiO4).The ceramic raw materials and the final products contain naturally occurring radionuclide mainly U-238 and, Th-232 series, and the radioactive isotope of potassium K-40. Six raw ceramic samples were obtained from the Aracemco Company at Egypt together with a floor tile sample (final product) for measuring radioactive concentration levels., The activity of the naturally U-238, Th-232, and K-40 were determined as (Bq/kg) using gamma spectroscopy (Hyperactive pure germanium detector). Concentration of U and Th were determined in (ppm) using spectrophotometer technique by Arsenazo 111 and Piridy l-Azo -Resorcinol (PAR) indicators. Sequential extraction tests were carried out in order to determine the quantity of the radionuclide associated with various fractions as exchangeable, carbonate, acid soluble and in the residue. The results evaluated were compared to the associated activity indices (AI) that were defined by former USSR and West Germany

Compatibility of sodium with ceramic oxides employed in nuclear reactors

International Nuclear Information System (INIS)

Acena, V.

1981-01-01

A review of experiments carried out up to the present time on the corrosion and compatibility of ceramic oxides with liquid sodium at temperatures corresponding to those in fast breeder reactors, is presented. The results of a thermo-dynamic/liquid sodium reactions are included. The exercise has been conducted with a view to effecting experimental studies in the future. (author) [es

Compatibility of sodium with ceramic oxides employed in nuclear reactors

International Nuclear Information System (INIS)

Acena Moreno, V.

1981-01-01

This work is a review of experiments carried out up to the present time on the corrosion and compatibility of ceramic oxides with liquid sodium at temperatures corresponding to those in fast breeder reactors. The review also includes the results of a thermo-dynamic/liquid sodium reactions. The exercise has been conducted with a view to effecting experimental studies in the future. (Author)

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)

The characterization of an oxide interfacial coating for ceramic matrix composites

International Nuclear Information System (INIS)

Coons, Timothy P.; Reutenauer, Justin W.; Mercado, Andrew; Kmetz, Michael A.; Suib, Steven L.

2013-01-01

This work focused on the use of metal organic chemical vapor deposition (MOCVD) to deposit a zinc oxide (ZnO) coating on ceramic fibers as an interfacial system for continuous fiber reinforced ceramic matrix composites (CFR-CMCs). ZnO coatings were deposited on ceramic grade (CG) Nicalon ™ , Hi-Nicalon ™ , and Hi-Nicalon ™ Type S fabric by the thermal decomposition of zinc acetate dihydrate in a low pressure hot wall CVD reactor. A duplex SiO 2 coating was also deposited in order to protect the ZnO layer from the reducing conditions during composite fabrication. Tow testing was used to evaluate the effect of the ZnO coating on the strength retention of the ceramic fabrics. Single strand unidirectional mini composites were fabricated by infiltrating SiC into the ZnO/SiO 2 duplex coated tows in order to understand the interfacial properties of the ZnO coating. The mini composite utilizing Hi-Nicalon ™ Type S produced the highest ultimate tensile strength (UTS) of 330 MPa. The coated fabrics and the mini composites were characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and scanning Auger microscopy (SAM)

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.

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

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.

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.

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

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)

On the initial corrosion mechanism of zirconium alloy: Interaction of oxygen and water with Zircaloy at room temperature and 450 C evaluated by x-ray absorption spectroscopy and photoelectron spectroscopy

International Nuclear Information System (INIS)

Doebler, U.; Knop, A.

1994-01-01

The initial stages of zirconium oxide formation on Zircaloy after water (H 2 O) and oxygen (O 2 ) exposures have been investigated in situ using photoelectron spectroscopy and X-ray-absorption spectroscopy. The reactivity of the zirconium alloy with O 2 at room temperature is about 1,000 times higher than for H 2 O. Up to 100 L (1 L = 1 Langmuir unit = 1 · 10 -6 mbar · s) H 2 O exposure, the reactivity of the zirconium alloy at 450 C is comparable to the room temperature reaction. At higher H 2 O exposure, a sharp increase in the reaction rate for the high-temperature oxidation is observed. From the energy position of the Zr 3d photo emission line and their oxygen-induced chemical shifts, one can really follow the formation of the oxide films. Two different substoichiometric oxides were found during reaction with water. Suboxide (1) is located at the zirconium/zirconium-oxide interface. Subsequently, a Suboxide (2) is concluded from the chemical shift of the zirconium photoelectrons. After an oxide thickness of 2 nm, the stoichiometric ZrO 2 phase is not yet developed

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

High pressure low temperature hot pressing method for producing a zirconium carbide ceramic

Science.gov (United States)

Cockeram, Brian V.

