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

Science.gov (United States)

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

2015-01-01

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

Method of producing thermally stable uranium carbonitrides

International Nuclear Information System (INIS)

Ugajin, M.; Takahashi, I.

1975-01-01

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

Corrosion resistance and biocompatibility of zirconium oxynitride thin film growth by RF sputtering

Energy Technology Data Exchange (ETDEWEB)

Cubillos, G. I.; Olaya, J. J.; Clavijo, D.; Alfonso, J. E. [Universidad Nacional de Colombia, Carrera 45 No. 26-85, AA 14490 Bogota D. C. (Colombia); Bethencourt, M., E-mail: jealfonsoo@unal.edu.co [Universidad de Cadiz, Centro Andaluz de Ciencia y Tecnologia Marinas, Departamento de Ciencia de los Materiales e Ingenieria Metalurgica y Quimica Inorganica, Av. Republica de Saharaui, Puerto Real, E-11510 Cadiz (Spain)

2012-07-01

Thin films of zirconium oxynitride were grown on common glass, silicon (100) and stainless steel 316 L substrates using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (Sem) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The corrosion resistance studies were made on samples of stainless steel 316 L coated and uncoated with Zr{sub x}N{sub y}O films, through of polarization curves. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316 L through proliferation and cellular adhesion. The XRD analysis shows that films deposited at 623 K, with a flow ratio {Phi}N{sub 2}/{Phi}O{sub 2} of 1.25 and a total deposit time of 30 minutes grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The Sem analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. The analysis of the corrosion resistant, shows that the stainless steel coated with the film was increased a factor 10. Finally; through the analysis of the biocompatibility we established that the films have a better surface than the substrate (stainless steel 316 L) in terms of the adhesion and proliferation of bone cells. (Author)

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

Energy Technology Data Exchange (ETDEWEB)

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

1963-07-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1963-07-01

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

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

Synthesis and biological characterization of zirconium oxynitride thin film growth by radio-frequency sputtering

Energy Technology Data Exchange (ETDEWEB)

Cubillos, G.I. [Departamento de Química, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Olaya, J.J. [Facultad de Ingeniería, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Clavijo, D. [Facultad de Medicina, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Alfonso, J.E., E-mail: jealfonsoo@unal.edu.co [Grupo de materiales con Aplicaciones Tecnológicas, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia); Cardozo, C. [Instituto de Biotecnología, Universidad Nacional de Colombia, AA 14490 Bogotá (Colombia)

2013-02-01

Thin films of zirconium oxynitride were grown on common glass, silicon substrates (100) and on stainless steel 316L using the reactive RF magnetron sputtering technique. The films were analyzed through structural, morphological, and biocompatibility studies. The structural analysis was carried out using X-ray diffraction (XRD), and the morphological analysis was carried out using scanning electron microscopy (SEM) and atomic force microscopy (AFM). These studies were done as a function of growth parameters, such as power applied to the target, substrate temperature, and flow ratios. The studies of biocompatibility were carried out on zirconium oxynitride films deposited on stainless steel 316L through proliferation and cellular adhesion. The XRD analysis showed that films deposited at 623 K, with a flow ratio ΦN{sub 2}/ΦO{sub 2} of 1.25 and a total deposit time of 30 min grew preferentially oriented along the (111) plane of the zirconium oxynitride monoclinic phase. The SEM analyses showed that the films grew homogeneously, and the AFM studies indicated that the average rugosity of the film was 5.9 nm and the average particle size was 150 nm. Finally, through the analysis of the biocompatibility, we established that the films have a better surface than the substrate (stainless steel 316L) in terms of adhesion and proliferation of bone cells. - Highlights: ►ZrO{sub x}N{sub y} thin films were deposited using reactive radio-frequency magnetron sputtering. ►We studied the effect of deposition parameters on ZrO{sub x}N{sub y} thin films microstructure. ►We have been able to grow bone cells on ZrO{sub x}N{sub y} coated stainless steel 316L.

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)

Properties of zirconium ceramics and film stabilized by yttrium

International Nuclear Information System (INIS)

Korobova, N.

2004-01-01

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

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

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

Science.gov (United States)

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

2016-09-15

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

Plastic flow and preferred orientation in molybdenum and zirconium films

International Nuclear Information System (INIS)

Window, B.

1989-01-01

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

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.

Dissolution of anodic zirconium dioxide films in aqueous media

International Nuclear Information System (INIS)

Merati, A.; Cox, B.

1999-01-01

Zirconium with a low thermal neutron cross section, good corrosion resistance in high-temperature water, and high thermal conductivity is an ideal material for nuclear reactors. Its good resistance to water and steam at reactor temperatures is of the greatest interest to nuclear fuel designers. Dissolution of zirconium dioxide (ZrO 2 ) films in aggressive media was investigated. The extent of uniform and localized dissolution was measured by ultraviolet-visible (UV-VIS) spectrometry and an alternating current (AC) impedance test, respectively. Scanning electron microscopy (SEM) showed the extent of dissolution of ZrO 2 was a function only of the fluoride ion content and pH of the medium. Cathodic polarization was used to identify the preferred sites for localized dissolution of the oxide film. In 0.1 M potassium bifluoride (KHF 2 ), both uniform thinning and local breakdown of the oxide were observed. Within the limits of the investigating techniques, no evidence of dissolution was observed in the other solutions tested: 0.5 M sulfuric acid (H 2 SO 4 ). 1.0 M nitric acid (HNO 3 ), 5 M hydrochloric acid (HCl), or 0.1 M potassium fluoride (KF). In areas around iron-containing particles, fine cracks in the anodic oxide at prior metal grain boundaries and arrays of cracks in the oxide associated with residual scratches from the initial specimen preparation were the preferred spots for localized dissolution of the oxide film. Iron precipitates immediately below the surface of the oxide layer increased the local electrical conductivity. Enrichment of iron in the oxide matrix around these precipitates during the anodization process appeared to cause prospective spots, acting as anodic sites for pH formation

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.

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.

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.

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

International Nuclear Information System (INIS)

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

1987-01-01

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

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.

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

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

Science.gov (United States)

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

2013-11-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-12-07

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

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.

Thermophysical and elastic properties of titanium carbonitrides containing molybdenum and tungsten

International Nuclear Information System (INIS)

Matsuda, Tetsushi; Matsubara, Hideaki

2013-01-01

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

Investigation of Zirconium Oxide Films in Different Dissolved Hydrogen Concentration

International Nuclear Information System (INIS)

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

2016-01-01

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

Niobium and zirconium telluride thin films prepared by sputtering

International Nuclear Information System (INIS)

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

2000-01-01

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

Carbonitrides in the system Ta-TaC-TaN

International Nuclear Information System (INIS)

Ritzhaupt-Kleissl, H.J.

1975-04-01

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

Synthesis, sintering properties and thermal conductivity of uranium carbonitrides

International Nuclear Information System (INIS)

Wolters, R.A.M.

1978-01-01

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

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

International Nuclear Information System (INIS)

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

1999-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2009-04-01

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

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

International Nuclear Information System (INIS)

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

1978-01-01

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

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

Indian Academy of Sciences (India)

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

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 chemical vapor deposition of zirconium carbide onto ceramic substrates

International Nuclear Information System (INIS)

Glass A, John Jr.; Palmisiano, Nick Jr.; Welsh R, Edward

1999-01-01

Zirconium carbide is an attractive ceramic material due to its unique properties such as high melting point, good thermal conductivity, and chemical resistance. The controlled preparation of zirconium carbide films of superstoichiometric, stoichiometric, and substoichiometric compositions has been achieved utilizing zirconium tetrachloride and methane precursor gases in an atmospheric pressure high temperature chemical vapor deposition system

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-08-30

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1957-01-15

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

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

Institute of Scientific and Technical Information of China (English)

无

2006-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-04-24

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2006-05-01

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

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

Science.gov (United States)

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

2013-01-01

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

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.

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

Directory of Open Access Journals (Sweden)

Mozafari M

2013-04-01

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

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

International Nuclear Information System (INIS)

Pinard Legry, G.

1990-01-01

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

Optical properties of zirconium oxynitride films: The effect of composition, electronic and crystalline structures

Energy Technology Data Exchange (ETDEWEB)

Carvalho, P. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Borges, J., E-mail: joelborges@fisica.uminho.pt [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Department of Control Engineering, Faculty of Electrical Engineering, Czech Technical University in Prague, Technická 2, Prague 6 (Czech Republic); Rodrigues, M.S. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal); Barradas, N.P. [Centro de Ciências e Tecnologias Nucleares, Instituto Superior Técnico, Universidade de Lisboa, E.N. 10 (km 139,7), 2695-066 Bobadela LRS (Portugal); Alves, E. [Instituto de Plasmas e Fusão Nuclear, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049-001 Lisbon (Portugal); Espinós, J.P.; González-Elipe, A.R. [Instituto de Ciencia de Materiales de Sevilla (CSIC-University Sevilla), Avda. Américo Vespucio 49, 41092 Sevilla (Spain); Cunha, L.; Marques, L.; Vasilevskiy, M.I.; Vaz, F. [Centro de Física, Universidade do Minho, 4710-057 Braga (Portugal)

2015-12-15

Highlights: • Optical behaviour of ZrO{sub x}N{sub y} films were correlated with structural properties. • A continuous depopulation of the d-band and an opening of an energy gap was observed. • Drude–Lorentz parameters changed for the metallic samples. • Optical bandgap of the films increases with non-metallic elements incorporation. - Abstract: This work is devoted to the investigation of zirconium oxynitride (ZrO{sub x}N{sub y}) films with varied optical responses prompted by the variations in their compositional and structural properties. The films were prepared by dc reactive magnetron sputtering of Zr, using Ar and a reactive gas mixture of N{sub 2} + O{sub 2} (17:3). The colour of the films changed from metallic-like, very bright yellow-pale and golden yellow, for low gas flows to red-brownish for intermediate gas flows. Associated to this colour change there was a significant decrease of brightness. With further increase of the reactive gas flow, the colour of the samples changed from red-brownish to dark blue or even to interference colourations. The variations in composition disclosed the existence of four different zones, which were found to be closely related with the variations in the crystalline structure. XRD analysis revealed the change from a B1 NaCl face-centred cubic zirconium nitride-type phase for films prepared with low reactive gas flows, towards a poorly crystallized over-stoichiometric nitride phase, which may be similar to that of Zr{sub 3}N{sub 4} with some probable oxygen inclusions within nitrogen positions, for films prepared with intermediate reactive gas flows. For high reactive gas flows, the films developed an oxynitride-type phase, similar to that of γ-Zr{sub 2}ON{sub 2} with some oxygen atoms occupying some of the nitrogen positions, evolving to a ZrO{sub 2} monoclinic type structure within the zone where films were prepared with relatively high reactive gas flows. The analysis carried out by reflected electron energy

Method to electrolytically precipitate metals onto zirconium objects

International Nuclear Information System (INIS)

Donaghy, R.E.

1978-01-01

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

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

International Nuclear Information System (INIS)

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

2016-01-01

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

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

CERN Document Server

Kim, C H

2002-01-01

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

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

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

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

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-11-30

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

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

Science.gov (United States)

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

2010-01-05

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-12-01

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

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

International Nuclear Information System (INIS)

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

1996-01-01

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

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

Science.gov (United States)

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

2017-10-01

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

Method of preparing uranium nitride or uranium carbonitride bodies

International Nuclear Information System (INIS)

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

1976-01-01

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

Zirconium nitride hard coatings

International Nuclear Information System (INIS)

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

2010-01-01

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

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)

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

International Nuclear Information System (INIS)

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

2001-01-01

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

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.

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

Directory of Open Access Journals (Sweden)

Yanlin WANG

2015-11-01

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

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.

Electrochemical impedance spectroscopic study of passive zirconium

Energy Technology Data Exchange (ETDEWEB)

Ai Jiahe; Chen Yingzi [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States); Urquidi-Macdonald, Mirna [Department of Engineering Science and Mechanics, Pennsylvania State University, University Park, PA 16802 (United States); Macdonald, Digby D. [Center for Electrochemical Science and Technology, Department of Materials Science and Engineering, Pennsylvania State University, University Park, PA 16802 (United States)], E-mail: ddm2@psu.edu

2008-09-30

Spent, unreproccessed nuclear fuel is generally contained within the operational fuel sheathing fabricated from a zirconium alloy (Zircaloy 2, Zircaloy 4, or Zirlo) and is then stored in a swimming pool and/or dry storage facilities until permanent disposal in a licensed repository. During this period, which begins with irradiation of the fuel in the reactor during operation, the fuel sheathing is exposed to various, aggressive environments. The objective of the present study was to characterize the nature of the passive film that forms on pure zirconium in contact with an aqueous phase [0.1 M B(OH){sub 3} + 0.001 M LiOH, pH 6.94] at elevated temperatures (in this case, 250 deg. C), prior to storage, using electrochemical impedance spectroscopy (EIS) with the data being interpreted in terms of the point defect model (PDM). The results show that the corrosion resistance of zirconium in high temperature, de-aerated aqueous solutions is dominated by the outer layer. The extracted model parameter values can be used in deterministic models for predicting the accumulation of general corrosion damage to zirconium under a wide range of conditions that might exist in some repositories.

Mean-square displacement of atomic complex in titanium carbonitrides TiCxNy

International Nuclear Information System (INIS)

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

2004-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-12-30

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

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Nanostructured thin film coatings with different strengthening effects

Directory of Open Access Journals (Sweden)

Panfilov Yury

2017-01-01

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

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

Green Synthesis of Boron Carbonitride with High Capacitance

Directory of Open Access Journals (Sweden)

Dongping Chen

2018-03-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2018-03-31

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

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

Science.gov (United States)

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

2017-02-01

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

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.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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.

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

International Nuclear Information System (INIS)

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

2011-01-01

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

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

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

International Nuclear Information System (INIS)

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

2013-01-01

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

Facile Synthesis of Ternary Boron Carbonitride Nanotubes

Directory of Open Access Journals (Sweden)

Luo Lijie

2009-01-01

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

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

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

International Nuclear Information System (INIS)

M, Sandhyarani; T, Prasadrao; N, Rameshbabu

2014-01-01

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

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.

Superconductive transition metal carbonitride fibers and method for the preparation thereof

International Nuclear Information System (INIS)

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

1976-01-01

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

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

Directory of Open Access Journals (Sweden)

Boby John

2013-06-01

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

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

International Nuclear Information System (INIS)

Garcia, J.; Lengauer, W.

2001-01-01

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

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

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

International Nuclear Information System (INIS)

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

2017-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2017-02-01

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

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

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)

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

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.

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

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

Science.gov (United States)

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

2014-04-01

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

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

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

International Nuclear Information System (INIS)

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

1980-01-01

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

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)

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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.

Process for electrolytic deposition of metals on zirconium materials

International Nuclear Information System (INIS)

Donaghy, R.E.

1981-01-01

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

Synthesis and cathodoluminescence characterization of ZrO2:Er3+ films

International Nuclear Information System (INIS)

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

2014-01-01

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

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)

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...

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

Directory of Open Access Journals (Sweden)

Ming-Zhi Yang

2013-03-01

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

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

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

Process for purifying zirconium sponge

International Nuclear Information System (INIS)

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

1992-01-01

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

Contribution to the study of zirconium self-diffusion in zirconium carbide

International Nuclear Information System (INIS)

An, Chul

1972-01-01

The objective of this research thesis is to determine experimental conditions allowing the measurement of the self-diffusion coefficient of zirconium in zirconium carbide. The author reports the development of a method of preparation of zirconium carbide samples. He reports the use of ion implantation as technique to obtain a radio-tracer coating. The obtained results give evidence of the impossibility to use sintered samples with small grains because of the demonstrated importance of intergranular diffusion. The self-diffusion coefficient is obtained in the case of zirconium carbide with grains having a diameter of few millimetres. The presence of 95 Nb from the disintegration of 95 Zr indicates that these both metallic elements have very close diffusion coefficients at 2.600 C [fr

Dissolving of Nb and Ti carbonitride precipitates in microalloyed steels

Institute of Scientific and Technical Information of China (English)

Wenjin Nie; Shanwu Yang; Shaoqiang Yuan; Xinlai He

2003-01-01

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

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

Science.gov (United States)

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

2013-01-01

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

Thermal behaviour of nitrogen implanted into zirconium

International Nuclear Information System (INIS)

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

1994-01-01

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

Artefacts in multimodal imaging of titanium, zirconium and binary titanium-zirconium alloy dental implants: an in vitro study.

Science.gov (United States)

Smeets, Ralf; Schöllchen, Maximilian; Gauer, Tobias; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

2017-02-01

To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium-zirconium alloy dental implants. Zirconium, titanium and titanium-zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line-distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. While titanium and titanium-zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium-zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium-zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium-zirconium alloy induced more severe artefacts than zirconium and titanium. MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium-zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting.

Artefacts in multimodal imaging of titanium, zirconium and binary titanium–zirconium alloy dental implants: an in vitro study

Science.gov (United States)

Schöllchen, Maximilian; Aarabi, Ghazal; Assaf, Alexandre T; Rendenbach, Carsten; Beck-Broichsitter, Benedicta; Semmusch, Jan; Sedlacik, Jan; Heiland, Max; Fiehler, Jens; Siemonsen, Susanne

2017-01-01

Objectives: To analyze and evaluate imaging artefacts induced by zirconium, titanium and titanium–zirconium alloy dental implants. Methods: Zirconium, titanium and titanium–zirconium alloy implants were embedded in gelatin and MRI, CT and CBCT were performed. Standard protocols were used for each modality. For MRI, line–distance profiles were plotted to quantify the accuracy of size determination. For CT and CBCT, six shells surrounding the implant were defined every 0.5 cm from the implant surface and histogram parameters were determined for each shell. Results: While titanium and titanium–zirconium alloy induced extensive signal voids in MRI owing to strong susceptibility, zirconium implants were clearly definable with only minor distortion artefacts. For titanium and titanium–zirconium alloy, the MR signal was attenuated up to 14.1 mm from the implant. In CT, titanium and titanium–zirconium alloy resulted in less streak artefacts in comparison with zirconium. In CBCT, titanium–zirconium alloy induced more severe artefacts than zirconium and titanium. Conclusions: MRI allows for an excellent image contrast and limited artefacts in patients with zirconium implants. CT and CBCT examinations are less affected by artefacts from titanium and titanium–zirconium alloy implants compared with MRI. The knowledge about differences of artefacts through different implant materials and image modalities might help support clinical decisions for the choice of implant material or imaging device in the clinical setting. PMID:27910719

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

Theoretical Investigations of the Hexagonal Germanium Carbonitride

Directory of Open Access Journals (Sweden)

Xinhai Yu

2018-04-01

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

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

Experimental studies of relevance on zirconium nitrate raffinate sludge for its disposal as well as zirconium recovery

International Nuclear Information System (INIS)

Brahmananda Reddy, G.; Narasimha Murty, B.; Ravindra, H.R.

2013-01-01

One of the many routes of production of nuclear grade zirconium dioxide involve separation of zirconium and hafnium by solvent extraction of zirconium nitrate using tri-n-butyl phosphate followed by precipitation of zirconium with ammonia and finally calcination of the so obtained hydrated zirconia at elevated temperature. The zirconium feed solution as is generated from digestion of zirconium washed dried frit (produced by the caustic fusion of zircon sand which is one of the beach sand heavy minerals) in nitric acid contain considerable amount of sludge material and after solvent extraction this whole sludge material rests with raffinate. This sludge material has a scope to contain considerable amounts of zirconium along with other metal ions such as hafnium, aluminium, iron, etc. besides nitric acid and it constitutes one of the important solid wastes that needs to be disposed suitably. One of the disposal means of this sludge material is to use it as a land fill for which two important criteria are to be viz the pH of 10% solid waste solution should be near to neutral pH and the loss on ignition at 550℃ on dry basis of the sludge to be below 20%. In order to study the implications of presence of varying amounts of zirconium nitrate in the sludge on the pH of 10% solution of the sludge various synthetic zirconium nitrate solid waste were prepared using the sludge material generated at the laboratory during the analysis of zirconium washed dried frit. Presence of zirconium in the sludge is expected to decrease the overall pH of the 10% solution of the sludge because zirconium is prone to hydrolyze especially locally when zirconium ion comes into contact with water according to the chemical equation Zr 4+ H 2 O → ZrO 2+ + 2H + . From this equation, it is clear that for every one mole of zirconium ions two moles of hydrogen ions are produced. This is verified experimentally using the synthetically prepared sludge materials with varying amounts of zirconium

Localized deformation of zirconium-liner tube

International Nuclear Information System (INIS)

Nagase, Fumihisa; Uchida, Masaaki

1988-03-01

Zirconium-liner tube has come to be used in BWR. Zirconium liner mitigates the localized stress produced by the pellet-cladding interaction (PCI). In this study, simulating the ridging, stresses were applied to the inner surfaces of zirconium-liner tubes and Zircaloy-2 tubes, and, to investigate the mechanism and the extent of the effect, the behavior of zirconium liner was examined. As the result of examination, stress was concentrated especially at the edge of the deformed region, where zirconium liner was highly deformed. Even after high stress was applied, the deformation of Zircaloy part was small, since almost the concentrated stress was mitigated by the deformation of zirconium liner. In addition, stress and strain distributions in the cross section of specimen were calculated with a computer code FEMAXI-III. The results also showed that zirconium liner mitigated the localized stress in Zircaloy, although the affected zone was restricted to the region near the boundary between zirconium liner and Zircaloy. (author)

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...

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

Zirconium isotope separation process

International Nuclear Information System (INIS)

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

1988-01-01

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

Zirconium for nitric acid solutions

International Nuclear Information System (INIS)

Yau, T.L.

1984-01-01

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

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

Science.gov (United States)

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

2016-05-01

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

Experimental and thermodynamic study of the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems

International Nuclear Information System (INIS)

Jourdan, J.

2009-11-01

This work is a contribution to the development of innovative concepts for fuel cladding in pressurized water nuclear reactors. This concept implies the insertion of rare earth (erbium and gadolinium) in the zirconium fuel cladding. The determination of phase equilibria in the systems is essential prior to the implementation of such a promising solution. This study consisted in an experimental determination of the erbium-zirconium phase diagram. For this, we used many different techniques in order to obtain diagram data such as solubility limits, solidus, liquidus or invariant temperatures. These data allowed us to present a new diagram, very different from the previous one available in the literature. We also assessed the diagram using the CALPHAD approach. In the gadolinium-zirconium system, we determined experimentally the solubility limits. Those limits had never been determined before, and the values we obtained showed a very good agreement with the experimental and assessed versions of the diagram. Because these alloys are subjected to oxygen diffusion throughout their life, we focused our attention on the erbium-oxygen-zirconium and gadolinium-oxygen-zirconium systems. The first system has been investigated experimentally. The alloys fabrication has been performed using powder metallurgy. In order to obtain pure raw materials, we fabricated powder from erbium and zirconium bulk metals using hydrogen absorption/desorption. The characterisation of the ternary pellets allowed the determination of two ternary isothermal sections at 800 and 1100 C. For the gadolinium-oxygen-zirconium system, we calculated the phase equilibria at temperatures ranging from 800 to 1100 C, using a homemade database compiled from literature assessments of the oxygen-zirconium, gadolinium-zirconium and gadolinia-zirconia systems. Finally, we determined the mechanical properties, in connexion with the microstructure, of industrial quality alloys in order to identify the influence of

Process for etching zirconium metallic objects

International Nuclear Information System (INIS)

Panson, A.J.