2017-01-10

A method for producing monolithic Zirconium Carbide (ZrC) is described. The method includes raising a pressure applied to a ZrC powder until a final pressure of greater than 40 MPa is reached; and raising a temperature of the ZrC powder until a final temperature of less than 2200.degree. C. is reached.

Laser beam joining of non-oxidic ceramics for ultra high temperature resistant joints

International Nuclear Information System (INIS)

Lippmann, W.; Knorr, J.; Wolf, R.; Reinecke, A.M.; Rasper, R.

2004-01-01

The excellent technical properties of silicon carbide (SiC) and silicon nitride (Si 3 N 4 ) ceramics, such as resistance to extreme temperatures, oxidation, mechanical wear, aggressive chemical substances and radioactive radiation and also its high thermal conductivity and good temperature-shock resistance, make these ceramics ideally suited for use in the field of nuclear technology. However, their practical use has been limited so far because of the unavailability of effective joining techniques for these ceramics, especially for high temperature applications. A new joining technology (CERALINK registered ) has been developed in a network project which allowed high temperature resistant and vacuum-tight joining of SiC or Si 3 N 4 ceramics. A power laser is used as heat source, which makes it possible to join ceramic components in free atmosphere in combination with a pure oxidic braze filler. As no furnace is necessary, there are no limitations on the component dimensions by the furnace-geometry. During the joining process, the heated area can be limited to the seam area so that this technology can also be used to encapsulate materials with a low melting point. The seam has a high mechanical strength, it is resistant to a wide range of chemicals and radiation and it is also vacuum-tight. The temperature resistance can be varied by variation of the braze filler composition - usually between 1,400 C and >1,600 C. Beside the optimum filler it is also important to select the suitable laser wavelength. The paper will demonstrate the influence of different wave lengths, i. e. various laser types, on the seam quality. Examples are chosen to illustrate the strengths and limitations of the new technology

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.

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.

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)

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.

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.

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.

Synthesis and characterization of ceramic pigments based on oxides of chromium and iron, on TiO2

International Nuclear Information System (INIS)

Silva, E.M. da; Galvao, S.B.; Paskocimas, C.A.

2011-01-01

This work used oxides of chromium and iron, as precursors of the synthesis of ceramic pigments. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through pre-calcination, breakdown, calcination at different temperatures (900 and 1100 ° C), resulting in pigments: green for pigment chrome deposited on TiO 2 and orange for iron on TiO 2 . Noticing an increase in the opacity with increasing temperature. The thermal analysis (TG and DTA), evaluated their thermal behavior, the XRD revealed the formation of crystalline phases as Iron Titanate and Chrome Titanate; SEM showed the formation of hexagonal particles for both oxides. Thus, the synthesized oxides were within the requirements for application as ceramic pigments. (author)

FIBROUS CERAMIC-CERAMIC COMPOSITE MATERIALS PROCESSING AND PROPERTIES

OpenAIRE

Naslain , R.

1986-01-01

The introduction of continuous fibers in a ceramic matrix can improve its toughness, if the fiber-matrix bonding is weak enough, due to matrix microcracking and fiber pull-out. Ceramic-ceramic composite materials are processed according to liquid or gas phase techniques. The most important are made of glass, carbide, nitride or oxide matrices reinforced with carbon, SiC or Al2O3 fibers.