1988-01-01

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

Zirconium and cast zirconium

Energy Technology Data Exchange (ETDEWEB)

Krone, K

1977-04-01

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

Synthesis of zirconium by zirconium tetrachloride reduction by magnesio-thermia. Experimental study and modelling

International Nuclear Information System (INIS)

Basin, N.

2001-01-01

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

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

Science.gov (United States)

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

2001-01-01

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

Neutron activation of chlorine in zirconium and zirconium alloys use of the matrix as comparator

International Nuclear Information System (INIS)

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

1981-01-01

A procedure is described for neutron activation analysis of chlorine in zirconium and zirconium alloys. Calculation of chlorine concentration is performed relative to zirconium concentration in the matrix in order to minimize effects of differences in irradiation and counting geometry. Principles of the method and the results obtained are discussed. (author)

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

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.)

Protection of zirconium and its alloys by metallic coatings

International Nuclear Information System (INIS)

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

1968-01-01

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

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

International Nuclear Information System (INIS)

Cox, B.

1987-03-01

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

Modification in band gap of zirconium complexes

Energy Technology Data Exchange (ETDEWEB)

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

2016-05-06

The optical properties of zirconium complexes with amino acid based Schiff bases are reported here. The zirconium complexes show interesting stereo chemical features, which are applicable in organometallic and organic synthesis as well as in catalysis. The band gaps of both Schiff bases and zirconium complexes were obtained by UV-Visible spectroscopy. It was found that the band gap of zirconium complexes has been modified after adding zirconium compound to the Schiff bases.

Method to precipitate metals on zirconium articles without using current

International Nuclear Information System (INIS)

Donaghy, R.E.

1978-01-01

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

Plasma arc melting of zirconium

International Nuclear Information System (INIS)

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

1997-01-01

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

Comparison of different methods for measuring the passive film thickness on metals

International Nuclear Information System (INIS)

Benoit, Marie; Bataillon, Christian; Gwinner, Benoit; Miserque, Frédéric; Orazem, Mark E.; Sánchez-Sánchez, Carlos M.; Tribollet, Bernard; Vivier, Vincent

2016-01-01

Highlights: • In situ EIS and ex situ XPS were used for the characterization of zirconium oxide films. • The film thicknesses can be obtained from the analysis of a single EIS diagram. • A convenient graphical method to extract film properties is proposed. - Abstract: In situ electrochemical impedance spectroscopy (EIS) and ex situ X-ray photoelectron spectroscopy (XPS) measurements on electrogenerated zirconium oxide films on zirconium (Zr/ZrO_2) were used to quantify the oxide film thickness and resistivity profiles through the oxide. The EIS analysis presented here takes advantage of the high-frequency domain at which the constant-phase element (CPE) behavior of the oxide film reverts to a capacitive response and the Cole-Cole representations of the complex capacitance to extract the high-frequency capacitance of the oxide film without reference to the nature of the time-constant distribution within the oxide film. The film thickness of the ZrO_2 samples measured from the high-frequency capacitance of EIS were in good agreement with the thickness obtained from XPS. Moreover, the EIS analysis presented is based on the use of the integral solution of the power law model, which allows to obtain in one single EIS experiment, both the film thickness and the resistivity profile in the ZrO_2 film. This work suggests a convenient graphical method to extract film properties and serves to validate a key assumption of the power-law model for interpretation of CPE parameters in terms of physical properties.

Anticorrosion ion implantation of fragments of zirconium fuel can specimens

International Nuclear Information System (INIS)

Kalin, B.A.; Osipov, V.V.; Volkov, N.V.; Khernov, V.Yu.

2001-01-01

Aimed at the study of specific features of oxide film formation in the initial stage of Eh110 and Eh635 alloy fuel can oxidation the modification of tubular specimen surfaces is performed using an ion mixing technique, and the structure of oxide films produced in a steam-water environment is investigated. Using the method of vacuum vapor deposition the outer surface of specimens is coated with alloying element films irradiated by a polyenergetic Ar + ion beam with a 10 keV mean energy up to radiation doses of (7-10) x 10 17 ion/cm 2 . Monatomic (Al, Fe, Cu, Cr, Mo, Sn) or diatomic (Al-Fe, Al-Mo, Al-Sn, Fe-Cu, Fe-Mo, Fe-Sn, Cr-Mo, Cr-Sn) implantation into a zirconium cladding occurs under irradiation effect. The positive influence of combined intrusion of Al and other elements is revealed. The presence of Al atoms enhances the oxide film structure. The least ZeO 2 film thickness is observed when alloying with molybdenum, Al-Fe, Al-Mo and Al-Sn [ru

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

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)

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-12-01

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

Zirconium behaviour in purex process solutions

International Nuclear Information System (INIS)

Shu, J.

1982-01-01

The extraction behaviour of zirconium, as fission product, in TBP/diluent- HNO 3 -H 2 O systems, simulating Purex solutions, is studied. The main purpose is to attain an increasing in the zirconium decontamination factor by adjusting the extraction parameters. Equilibrium diagram, TBP concentration, aqueous:organic ratio, salting-out effects and, uranium loading in the organic phase were the main factors studied. All these experiments had been made with zirconium in the 10 - 2 - 10 - 3 concentration range. The extractant degradation products influence uppon the zirconium behaviour was also verified. With the obtained data it was possible to introduce some modification in the standard Purex flow-sheet in order to obtain the uranium product with higher zirconium decontamination. (Author) [pt

Anisotropy of mechanical properties of zirconium and zirconium alloys

International Nuclear Information System (INIS)

Medrano, R.E.

1975-01-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Corrosion-electrochemical behavior of zirconium in molten alkali metal carbonates

Science.gov (United States)

Nikitina, E. V.

2016-08-01

The corrosion and electrochemical characteristics of zirconium during its interaction with molten lithium, sodium, and potassium carbonates containing from 1 to 5 wt % additives to the salt phase are studied in a temperature range of 500-800°C using gravimetry, corrosion potential measurement, and anodic polarization. The substances decreasing the corrosion losses due to the strengthening and thickening of an oxide film (lithium, sodium, potassium hydroxides) are used as passivators. Sodium chloride, fluoride, and sulfate serve as corrosion stimulators (activators).

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)

New solvent extraction process for zirconium and hafnium

International Nuclear Information System (INIS)

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

1984-01-01

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

Fine-grained zirconium-base material

Science.gov (United States)

Van Houten, G.R.

1974-01-01

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

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Microhardness and microplasticity of zirconium nitride

International Nuclear Information System (INIS)

Neshpor, V.S.; Eron'yan, M.A.; Petrov, A.N.; Kravchik, A.E.

1978-01-01

To experimentally check the concentration dependence of microhardness of 4 group nitrides, microhardness of zirconium nitride compact samples was measured. The samples were obtained either by bulk saturation of zirconium iodide plates or by chemical precipitation from gas. As nitrogen content decreased within the limits of homogeneity of zirconium nitride samples where the concentration of admixed oxygen was low, the microhardness grew from 1500+-100 kg/mm 2 for ZrNsub(1.0) to 27000+-100 kg/mm 2 for ZrNsub(0.78). Microplasticity of zirconium nitride (resistance to fracture) decreased, as the concentration of nitrogen vacancies was growing

SEPARATION OF HAFNIUM FROM ZIRCONIUM

Science.gov (United States)

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

1960-05-31

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

Zirconium

Science.gov (United States)

Bedinger, G.M.

2013-01-01

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

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.

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

Difference in surface reactions between titanium and zirconium in Hanks' solution to elucidate mechanism of calcium phosphate formation on titanium using XPS and cathodic polarization

International Nuclear Information System (INIS)

Tsutsumi, Y.; Nishimura, D.; Doi, H.; Nomura, N.; Hanawa, T.

2009-01-01

Titanium and zirconium were immersed in Hanks' solution with and without calcium and phosphate ions, and the surfaces were characterized with X-ray photoelectron spectroscopy (XPS) to determine the mechanism of calcium phosphate formation on titanium in simulated body fluids and in a living body. In addition, they were cathodically polarized in the above solutions. XPS characterization and cathodic polarization revealed differences in the surface properties in the ability of calcium phosphate formation between titanium and zirconium. The surface oxide film on titanium is not completely oxidized and is relatively reactive; that on zirconium is more passive and protective than that on titanium. Neither calcium nor phosphate stably exists alone on titanium, and calcium phosphate is naturally formed on it; calcium phosphate formed on titanium is stable and protective. On the other hand, calcium is never incorporated on zirconium, while zirconium phosphate, which is easily formed on zirconium, is highly stable and protective. Our study presents new information regarding the surface property of titanium and demonstrates that the characteristics of titanium and zirconium may be applied to various medical devices and new surface modification techniques.

Solvent extraction of zirconium

International Nuclear Information System (INIS)

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

1981-01-01

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

Purification of zirconium concentrates

International Nuclear Information System (INIS)

Brown, A.E.P.

1976-01-01

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

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

Thermofluency in zirconium alloys

International Nuclear Information System (INIS)

Orozco M, E.A.

1976-01-01

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

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

International Nuclear Information System (INIS)

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

1977-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1957-07-01

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

40 CFR 721.9973 - Zirconium dichlorides (generic).

Science.gov (United States)

2010-07-01

... 40 Protection of Environment 30 2010-07-01 2010-07-01 false Zirconium dichlorides (generic). 721... Substances § 721.9973 Zirconium dichlorides (generic). (a) Chemical substance and significant new uses subject to reporting. (1) The chemical substances identified generically as zirconium dichlorides (PMNs P...

Molten salt scrubbing of zirconium or hafnium tetrachloride

International Nuclear Information System (INIS)

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

1990-01-01

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

Advances in zirconium technology for nuclear reactor application

International Nuclear Information System (INIS)

Ganguly, C.

2002-01-01

Zirconium alloys are extensively used as a material for cladding nuclear fuels and for making core structurals of water-cooled nuclear power reactors all over the world for generation of nearly 16 percent of the worlds electricity. Only four countries in the world, namely France, USA, Russia and India, have large zirconium industry and capability to manufacture reactor grade zirconium sponge, a number of zirconium alloys and a wide variety of structural components for water cooled nuclear reactor. The present paper summarises the status of zirconium technology and highlights the achievement of Nuclear Fuel Complex during the last ten years in developing a wide variety of zirconium alloys and components for water-cooled nuclear power programme

Applications for zirconium and columbium alloys

International Nuclear Information System (INIS)

Condliff, A.F.

1986-01-01

Currently, zirconium and columbium are used in a wide range of applications, overlapping only in the field of corrosion control. As a construction material, zirconium is primarily used by the nuclear power industry. The use of zirconium in the chemical processing industry (CPI) is, however, increasing steadily. Columbian alloys are primarily applied as superconducting alloys for research particle accelerators and fusion generators as well as in magnetic resonance imaging for medical diagnosis

The development of zirconium alloy and its manufacturing

International Nuclear Information System (INIS)

Yuan Gaihuan; Yue Qiang

2015-01-01

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

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

Oxidized zirconium on ceramic; Catastrophic coupling.

Science.gov (United States)

Ozden, V E; Saglam, N; Dikmen, G; Tozun, I R

2017-02-01

Oxidized zirconium (Oxinium™; Smith & Nephew, Memphis, TN, USA) articulated with polyethylene in total hip arthroplasty (THA) appeared to have the potential to reduce wear dramatically. The thermally oxidized metal zirconium surface is transformed into ceramic-like hard surface that is resistant to abrasion. The exposure of soft zirconium metal under hard coverage surface after the damage of oxidized zirconium femoral head has been described. It occurred following joint dislocation or in situ succeeding disengagement of polyethylene liner. We reported three cases of misuse of Oxinium™ (Smith & Nephew, Memphis, TN, USA) heads. These three cases resulted in catastrophic in situ wear and inevitable failure although there was no advice, indication or recommendation for this use from the manufacturer. Copyright © 2016 Elsevier Masson SAS. All rights reserved.

Electrochemical-metallothermic reduction of zirconium in molten salt solutions

International Nuclear Information System (INIS)

McLaughlin, D.F.; Talko, F.

1990-01-01

This patent describes a method for separating hafnium from zirconium of the type wherein a feed containing zirconium and hafnium chlorides is prepared from zirconium-hafnium chloride and the feed is introduced into a distillation column, which distillation column has a reboiler connected at the bottom and a reflux condenser connected at the top and wherein a hafnium chloride enriched stream is taken from the top of the column and a zirconium enriched chloride stream is taken from the bottom of the column. It comprises: reducing the zirconium enriched chloride stream taken from the distillation column to metal by electrochemically reducing an alkaline earth metal in a molten salt bath with the molten salt in the molten salt bath consisting essentially of a mixture of at least one alkali metal chloride and at least one alkaline earth metal chloride and zirconium chloride, with the reduced alkaline earth metal reacting with the zirconium chloride to produce zirconium metal and alkaline earth metal chloride

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

Directory of Open Access Journals (Sweden)

Haitao Li

2016-12-01

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

Problems of zirconium metal production in Czechoslovakia

International Nuclear Information System (INIS)

Vareka, J.; Vaclavik, E.

1975-01-01

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

Zirconium coatings doped with nanoparticles for the protection of stainless steel

International Nuclear Information System (INIS)

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

2008-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2015-02-01

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

Dry And Ringer Solution Lubricated Tribology Of Thin Osseoconductive Metal Oxides And Diamond-Like Carbon Films

Directory of Open Access Journals (Sweden)

Waldhauser W.

2015-09-01

Full Text Available Achieving fast and strong adhesion to jawbone is essential for dental implants. Thin deposited films may improve osseointegration, but they are prone to cohesive and adhesive fracture due to high stresses while screwing the implant into the bone, leading to bared, less osteoconductive substrate surfaces and nano- and micro-particles in the bone. Aim of this work is the investigation of the cohesion and adhesion failure stresses of osteoconductive tantalum, titanium, silicon, zirconium and aluminium oxide and diamond-like carbon films. The tribological behaviour under dry and lubricated conditions (Ringer solution reveals best results for diamond-like carbon, while cohesion and adhesion of zirconium oxide films is highest.

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

International Nuclear Information System (INIS)

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

2000-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Lagerberg, G

1961-04-15

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

The fluorimetric titration of zirconium in the ppm-range

International Nuclear Information System (INIS)

Linden, W.E. von der; Boef, G. den; Ozinga, W.

1976-01-01

A fluorimetric titration of zirconium(IV) with EDTA is proposed. The fluorescence intensity of the zirconium-morin complex is used to indicate the end-point. More than twenty other cations were investigated and it was found that they did not interfere, neither did common anions. Mercury(II) can only be tolerated in amount not exceeding that of zirconium. Bismuth(III) interferes and hafnium(IV0 is titrated together with zirconium. The relative standard deviation of the titration of 10ml of a solution containing 1 ppm of zirconium does not exceed 1.5%

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

Energy Technology Data Exchange (ETDEWEB)

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

2016-04-15

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

SEPARATING HAFNIUM FROM ZIRCONIUM

Science.gov (United States)

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

1956-08-21

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

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)

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

International Nuclear Information System (INIS)

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

1984-01-01

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

Study for the chlorination of zirconium oxide

International Nuclear Information System (INIS)

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

1990-12-01

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

Ductile zirconium powder by hydride-dehydride process

Energy Technology Data Exchange (ETDEWEB)

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

1976-09-01

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

Joint titrimetric determination of zirconium and hafnium

International Nuclear Information System (INIS)

Vazquez, Cristina; Botbol, Moises; Bianco de Salas, G.N.; Cornell de Casas, M.I.

1980-01-01

A method for the joint titrimetric determination of zirconium and hafnium, which are elements of similar chemical behaviour, is described. The disodic salt of the ethylendiaminetetracetic acid (EDTA) is used for titration, while xilenol orange serves as final point indicator. Prior to titration it is important to evaporate with sulfuric acid, the solution resulting from the zirconium depolymerization process, to adjust the acidity and to eliminate any interferences. The method, that allows the quick and precise determination of zirconium and hafnium in quantities comprised between 0.01 and mg, was applied to the analysis of raw materials and of intermediate and final products in the fabrication of zirconium sponge and zircaloy. (M.E.L.) [es

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

International Nuclear Information System (INIS)

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

2011-01-01

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

Voltammetric determination of zirconium using azo compounds

International Nuclear Information System (INIS)

Orshulyak, O.O.; Levitskaya, G.D.

2008-01-01

The optimum conditions for zirconium complexation with azo compounds are found. The applicability of Eriochrome Red B, Calcon, and Calcion to the voltammetric determination of zirconium, total Zr(IV) and Hf(IV), and Zr(IV) in the presence of Zn(II), Cu(II), Cd(II), Ni(II), or Ti(IV) is demonstrated. The developed procedures are used to determine zirconium in a terbium alloy and in an alloy for airplane wheel drums [ru

URANIUM DECONTAMINATION WITH RESPECT TO ZIRCONIUM

Science.gov (United States)

Vogler, S.; Beederman, M.

1961-05-01

A process is given for separating uranium values from a nitric acid aqueous solution containing uranyl values, zirconium values and tetravalent plutonium values. The process comprises contacting said solution with a substantially water-immiscible liquid organic solvent containing alkyl phosphate, separating an organic extract phase containing the uranium, zirconium, and tetravalent plutonium values from an aqueous raffinate, contacting said organic extract phase with an aqueous solution 2M to 7M in nitric acid and also containing an oxalate ion-containing substance, and separating a uranium- containing organic raffinate from aqueous zirconium- and plutonium-containing extract phase.

Effects of titanium and zirconium on iron aluminide weldments

Energy Technology Data Exchange (ETDEWEB)

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

1997-12-01

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

Production of nuclear grade zirconium: A review

Energy Technology Data Exchange (ETDEWEB)

Xu, L., E-mail: L.Xu-2@tudelft.nl [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands); Xiao, Y. [Department of Metallurgical Engineering, Anhui University of Technology, Ma' anshan 243002 (China); Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Sandwijk, A. van [Zr-Hf-Ti Metallurgie B.V., Den Haag 2582 SB (Netherlands); Xu, Q. [School of Materials Science and Metallurgy, Northeastern University, Shenyang 110004 (China); Yang, Y. [Department of Materials Science and Engineering, Delft University of Technology, Delft 2628 CD (Netherlands)

2015-11-15

Zirconium is an ideal material for nuclear reactors due to its low absorption cross-section for thermal neutrons, whereas the typically contained hafnium with strong neutron-absorption is very harmful for zirconium as a fuel cladding material. This paper provides an overview of the processes for nuclear grade zirconium production with emphasis on the methods of Zr–Hf separation. The separation processes are roughly classified into hydro- and pyrometallurgical routes. The known pyrometallurgical Zr–Hf separation methods are discussed based on the following reaction features: redox characteristics, volatility, electrochemical properties and molten salt–metal equilibrium. In the present paper, the available Zr–Hf separation technologies are compared. The advantages and disadvantages as well as future directions of research and development for nuclear grade zirconium production are discussed.

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.

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

Review of zirconium-zircaloy pyrophoricity

International Nuclear Information System (INIS)

Cooper, T.D.

1984-11-01

Massive zirconium metal scrap can be handled, shipped, and stored with no evidence of combustion or pyrophoricity hazards. Mechanically produced fine scrap such as shavings, turnings, or powders can burn but are not pyrophoric unless the particle diameter is less than 54 μm. Powders with particle diameters less than 54 μm can be both pyrophoric and explosive. Pyrophoric powders should be collected and stored underwater or under inert gas cover to reduce the flammability hazard. Opening sealed containers of zirconium stored underwater should be attempted with caution since hydrogen may be present. The factors that influence the ignition temperature have been explored in depth and recommendations are included for the safe handling, shipping, and storage of pyrophoric or flammable zirconium. 29 refs., 5 figs., 6 tabs

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.)

Removal of iron contaminant from zirconium chloride solution

International Nuclear Information System (INIS)

Voit, D.O.

1992-01-01

This patent describes a process for eliminating iron contaminant from an aqueous zirconium chloride solution that has been contaminated with FeCl 3 in a plant in which zirconium and hafnium chloride solutions are separated by a main MINK solvent extraction system and the FeCl 3 is normally removed from the zirconium chloride solution by a secondary MINK solvent extraction system

Effect of the substrate temperature on the microstructure and texture of Mg90Zr10 (at.%) films deposited by sputtering

International Nuclear Information System (INIS)

Garces, Gerardo; Landais, Stephan; Adeva, Paloma

2006-01-01

The microstructure of Mg 90 Zr 10 (at.%) films obtained by sputtering onto copper substrate at three different temperatures (180, 320 and 350 deg. C) has been studied. Films exhibited an intense (0 0 0 1) basal plane fibre texture with the fibre axis parallel to the growth direction. Their microstructure consisted of columnar grains growing from the copper substrate to the free surface which is typical of the zone II of the Movchan and Demchishin zone model developed for PVD materials. Nevertheless, the microstructure of films was dependent on the substrate temperature. The grain diameter increased as the substrate temperature was increased. Moreover, the dislocation density inside the grains as well as that piled-up forming sub-grain boundaries decreased as the deposition temperature increased. Although the film growth in zone II is controlled by surface diffusion the larger surface mobility of the atoms as the substrate temperature increased led to changes in the solubility of zirconium. At low substrate temperatures all zirconium was in solid solution. However, at 350 deg. C the formation of small zirconium particles occurred at grain boundaries

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

High purity zirconium obtainment through the iodine compounds transport method

International Nuclear Information System (INIS)

Bolcich, J.C.; Zuzek, E.; Dutrus, S.M.; Corso, H.L.

1987-01-01

This paper describes the experimental method and the equipment designed, constructed and actually applied for the high purity zirconium obtainment from a zirconium sponge of the nuclear type. The mechanism of purification is based on the impure metal attack with gaseous iodine (at 200 deg C) to obtain zirconium tetra iodine as main product which is then transformed into a pure zirconium base (at 1000-1300 deg C), precipitating the metallic zirconium and releasing the gaseous iodine. From the first experiences carried out, pure zirconium has been obtained from an initial filament of 0.5 mm of diameter as well as wires up to 2.5 mm of diameter. This work presents the results from the studies and analysis made to characterize the material obtained. Finally, the refining methods to which the zirconium produced may be submitted so as to optimize the final purity are discussed. (Author)

Quercetin as colorimetric reagent for determination of zirconium

Science.gov (United States)

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

1953-01-01

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

Antimony removal from aqueous solutions using Zirconium hydroxide

International Nuclear Information System (INIS)

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

2016-01-01

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

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.