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)

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)

Adherent zirconia films by reactive ion implantation

International Nuclear Information System (INIS)

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

1993-01-01

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

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

Science.gov (United States)

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

2014-11-01

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

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

Processing, Structure and High Temperature Oxidation Properties of Polymer-Derived and Hafnium Oxide Based Ceramic Systems

Science.gov (United States)

Terauds, Kalvis

Demands for hypersonic aircraft are driving the development of ultra-high temperature structural materials. These aircraft, envisioned to sustain Mach 5+, are expected to experience continuous temperatures of 1200--1800°C on the aircraft surface and temperatures as high as 2800°C in combustion zones. Breakthroughs in the development of fiber based ceramic matrix composites (CMCs) are opening the door to a new class of high-tech UHT structures for aerospace applications. One limitation with current carbon fiber or silicon carbide fiber based CMC technology is the inherent problem of material oxidation, requiring new approaches for protective environmental barrier coatings (EBC) in extreme environments. This thesis focuses on the development and characterization of SiCN-HfO2 based ceramic composite EBC systems to be used as a protective layer for silicon carbide fiber based CMCs. The presented work covers three main architectures for protection (i) multilayer films, (ii) polymer-derived HfSiCNO, and (iii) composite SiCN-HfO 2 infiltration. The scope of this thesis covers processing development, material characterization, and high temperature oxidation behavior of these three SiCN-HfO2 based systems. This work shows that the SiCN-HfO 2 composite materials react upon oxidation to form HfSiO4, offering a stable EBC in streaming air and water vapor at 1600°C.

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.

The characterization of an oxide interfacial coating for ceramic matrix composites

Energy Technology Data Exchange (ETDEWEB)

Coons, Timothy P., E-mail: tpcoons@gmail.com [Department of Chemistry, Unit 3060, University of Connecticut, 55 North Eagleville Road, Storrs, CT 06269-3060 (United States); Reutenauer, Justin W.; Mercado, Andrew [Department of Chemistry, Unit 3060, University of Connecticut, 55 North Eagleville Road, Storrs, CT 06269-3060 (United States); Kmetz, Michael A. [Pratt and Whitney, 400 Main Street M/S 114-43, East Hartford, CT 06108 (United States); Suib, Steven L. [Department of Chemistry, Unit 3060, University of Connecticut, 55 North Eagleville Road, Storrs, CT 06269-3060 (United States)

2013-06-20

This work focused on the use of metal organic chemical vapor deposition (MOCVD) to deposit a zinc oxide (ZnO) coating on ceramic fibers as an interfacial system for continuous fiber reinforced ceramic matrix composites (CFR-CMCs). ZnO coatings were deposited on ceramic grade (CG) Nicalon{sup ™}, Hi-Nicalon{sup ™}, and Hi-Nicalon{sup ™} Type S fabric by the thermal decomposition of zinc acetate dihydrate in a low pressure hot wall CVD reactor. A duplex SiO{sub 2} coating was also deposited in order to protect the ZnO layer from the reducing conditions during composite fabrication. Tow testing was used to evaluate the effect of the ZnO coating on the strength retention of the ceramic fabrics. Single strand unidirectional mini composites were fabricated by infiltrating SiC into the ZnO/SiO{sub 2} duplex coated tows in order to understand the interfacial properties of the ZnO coating. The mini composite utilizing Hi-Nicalon{sup ™} Type S produced the highest ultimate tensile strength (UTS) of 330 MPa. The coated fabrics and the mini composites were characterized using field emission scanning electron microscopy (FE-SEM), X-ray diffraction (XRD) and scanning Auger microscopy (SAM)

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

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).

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

Application of modified multiwall carbon nanotubes as a sorbent for zirconium (IV) adsorption from aqueous solution

International Nuclear Information System (INIS)

Yavari, R.; Davarkhah, R.