Molten salt extractive distillation process for zirconium-hafnium separation

International Nuclear Information System (INIS)

McLaughlin, D.F.; Stoltz, R.A.

1989-01-01

This patent describes an improvement in a process for zirconium-hafnium separation. It utilizes an extractive distillation column with a mixture of zirconium and hafnium tetrachlorides introduced into a distillation column having a top and bottom with hafnium enriched overheads taken from the top of the column and a molten salt solvent circulated through the column to provide a liquid phase, and with molten salt solvent containing zirconium chloride being taken from the bottom of the distillation column. The improvements comprising: utilizing a molten salt solvent consisting principally of lithium chloride and at least one of sodium, potassium, magnesium and calcium chlorides; stripping of the zirconium chloride taken from the bottom of the distillation column by electrochemically reducing zirconium from the molten salt solvent; and utilizing a pressurized reflux condenser on the top of the column to add the hafnium chloride enriched overheads to the molten salt solvent previously stripped of zirconium chloride

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)

Intercalation chemistry of zirconium 4-sulfophenylphosphonate

International Nuclear Information System (INIS)

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

2013-01-01

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

Chemistry of titanium, zirconium and thorium picramates

International Nuclear Information System (INIS)

Srivastava, R.S.; Agrawal, S.P.; Bhargava, H.N.

1976-01-01

Picramates of titanium, zirconium and thorium are prepared by treating the aqueous sulphate, chloride and nitrate solutions with sodium picramate. Micro-analysis, colorimetry and spectrophotometry are used to establish the compositions (metal : ligand ratio) of these picramates as 1 : 2 (for titanium and zirconium) and 1 : 4 (for thorium). IR studies indicate H 2 N → Me coordination (where Me denotes the metal). A number of explosive properties of these picramates point to the fact that the zirconium picramate is thermally more stable than the picramates of titanium and thorium. (orig.) [de

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

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Science.gov (United States)

2010-04-01

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

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

Zirconium alloy fuel cladding resistant to PCI crack propagation

International Nuclear Information System (INIS)

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

1987-01-01

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

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

Processing fissile material mixtures containing zirconium and/or carbon

Science.gov (United States)

Johnson, Michael Ernest; Maloney, Martin David

2013-07-02

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

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

Analysis of hydrogen in zirconium metallic

International Nuclear Information System (INIS)

Rodrigues, A.N.; Vega Bustillos, J.O.W.

1991-02-01

Determination of hydrogen in zirconium metallic have been performed using the hot vacuum extraction system and the gas chromatographic technique. The zirconium metallic samples were hydrieded by electrolitic technique at difference temperatures and times, then the samples were annealing at vacuum and eatching by fluoridric acid solution. The details of the hydrieded process, analytical technique and the data obtained are discussed. (author)

Development of zirconium hydride highly effective moderator materials

International Nuclear Information System (INIS)

Yin Changgeng

2005-10-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1955-07-01

About the separation different processes of zirconium-hafnium, the extraction by solvent in cross-current is the most easily the process usable on an industrial scale. It uses tributyl phosphate as solvent, diluted with white spirit to facilitate the decanting. Some exploratory tests showed that nitric environment seemed the most favorable for extraction; but a lot of other factors intervene in the separation process. We studied the influence of the acidity successively, the NO{sub 3}{sup -} ions concentration, the role of the cation coming with NO{sub 3}{sup -}, as well as the influence of the concentration of zirconium in the solution on the separation coefficient {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (M.B.) [French] Des differents procedes de separation zirconium-hafnium, l'extraction par solvant en contre-courant est le procede le plus facilement utilisable a l'echelle industrielle. On utilise comme solvant le phosphate de tributyle, dilue avec du white spirit pour faciliter les decantations. Des essais preliminaires ont montre que le milieu nitrique semblait le plus favorable a l'extraction; mais beaucoup d'autres facteurs interviennent dans le processus de separation. Nous avons etudie successivement l'influence de l'acidite, celle de la concentration en ions NO{sub 3}{sup -}, le role du cation accompagnant NO{sub 3}{sup -}, ainsi que l'influence de la concentration en zirconium de la solution sur le coefficient de separation {beta} = {alpha}{sub Zr} / {alpha}{sub Hf}. (MB)

A study of the fixing of phosphoric ions by zirconium-montmorillonite; Etude de la fixation d'ions phosphoriques par la montmorillonite-zirconium

Energy Technology Data Exchange (ETDEWEB)

Bittel, R; Boursat, C; Platzer, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1960-07-01

In connection with the research carried out on the purification of nuclear reactor water, we have undertaken a study of the ion-exchange properties of acid montmorillonite. In a previous paper, we described the preparation of zirconium-montmorillonite small plate. The present article aims to study some of the properties of the clay obtained. We have observed that zirconium-montmorillonite fixes very strongly the phosphorus from solutions of phosphoric acid or of phosphates: on 1 g of clay it is possible to fix 1,2 milli-atoms-gram of zirconium and the zirconium montmorillonite itself fixes 2,1 milli-atoms-gram of phosphorus. An explanation of these experimental results, which is as much chemical as mineralogical, is the hypothesis that the fixing of phosphoric ions modifies the distribution of the ions between the platelets and precipitates a very slightly soluble product of the type diphospho-zirconic acid. (author) [French] En rapport avec des recherches sur I'epuration de l'eau des reacteurs nucleaires nous avons entrepris une etude sur les proprietes d'echangeur d'ions de la montmorillonite-acide. Dans une precedente publication, nous avons decrit la preparation des plaquettes de montmorillonite-zirconium. La presente communication a pour but d'etudier quelques proprietes de l'argile obtenue. Nous avons constate que la montmorilionite-zirconium fixe le phosphore de solutions d'acide phosphorique ou de phosphate avec une grande intensite: sur 1 g d'argile, on peut fixer 1,2 atomes-gramme de zirconium, et la montmorillonite-zirconium fixe a son tour 2,1 milli-atomesgramme de phosphore. Une explication des resultats experimentaux, tant d'ordre chimique que d'ordre mineralogique, consiste en l'hypothese suivant laquelle la fixation d'ions phosphoriques modifierait la repartition des ions entre les feuillets avec precipitation du compose tres peu soluble (type: acide diphosphozirconique). (auteur)

A computation model for the corrosion resistance of nanocrystalline zirconium metal

International Nuclear Information System (INIS)

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

2007-01-01

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

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

Science.gov (United States)

2010-07-01

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

Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

International Nuclear Information System (INIS)

McLaughlin, D.F.

1989-01-01

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

Low cycle fatigue behaviour of zirconium alloys at 3000C

International Nuclear Information System (INIS)

Hosbons, R.R.

1975-01-01

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

Low cycle fatigue behaviour of zirconium alloys at 3000C

International Nuclear Information System (INIS)

Hosbons, R.R.

1975-01-01

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

RECOVERY OF URANIUM FROM ZIRCONIUM-URANIUM NUCLEAR FUELS

Science.gov (United States)

Gens, T.A.

1962-07-10

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

Luminescent properties in films of ZrO2: Dy

International Nuclear Information System (INIS)

Martinez, R. C.; Guzman, J.; Rivera, T.; Ceron, P.; Montes, E.; Guzman, D.; Garcia H, M.; Falcony, C.; Azorin, J.

2014-08-01

In this work the luminescent characterization of zirconium oxide (ZrO 2 ) films impure with dysprosium (Dy +3 ) is reported, obtained by means of the ultrasonics spray pyrolysis technique. The films were deposited on glass substrates (Corning), in a temperatures interval of 400 to 550 grades C, using as precursor elements Zirconium oxide chloride octahydrate (ZrOCl 2 ·8H 2 O) and Dysprosium tri-chloride (DyCl 3 ), dissolved in deionized water, varying the concentration of the contaminated from the 1 to 20 atomic % with relationship to the zirconium in solution. The luminescent characterization was analyzed by means of photoluminescence and thermoluminescence. The photoluminescence results showed a spectrum with three maxima which correspond to the electronic transitions 4 F 9/2 - 6 H 15/2 , 4 F 9/2 - 6 H 13/2 and 4 F 9/2 - 6 H 11/2 characteristics of the Dy 3+ ion. The thermoluminescence (Tl) response when being exposed to a monochrome UV beam in 240 nm showed a wide curve that exhibits a maxim centered in 200 grades C. The Tl response of ZrO 2 :Dy in function of the dose was shown lineal in the interval of 24 mJ/cm 2 to 432 mJ/cm 2 . A study of the repeatability and dissipation of the ZrO 2 :Dy Tl response is included. Considering the shown previous results we can conclude that the ZrO 2 in film form obtained by spray pyrolysis has luminescent properties in 240 nm. (Author)

Beryllium and zirconium

International Nuclear Information System (INIS)

Salesse, Marc

1959-01-01

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

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.

Laser-Based Additive Manufacturing of Zirconium

Directory of Open Access Journals (Sweden)

Himanshu Sahasrabudhe

2018-03-01

Full Text Available Additive manufacturing of zirconium is attempted using commercial Laser Engineered Net Shaping (LENSTM technique. A LENSTM-based approach towards processing coatings and bulk parts of zirconium, a reactive metal, aims to minimize the inconvenience of traditional metallurgical practices of handling and processing zirconium-based parts that are particularly suited to small volumes and one-of-a-kind parts. This is a single-step manufacturing approach for obtaining near net shape fabrication of components. In the current research, Zr metal powder was processed in the form of coating on Ti6Al4V alloy substrate. Scanning electron microscopy (SEM and energy dispersive spectroscopy (EDS as well as phase analysis via X-ray diffraction (XRD were studied on these coatings. In addition to coatings, bulk parts were also fabricated using LENS™ from Zr metal powders, and measured part accuracy.

Quantitative analysis of nickel in zirconium and zircaloy

International Nuclear Information System (INIS)

Rastoix, M.

1957-01-01

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

Effect of the substrate temperature on the microstructure and texture of Mg{sub 90}Zr{sub 10} (at.%) films deposited by sputtering

Energy Technology Data Exchange (ETDEWEB)

Garces, Gerardo [Department of Physical Metallurgy, CENIM, CSIC, Av. De Gregorio del Amo 8, 28040 Madrid (Spain)]. E-mail: ggarces@cenim.csic.es; Landais, Stephan [Office National dEtudes et de Recherches Aerospatiales, ONERA, BP72-29 Avenue de la Division Leclerc F-92322 Chatillon, Paris (France); Adeva, Paloma [Department of Physical Metallurgy, CENIM, CSIC, Av. De Gregorio del Amo 8, 28040 Madrid (Spain)

2006-11-30

The microstructure of Mg{sub 90}Zr{sub 10} (at.%) films obtained by sputtering onto copper substrate at three different temperatures (180, 320 and 350 deg. C) has been studied. Films exhibited an intense (0 0 0 1) basal plane fibre texture with the fibre axis parallel to the growth direction. Their microstructure consisted of columnar grains growing from the copper substrate to the free surface which is typical of the zone II of the Movchan and Demchishin zone model developed for PVD materials. Nevertheless, the microstructure of films was dependent on the substrate temperature. The grain diameter increased as the substrate temperature was increased. Moreover, the dislocation density inside the grains as well as that piled-up forming sub-grain boundaries decreased as the deposition temperature increased. Although the film growth in zone II is controlled by surface diffusion the larger surface mobility of the atoms as the substrate temperature increased led to changes in the solubility of zirconium. At low substrate temperatures all zirconium was in solid solution. However, at 350 deg. C the formation of small zirconium particles occurred at grain boundaries.

Immobilization of transition metal ions on zirconium phosphate monolayers

International Nuclear Information System (INIS)

Melezhik, A.V.; Brej, V.V.

1998-01-01

It is shown that ions of transition metals (copper, iron, vanadyl, titanium) are adsorbed on zirconium phosphate monolayers. The zirconium phosphate threshold capacity corresponds to substitution of all protons of hydroxyphosphate groups by equivalent amounts of copper, iron or vanadyl. Adsorption of polynuclear ions is possible in case of titanium. The layered substance with specific surface up to 300 m 2 /g, wherein ultradispersed titanium dioxide particles are intercalirated between zirconium-phosphate layers, is synthesized

Titanium zirconium and hafnium coordination compounds with vanillin thiosemicarbazone

International Nuclear Information System (INIS)

Konunova, Ts.B.; Kudritskaya, S.A.

1987-01-01

Coordination compounds of titanium zirconium and hafnium tetrachlorides with vanillin thiosemicarbazone of MCl 4 x nLig composition, where n=1.5, 4 for titanium and 1, 2, 4 for zirconium and hafnium, are synthesized. Molar conductivity of ethanol solutions is measured; IR spectroscopic and thermochemical investigation are carried out. The supposition about ligand coordination via sulfur and azomethine nitrogen atoms is made. In all cases hafnium forms stable compounds than zirconium

Modelling of Zirconium and Hafnium separation using continuous annular chromatography

International Nuclear Information System (INIS)

Moch-Setyadji; Endang Susiantini

2014-01-01

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

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

Directory of Open Access Journals (Sweden)

François M.

2010-06-01

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

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

International Nuclear Information System (INIS)

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

1975-09-01

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

In vitro assessment of artifacts induced by titanium, titanium-zirconium and zirconium dioxide implants in cone-beam computed tomography.

Science.gov (United States)

Sancho-Puchades, Manuel; Hämmerle, Christoph H F; Benic, Goran I

2015-10-01

The aim of this study was to test whether or not the intensity of artifacts around implants in cone-beam computed tomography (CBCT) differs between titanium, titanium-zirconium and zirconium dioxide implants. Twenty models of a human mandible, each containing one implant in the single-tooth gap position 45, were cast in dental stone. Five test models were produced for each of the following implant types: titanium 4.1 mm diameter (Ti4.1 ), titanium 3.3 mm diameter (Ti3.3 ), titanium-zirconium 3.3 mm diameter (TiZr3.3 ) and zirconium dioxide 3.5-4.5 mm diameter (ZrO3.5-4.5 ) implants. For control purposes, three models without implants were produced. Each model was scanned using a CBCT device. Gray values (GV) were recorded at eight circumferential positions around the implants at 0.5 mm, 1 mm and 2 mm from the implant surface (GVT est ). GV were assessed in the corresponding volumes of interest (VOI) in the control models without implants (GVC ontrol ). Differences of gray values (ΔGV) between GVT est and GVC ontrol were calculated as percentages. One-way ANOVA and post hoc tests were applied to detect differences between implant types. Mean ΔGV for ZrO3.5-4.5 presented the highest absolute values, generally followed by TiZr3.3 , Ti4.1 and Ti3.3 implants. The differences of ΔGV between ZrO3.5-4.5 and the remaining groups were statistically significant in the majority of the VOI (P ≤ 0.0167). ΔGV for TiZr3.3 , Ti4.1 and Ti3.3 implants did not differ significantly in the most VOI. For all implant types, ΔGV showed positive values buccally, mesio-buccally, lingually and disto-lingually, whereas negative values were detected mesially and distally. Zirconium dioxide implants generate significantly more artifacts as compared to titanium and titanium-zirconium implants. The intensity of artifacts around zirconium dioxide implants exhibited in average the threefold in comparison with titanium implants. © 2014 John Wiley & Sons A/S. Published by John Wiley

Spectrophotometric titration of sulfates in the presence of zirconium

International Nuclear Information System (INIS)

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

1978-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1957-07-01

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

Uranium (Vi) sorption onto zirconium diphosphate chemically modified

International Nuclear Information System (INIS)

Garcia G, N.; Ordonez R, E.

2010-10-01

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

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

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

Science.gov (United States)

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

2017-08-24

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

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

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

DISSOLUTION OF ZIRCONIUM AND ALLOYS THEREFOR

Science.gov (United States)

Swanson, J.L.

1961-07-11

The dissolution of zirconium cladding in a water solution of ammonium fluoride and ammonium nitrate is described. The method finds particular utility in processing spent fuel elements for nuclear reactors. The zirconium cladding is first dissolved in a water solution of ammonium fluoride and ammonium nitrate; insoluble uranium and plutonium fiuorides formed by attack of the solvent on the fuel materiai of the fuel element are then separated from the solution, and the fuel materiai is dissolved in another solution.

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.

Investigate of analysis for hydrogen contents in carbon films

International Nuclear Information System (INIS)

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

2001-01-01

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

Investigate of analysis for hydrogen contents in carbon films

Energy Technology Data Exchange (ETDEWEB)

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

2001-07-01

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

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

Science.gov (United States)

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

1962-08-14

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

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

Science.gov (United States)

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

2014-01-15

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

Electrochemical properties of the passive film on bulk Zr–Fe–Cr intermetallic fabricated by spark plasma sintering

Energy Technology Data Exchange (ETDEWEB)

Bai, Yakui [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Ling, Yunhan, E-mail: yhling@mail.tsinghua.edu.cn [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Lai, Wensheng [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Xing, Shupei; Ma, Wen [School of Materials Science and Engineering, Inner Mongolia University of Technology, Huhhot 010051 (China)

2016-12-01

Highlights: • SPS was employed to prepare Zr-based intermetallics which were commonly existed in zircaloy. • Zr-based intermetallics act as cathode when they embedded in zirconium matrix. • The passive films on surface of intermetallics behaved as n-type semiconductors. • Carrier concentration of Zr(Fe{sub 3}Cr){sub 2} was much lower than that of other intermetallics. - Abstract: Although Zr-based second phase particles (SPPs) are important factors influencing corrosion resistance of zircaloy cladding materials, the corrosion behavior of SPPs has not been investigated by means of electrochemical method so far. In order to clarify the role of SPPs commonly existed in zircaloy, bulk Zr-based intermetallics were firstly fabricated by spark plasma sintering (SPS) at temperatures 1373 K and an applied pressure of 60 MPa in this work. Both the natural passive film on surface and oxidation behavior of intermetallic has been investigated in this work. X-ray diffraction (XRD) pattern showed that as-prepared intermetallic of crystal structure belongs to Laves phase with AB{sub 2} type. Electrochemical measurement of passive film on surface of bulk Zr-based intermetallic exhibited significant difference with that of zirconium. Potentiodynamic measurements results revealed that intermetallic exhibited higher corrosion potential and lower corrosion current density than that of pure zirconium, implying that Zr-based second phase will act as cathode when they are included in zirconium matrix. Meanwhile, significant improvement of Zr–Fe–Cr intermetallic on the water chemistry corrosion resistance was demonstrated comparing with Zr–Fe and Zr–Cr binary intermetallics.

Capture of Tritium Released from Cladding in the Zirconium Recycle Process

Energy Technology Data Exchange (ETDEWEB)

Spencer, Barry B [ORNL; Bruffey, Stephanie H [ORNL; DelCul, Guillermo Daniel [ORNL; Walker, Trenton Baird [ORNL

2016-08-31

Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-based cladding and could be released from the cladding when the solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using nonradioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.

Capture of Tritium Released from Cladding in the Zirconium Recycle Process

Energy Technology Data Exchange (ETDEWEB)

Bruffey, Stephanie H [ORNL; Spencer, Barry B [ORNL; DelCul, Guillermo Daniel [ORNL

2016-08-31

This report is issued as the first revision to FCRD-MRWFD-2016-000297. Zirconium may be recovered from the Zircaloy® cladding of used nuclear fuel (UNF) for recycle or to reduce the quantities of high-level waste destined for a geologic repository. Recovery of zirconium using a chlorination process is currently under development at the Oak Ridge National Laboratory. The approach is to treat the cladding with chlorine gas to convert the zirconium in the alloy (~98 wt % of the alloy mass) to zirconium tetrachloride. A significant fraction of the tritium (0–96%) produced in nuclear fuel during irradiation may be found in zirconium-based cladding and could be released from the cladding when the solid matrix is destroyed by the chlorination reaction. To prevent uncontrolled release of radioactive tritium to other parts of the plant or to the environment, a method to recover the tritium may be required. The focus of this effort was to (1) identify potential methods for the recovery of tritium from the off-gas of the zirconium recycle process, (2) perform scoping tests on selected recovery methods using non-radioactive gas simulants, and (3) select a process design appropriate for testing on radioactive gas streams generated by the engineering-scale zirconium recycle demonstrations on radioactive used cladding.

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.)

Corrosion resistant zirconium alloys prepared by powder metallurgy

International Nuclear Information System (INIS)

Wojeik, C.C.

1984-01-01

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

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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.)

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

International Nuclear Information System (INIS)

Cox, B.

1997-01-01

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

Thermotransport of nitrogen and oxygen in β-zirconium

NARCIS (Netherlands)

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

1971-01-01

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

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

METHOD OF IMPROVING CORROSION RESISTANCE OF ZIRCONIUM

Science.gov (United States)

Shannon, D.W.

1961-03-28

An improved intermediate rinse for zirconium counteracts an anomalous deposit that often results in crevices and outof-the-way places when ordinary water is used to rinse away a strong fluoride etching solution designed to promote passivation of the metal. The intermediate rinse, which is used after the etching solution and before the water, is characterized by a complexing agent for fluoride ions such as aluminum or zirconium nitrates or chlorides.

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

International Nuclear Information System (INIS)

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

2010-01-01

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

Accelerated irradiation growth of zirconium alloys

International Nuclear Information System (INIS)

Griffiths, M.; Gilbert, R.W.; Fidleris, V.

1989-01-01

This paper discusses how sponge zirconium and Zr-2.5 wt% Nb, Zircaloy, or Excel alloys all exhibit accelerated irradiation growth compared with high-purity crystal-bar zirconium for irradiation temperatures between 550 to 710 K and fluences between 0.1 to 10 x 10 25 n · m -2 (E > 1 MeV). There is generally an incubation period or fluence before the onset of accelerated or breakaway growth, which is dependent on the particular material being irradiated, its metallurgical condition before irradiation, and the irradiation temperature. Transmission electron microscopy has shown that there is a correlation between accelerated irradiation growth and the appearance of c-component vacancy loops on basal planes. Measurements in some specimens indicate that a significant fraction of the strain can be directly attributed to the loops themselves. There is considerable evidence to show that their formation is dependent both on the specimen purity and on the irradiation temperature. Materials that have a high interstitial-solute content contain c-component loops and exhibit high growth rates even at low fluences ( 2 :5 n · m -2 , E > 1 MeV). For sponge zirconium and the Zircaloys, c-component loop formation and the associated acceleration of growth (breakaway) during irradiation occurs because the intrinsic interstitial solute (mainly, oxygen, carbon and nitrogen) in the zirconium matrix is supplemented by interstitial iron, chromium, and nickel from the radiation-induced dissolution of precipitates. (author)

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

Science.gov (United States)

2015-06-05

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

Separation of zirconium from hafnium by ion exchange

Energy Technology Data Exchange (ETDEWEB)

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

2013-07-01

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

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

Science.gov (United States)

2010-07-01

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

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

International Nuclear Information System (INIS)

Friedmann, Ch.; Schoenfeld, T.