2013-01-01

Modified multiwall carbon nanotubes (MWCNTs) by nitric acid solution were used to investigate the adsorption behavior of zirconium from aqueous solution. Pristine and oxidized MWCNTs were characterized using nitrogen adsorption/desorption isotherm, Boehm's titration method, thermogravimetry analysis, transmission electron microscopy and Fourier transform infrared spectroscopy. The results showed that the surface properties of MWCNTs such as specific surface area, total pore volume, functional groups and the total number of acidic and basic sites were improved after oxidation. These improvements are responsible for their hydrophobic properties and consequently an easy dispersion in water and suitable active sites for more adsorption of zirconium. The adsorption of Zr(IV) as a function of initial concentration of zirconium, contact time, MWCNTs dosage, HCl and HNO 3 concentration and also ionic strength was investigated using a batch technique under ambient conditions. The experimental results indicated that sorption of Zr(IV) was strongly influenced by zirconium concentrations, oxidized MWCNTs content and acid pH values. The calculated correlation coefficient of the linear regressions values showed that Langmuir model fits the adsorption equilibrium data better than the Freundlich model. Kinetic data of sorption indicated that equilibrium was achieved within 60 min and the adsorption process can be described by the pseudo second-order reaction rate model. Based on the experimental results, surface complexation is the major mechanism for adsorption of Zr(IV) onto MWCNTs. Also, Study on the desorption process of zirconium showed that the complete recovery can be obtained using nitric or hydrochloric acids of 4 M. (author)

Hydrogen determination in magnesium, zirconium, sodium and lithium using installation, C2532

International Nuclear Information System (INIS)

Malikova, E.D.; Velyukhanov, V.P.; Makhinova, L.O.; Kunin, L.L.

1980-01-01

Techniques of hydrogen determination in magnesium, lithium, sodium and zirconium using the S 2532 installation are developed. The method of oxidizing melting using lead borate has been used for hydrogen determination in lithium and sodium and the method of vacuum extraction - for hydrogen determination in zirconium and magnesium. Zr and Mg extraction has been carried out in steel reactor at the temperatures of 1000 and 650 deg C, the time of extraction being 30 and 10 minutes respectively. A quartz reactor, temperatures of oxidizing melting of 700-800 deg C, the time of analysis 10 and 20 minutes have been used for sodium and lithium. A possibility to determine volumetric content of hydrogen in magnesium at the existing surface contaminations with hydrogen-containing compounds is shown [ru

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

Energy Technology Data Exchange (ETDEWEB)

Basin, N

2001-01-01

This work deals with the synthesis of zirconium. The ore is carbo-chlorinated to obtain the tetrachloride which is then purified by selective condensation and extractive distillation. Zirconium tetrachloride is then reduced by magnesium and the pseudo-alloy is obtained according to the global following reaction (Kroll process): ZrCl{sub 4} + 2 Mg = 2 MgCl{sub 2}. By thermodynamics, it has been shown that the volatilization of magnesium chloride and the formation of zirconium sub-chlorides are minimized when the combined effects of temperature and of dilution with argon are limited. With these conditions, the products, essentially zirconium and magnesium chloride, are obtained in equivalence ratio in the magnesio-thermia reaction. The global kinetics of the reduction process has been studied by a thermal gravimetric method. A thermo-balance device has been developed specially for this kinetics study. It runs under a controlled atmosphere and is coupled to a vapor tetrachloride feed unit. The transformation is modelled supposing that the zirconium and magnesium chloride formation result: 1)of the evaporation of magnesium from its liquid phase 2)of the transfer of magnesium and zirconium tetrachloride vapors towards the front of the reaction located in the gaseous phase 3)of the chemical reaction. In the studied conditions, the diffusion is supposed to be the limiting process. The influence of the following parameters: geometry of the reactive zone, temperature, scanning rate of the argon-zirconium tetrachloride mixture, composition of the argon-zirconium tetrachloride mixture has been experimentally studied and confronted with success to the model. (O.M.)

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

Formulation and synthesis by melting process of titanate enriched glass-ceramics and ceramics

International Nuclear Information System (INIS)

Advocat, T.; Fillet, C.; Lacombe, J.; Bonnetier, A.; McGlinn, P.

1999-01-01

The main objective of this work is to provide containment for the separated radionuclides in stable oxide phases with proven resistance to leaching and irradiation damage and in consequence to obtain a glass ceramic or a ceramic material using a vitrification process. Sphene glass ceramic, zirconolite glass ceramic and zirconolite enriched ceramic have been fabricated and characterized by XRD, SEM/EDX and DTA