1975-01-01

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

Microstructural modelling and lubrication study during zirconium alloy hot extrusion

International Nuclear Information System (INIS)

Gaudout, B.

2009-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2014-05-02

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

Photometric determination of zirconium in phosphorites by reaction with arsenazo III

Energy Technology Data Exchange (ETDEWEB)

Nikol' skaya, I V; Maksimov, A V

1976-05-01

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

A half-century of changes in zirconium alloys

International Nuclear Information System (INIS)

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

2008-01-01

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

Research and development of zirconium industry in China

International Nuclear Information System (INIS)

Liu Jianzhang; Tian Zhenye

2001-01-01

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

Roles of texture of Zr alloys in ZrO{sub 2} film formation and δ-hydride orientation near ZrO{sub 2}/Zr interface

Energy Technology Data Exchange (ETDEWEB)

Qin, W.; Szpunar, J.A., E-mail: weq565@mail.usask.ca, E-mail: jerzy.szpunar@usask.ca [Univ. of Saskatchewan, Dept. of Mechanical Engineering, Saskatoon, SK (Canada); Kozinski, J., E-mail: janusz.kozinski@lassonde.yorku.ca [York Univ., Faculty of Science and Engineering, Toronto, ON (Canada)

2014-07-01

Oxidation and hydrogen embrittlement are related to formation of cracks and failure of Zr alloys used in nuclear reactor applications. An in-depth understanding of the formation of ZrO{sub 2} film and the hydride precipitation and orientation is important for improving the corrosion resistance of zirconium alloys. In this work a theoretical model is developed to analyze the microstructure of ZrO{sub 2} film formed on Zr alloys and the effect of stress that results from ZrO{sub 2} formation on hydride reorientation in the region near oxide/metal interface. Our work shows that the macroscopic stress produced due to Pilling-Bedworth ratio for ZrO{sub 2}/Zr could lead to the hydride re-orientation in the region near ZrO{sub 2}/Zr interface. Whether or not this effect can occur is dependent on the texture of the zirconium alloys. Control of texture of zirconium alloys can affect the microstructure of ZrO{sub 2} film and can be responsible for change of hydride orientation. (author)

Preparation of complexes of zirconium and hafnium tetrachlorides with phosphorus oxychloride

International Nuclear Information System (INIS)

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

1989-01-01

This patent describes an improvement in a method for separating hafnium chloride from zirconium chloride using a distillation column, with a hafnium chloride enriched vapor stream taken from the top of the column and a zirconium enriched chloride stream taken from the bottom of the column. The improvement comprising: purifying the zirconium-hafnium chloride in a molten salt purification vessel prior to or after introduction into the distillation column to substantially eliminate iron chloride from the zirconium-hafnium chloride by at least periodically removing iron chloride from the molten salt purification vessel by electrochemically plating iron onto an electrode in the molten salt purification vessel. The molten salt in the molten salt purification vessel consisting essentially of a mixture of chlorides selected from the group consisting of alkali metals, alkaline earth metals, zirconium, hafnium, aluminum, manganese, and zinc

Zirconium distribution in the system HNO3-H2O-TBP-diluent

International Nuclear Information System (INIS)

Shu, J.; Araujo, B.F. de.

1984-01-01

The extraction behaviour of zirconium in TBP/diluent-HNO 3 -H 2 O systems is studied in order to increase the uranium decontamination factor by adjusting the extraction conditions so that zirconium extraction is kept at a minimum. Equilibrium diagram, TBP concentration, aqueous: organic phases ratio, salting-out effects and uranium loading in the organic phase were the main factors studied. All the experiments have been carried out with zirconium in the 10 -2 - 10 -3 M concentration range. The extractant degradation products influence upon zirconium behaviour was also verified. With the data obtained it was possible to introduce some modifications in the standard Purex flowsheet with the increase of the decontamination of uranium product from zirconium. (Author) [pt

Process effects on radio frequency diode reactively sputtered ZrO2 films

International Nuclear Information System (INIS)

Yang, M.M.; Reith, T.M.; Lin, C.J.

1990-01-01

The ZrO 2 thin film is deposited by means of a reactive radio frequency diode sputtering from an elemental zirconium target in an argon--oxygen mixture gas. The influence of the deposition process parameters on the microinstructure, composition, film stress, and refractive index is investigated. It is noted that the process parameters, in particular substrate bias, have a profound effect on the structure and properties. The possible mechanism, in terms of bombardment of energetic particles and adatom mobility on the film surface, is discussed

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)

Sorbents based on xerogels of zirconium, aluminum and manganese oxyhydroxides

Directory of Open Access Journals (Sweden)

R.V. Smotraiev

2016-05-01

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

Manufacturing process to reduce large grain growth in zirconium alloys

International Nuclear Information System (INIS)

Rosecrans, P.M.

1987-01-01

A method is described of treating cold worked zirconium alloys to reduce large grain growth during thermal treatment above its recrystallization temperature. The method comprises heating the zirconium alloy at a temperature of about 1300 0 F. to 1350 0 F. for about 1 to 3 hours subsequent to cold working the zirconium alloy and prior to the thermal treatment at a temperature of between 1450 0 -1550 0 F., the thermal treatment temperature being above the recrystallization temperature

TiCN thin films grown by reactive crossed beam pulsed laser deposition

Science.gov (United States)

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

2010-12-01

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

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

International Nuclear Information System (INIS)

Johnson, A.B. Jr.

1989-08-01

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

Evaluation of activities of carbons in chemical equilibrium with uranium carbonitride

International Nuclear Information System (INIS)

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

1992-01-01

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

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

International Nuclear Information System (INIS)

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

1992-01-01

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

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)

Corrosion resistance of ZrNxOy thin films obtained by rf reactive magnetron sputtering

International Nuclear Information System (INIS)

Ariza, E.; Rocha, L.A.; Vaz, F.; Cunha, L.; Ferreira, S.C.; Carvalho, P.; Rebouta, L.; Alves, E.; Goudeau, Ph.; Riviere, J.P.

2004-01-01

The main aim of this work is the investigation of the corrosion resistance of single layered zirconium oxynitride, ZrN x O y , thin films in artificial sweat solution at ambient temperature. The films were produced by rf reactive magnetron sputtering, using a pure Zr target at a constant temperature of 300 deg. C. Two different sets of samples were produced. In the first set of films, the substrate bias voltage was the main variable, whereas in the second set, the flow rate of reactive gases (oxygen/nitrogen ratio) was varied. The control of the amount of oxygen allowed the film properties to be tailored from those of covalent zirconium nitride to those of the correspondent ionic oxide. The corrosion behaviour was evaluated by potentiodynamic polarization and Electrochemical Impedance Spectroscopy (EIS) tests. The analysis of EIS data provided detailed information of the corrosion processes occurring at the surface of the system throughout the immersion time. The modifications of the coating microstructure and/or chemical composition induced by the variation of the deposition parameters were also evaluated and correlated with the corrosion mechanisms occurring in each system

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.

Low stress creep behaviour of zirconium

International Nuclear Information System (INIS)

Prasad, N.

1989-01-01

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

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

International Nuclear Information System (INIS)

Brun, R.

1989-01-01

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

Electrocnecical behaviour of zirconium during its anodic polarization in nitrate solutions

International Nuclear Information System (INIS)

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

1983-01-01

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

Spectrofluorimetric determination of hafnium and zirconium with 3,7-dihydroxyflavone

Energy Technology Data Exchange (ETDEWEB)

Ito, Takushi; Suzuki, Osamu; Seuzuki, Tetsuo; Murata, Akira

1986-04-01

The absorptive and fluorescent characteristics of the hafnium and zirconium complexes of 3-hydroxyflavone and its 12 hydroxy and methoxy derivatives have been studied. The fluorescence of the 1:1 hafnium - 3,7-dihydroxyflavone complex (lambdasub(ex.)397 nm,lambdasub(em.) 465 nm) in 3 M hydrochloric acid has been used to determine 2-40 ng ml/sup -1/ of hafnium. The fluorescence of the 1:1 zirconium - 3,7-dihydroxyflavone complex (lambdasub(ex.) 395 nm, lambda sub(em.) 465 nm) at pH 2.0 in 0.02 M sulphate solution has been used to determine 2-40 ng ml/sup -1/ of zirconium. These methods are very sensitive and can be used for the simultaneous determination of hafnium and zirconium with an error of about 5%.

Geologic structure of Gofitsky deposit of titanium and zirconium and perspectives of the reserve base of titanium and zirconium in Russia

Science.gov (United States)

Kukhmazov, Iskander

2016-04-01

With the fall of the Soviet Union, all the mining deposits of titanium and zirconium appeared outside of Russian Federation. Therefore the studying of deposits of titanium and zirconium in Russia is very important nowadays. There is a paradoxical situation in the country: in spite of possible existence of national mineral resource base of Ti-Zr material, which can cover needs of the country, Russia is the one of the largest buyers of imported Ti-Zr material in the world. Many deposits are not mined, and those which are in the process of mining have poor reserves. Demand for this raw material is very great not only for Russia, but also for the world in general. Today there is a scarcity of zircon around the world and it will only increase through time. Therefore prices of products of titanium and zirconium also increase. Consequently Russian deposits of titanium and zirconium with higher content than foreign may become competitive. Russia is forced to buy raw materials (zirconium and titanium production) from former Soviet Union countries at prices higher than the world's and thus incur huge losses, including customs charges. Russia should create its own mineral resource base of Ti-Zr. Studied titanium-zirconium deposits of Stavropol region may become the basis for the south part of Russia. At first, Beshpagirsky deposit should be pointed out. It has large reserves of ore sands with high content of Ti-Zr. A combination of favorable geographical position of the area with developed industrial infrastructure makes it very beneficial as an object for high priority development. Gofitsky deposit should be pointed out as well. Its sands have a wide areal distribution and a high content of titanium and zirconium. Chokrak, Karagan-Konksk and Sarmatian sediments of the Miocene of Gofitsky deposit are productive for titanium and zirconium placers within Stavropol region of Russia. Gofitsky deposit was evaluated from financial and economic point of view and the following data

Collaborative study of the colorimetric determination of zirconium in antiperspirant aerosols

International Nuclear Information System (INIS)

Beavin, P. Jr.

1977-01-01

A previously published method for determining zirconium in antiperspirant aerosols was collaboratively studied by 7 laboratories. The method consists of 2 procedures: a rapid dilution procedure for soluble zirconium compounds or a lengthier fusion procedure for total zirconium followed by colorimetric determination. The collaborators were asked to perform the following: Spiking materials representing 4 levels of soluble zirconium were added to weighed portions of a zirconium-free cream base concentrate and the portions were assayed by the dilution procedure. Spiking materials representing 4 levels of zirconium in either the soluble or the insoluble form (or as a mixture) were also added to portions of the same concentrate and these portions were assayed by the fusion procedure. They were also asked to concentrate and assay, by both procedures, 2 cans each of 2 commercial aerosol antiperspirants containing zirconyl hydroxychloride. The average percent recoveries and standard deviations for spiked samples were 99.8-100.2 and 1.69-2.71, respectively, for soluble compounds determined by the dilution procedure, and 93.8-97.4 and 3.09-4.78, respectively, for soluble and/or insoluble compounds determined by the fusion procedure. The average perent zirconium found by the dilution procedure in the 2 commercial aerosol products was 0.751 and 0.792. Insufficient collaborative results were received for the fusion procedure for statistical evaluation. The dilution procedure has been adopted as official first action

Hydrogen outbreak of Zirconium Molybdate Hihydrate

International Nuclear Information System (INIS)

Miura, Yasuhiko; Fukuda, Kazuhiro; Ochi, Eiji

2008-01-01

JNFL is planning to construct a facility for enclosing the hull and end pieces produced due to reprocessing of spent fuel into stainless canisters after compressing, while those hull and end pieces enclosed into the stainless canisters are called 'compressed hulls'. Since the compressed hulls contain moisture absorbent Zirconium Molybdate Hihydrate accompanying hull and end pieces, there is a risk of outbreak of radiolysisradiolysis gas such as hydrogen, etc. by radiolysisradiolysis. This report intends to state the result of radiation irradiation experiment with the purpose of examining the volume of hydrogen outbreak from Zirconium Molybdate Hihydrate of the compressed hulls. (author)

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

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

Energy Technology Data Exchange (ETDEWEB)

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

2013-08-15

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

A review of the inorganic and organometallic chemistry of zirconium

International Nuclear Information System (INIS)

Kalvins, A.K.

1985-01-01

The results of a literature review of the inorganic and organometallic chemistry of zirconium are presented. Compounds with physical and chemical properties compatible with the requirements of an ir laser zirconium isotope separation process have been identified

Mechanical resistance of zirconium implant abutments: A review of the literature

Science.gov (United States)

Vaquero-Aguilar, Cristina; Torres-Lagares, Daniel; Jiménez-Melendo, Manuel; Gutiérrez-Pérez, José L.

2012-01-01

The increase of aesthetic demands, together with the successful outcome of current implants, has renewed interest in the search for new materials with enough mechanical properties and better aesthetic qualities than the materials customarily used in implanto-prosthetic rehabilitation. Among these materials, zirconium has been used in different types of implants, including prosthetic abutments. The aim of the present review is to analyse current scientific evidence supporting the use of this material for the above mentioned purposes. We carried out the review of the literature published in the last ten years (2000 through 2010) of in vitro trials of dynamic and static loading of zirconium abutments found in the databases of Medline and Cochrane using the key words zirconium abutment, fracture resistance, fracture strength, cyclic loading. Although we have found a wide variability of values among the different studies, abutments show favourable clinical behaviour for the rehabilitation of single implants in the anterior area. Such variability may be explained by the difficulty to simulate daily mastication under in vitro conditions. The clinical evidence, as found in our study, does not recommend the use of implanto-prosthetic zirconium abutments in the molar area. Key words: Zirconium abutment, zirconium implant abutment, zirconia abutment, fracture resistance, fracture strength, cyclic loading. PMID:22143702

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

Energy Technology Data Exchange (ETDEWEB)

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

2012-08-15

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

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

Science.gov (United States)

2010-07-01

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

Laves intermetallics in stainless steel-zirconium alloys

International Nuclear Information System (INIS)

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

1997-01-01

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

Interrelationship between structure and corrosion behaviour of zirconium

Energy Technology Data Exchange (ETDEWEB)

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

1979-05-01

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1997-02-01

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

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

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

Surface Modification of Solution-Processed ZrO2 Films through Double Coating for Pentacene Thin-Film Transistors

Science.gov (United States)

Kwon, Jin-Hyuk; Bae, Jin-Hyuk; Lee, Hyeonju; Park, Jaehoon

2018-03-01

We report the modification of surface properties of solution-processed zirconium oxide (ZrO2) dielectric films achieved by using double-coating process. It is proven that the surface properties of the ZrO2 film are modified through the double-coating process; the surface roughness decreases and the surface energy increases. The present surface modification of the ZrO2 film contributes to an increase in grain size of the pentacene film, thereby increasing the field-effect mobility and decreasing the threshold voltage of the pentacene thin-film transistors (TFTs) having the ZrO2 gate dielectric. Herein, the molecular orientation of pentacene film is also studied based on the results of contact angle and X-ray diffraction measurements. Pentacene molecules on the double-coated ZrO2 film are found to be more tilted than those on the single-coated ZrO2 film, which is attributed to the surface modification of the ZrO2 film. However, no significant differences are observed in insulating properties between the single-and the double-coated ZrO2 dielectric films. Consequently, the characteristic improvements of the pentacene TFTs with the double-coated ZrO2 gate dielectric film can be understood through the increase in pentacene grain size and the reduction in grain boundary density.

Identification and characterization of a new Zirconium hydride

International Nuclear Information System (INIS)

Zhao, Z.

2007-01-01

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

Sorption of cesium on titanium and zirconium phosphates

International Nuclear Information System (INIS)

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

2003-01-01

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

[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.

Orbital hybridization, crystal structure and anomalous resistivity of ultrathin CrZrx alloy films on polymeric substrates

International Nuclear Information System (INIS)

Evans, Drew; Zuber, Kamil; Merkens, Kerstin; Murphy, Peter

2012-01-01

The orbital hybridization and crystal structure are experimentally explored for ultrathin chrome zirconium (CrZr x ) alloy films co-sputtered on precoated polymeric substrates. We determine the level of orbital hybridization and crystal structure using X-ray photoelectron spectroscopy and electron diffraction. Body-centred cubic and Ω-hexagonally close-packed phases are observed to coexist in the sputtered Cr-based films. Experiments reveal the orbital hybridization and crystal structure combine to produce anomalous resistivity for these ultrathin films.

Peculiarities of formation of zirconium aluminides in hydride cycle mode

International Nuclear Information System (INIS)

Muradyan, G.N.

2016-01-01

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

Distribution of zirconium in the nitric acid-water-TPB-diluent system

International Nuclear Information System (INIS)

Shu, J.; Floh de Araujo, B.

1984-10-01

This paper deals with the extraction behaviour of zirconium in TBP/diluent-HNO 3 -H 2 O systems. The main purpose is to increase the uranium decontamination factor by adjusting the extraction conditions so that zirconium extraction is kept at a mininum. Equilibrium diagram, TBP concentration, aqueous: organic phases ratio, salting-out effects and uranium loading in the organic phase were the main factors studied. All the experiments have been carried out with zirconium in the 10 -2 - 10 -3 M concentration range. The extractant degradation products influence upon ziconium behaviour was also verified. With the data obtained it was possible to introduce some modification in the standard Purex flow-sheet with the increase of the decontamination of uranium from zirconium. 5 refs., 9 figs

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.

Separation process of zirconium and hafnium

International Nuclear Information System (INIS)

Hure, J.; Saint-James, R.

1955-01-01

About the separation different processes of zirconium-hafnium, the extraction by solvent in cross-current is the most easily the process usable on an industrial scale. It uses tributyl phosphate as solvent, diluted with white spirit to facilitate the decanting. Some exploratory tests showed that nitric environment seemed the most favorable for extraction; but a lot of other factors intervene in the separation process. We studied the influence of the acidity successively, the NO 3 - ions concentration, the role of the cation coming with NO 3 - , as well as the influence of the concentration of zirconium in the solution on the separation coefficient β = α Zr / α Hf . (M.B.) [fr

Zirconium diselenite microstructures, formation and mechanism

Science.gov (United States)

Naik, Chandan C.; Salker, A. V.

2018-04-01

In this work, a series of microstructures of zirconium diselenite (Zr(SeO3)2) has been prepared via a simple precipitation method at room temperature without adding any organic surfactants. Phase purity of the sample has been checked by X-ray Diffraction. From the SEM, FESEM, and TEM images spheroid nanoparticles to the starfish-like structure of zirconium diselenite are detected. The morphological evolution processes were investigated carefully following time-dependent experiments and a growth mechanism has been proposed. Two different crystal growth processes, the oriented attachment process accompanying the Ostwald ripening process were held responsible for the formation of a structure resembling starfish having four arms.

Aqueous metal–organic solutions for YSZ thin film inkjet deposition

DEFF Research Database (Denmark)

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

2017-01-01

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

A computer model for hydride blister growth in zirconium alloys

International Nuclear Information System (INIS)

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

1985-06-01

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

SURFACE FILMS TO SUPPRESS FIELD EMISSION IN HIGH-POWER MICROWAVE COMPONENTS

Energy Technology Data Exchange (ETDEWEB)

Hirshfield, Jay l

2014-02-07

Results are reported on attempts to reduce the RF breakdown probability on copper accelerator structures by applying thin surface films that could suppress field emission of electrons. Techniques for application and testing of copper samples with films of metals with work functions higher than copper are described, principally for application of platinum films, since platinum has the second highest work function of any metal. Techniques for application of insulating films are also described, since these can suppress field emission and damage on account of dielectric shielding of fields at the copper surface, and on account of the greater hardness of insulating films, as compared with copper. In particular, application of zirconium oxide films on high-field portions of a 11.424 GHz SLAC cavity structure for breakdown tests are described.

Investigation of the evaporation process conditions on the optical constants of zirconia films

International Nuclear Information System (INIS)

Dobrowolski, J.A.; Grant, P.D.; Simpson, R.; Waldorf, A.

1989-01-01

Deposition parameters required for producing zirconia films for use in optical multilayer systems by electron-beam gun evaporation of zirconia and zirconium starting materials were investigated. The optical constants were determined as a function of distance, partial pressure of oxygen, and angle of incidence. The direct and reactive evaporation processes yielded ZrO 2 films with refractive indices of 2.08 and 2.14, respectively, for vapor incident on the substrate at normal incidence

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

Hydrogen content in titanium and a titanium–zirconium alloy after acid etching

Energy Technology Data Exchange (ETDEWEB)

Frank, Matthias J.; Walter, Martin S. [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway); Institute of Medical and Polymer Engineering, Chair of Medical Engineering, Technische Universität München, Boltzmannstrasse 15, 85748 Garching (Germany); Lyngstadaas, S. Petter [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway); Wintermantel, Erich [Institute of Medical and Polymer Engineering, Chair of Medical Engineering, Technische Universität München, Boltzmannstrasse 15, 85748 Garching (Germany); Haugen, Håvard J., E-mail: h.j.haugen@odont.uio.no [Department of Biomaterials, Institute for Clinical Dentistry, University of Oslo, P.O. Box 1109, Blindern, NO-0317 Oslo (Norway)

2013-04-01

Dental implant alloys made from titanium and zirconium are known for their high mechanical strength, fracture toughness and corrosion resistance in comparison with commercially pure titanium. The aim of the study was to investigate possible differences in the surface chemistry and/or surface topography of titanium and titanium–zirconium surfaces after sand blasting and acid etching. The two surfaces were compared by X-ray photoelectron spectroscopy, secondary ion mass spectroscopy, scanning electron microscopy and profilometry. The 1.9 times greater surface hydrogen concentration of titanium zirconium compared to titanium was found to be the major difference between the two materials. Zirconium appeared to enhance hydride formation on titanium alloys when etched in acid. Surface topography revealed significant differences on the micro and nanoscale. Surface roughness was increased significantly (p < 0.01) on the titanium–zirconium alloy. High-resolution images showed nanostructures only present on titanium zirconium. - Highlights: ► TiZr alloy showed increased hydrogen levels over Ti. ► The alloying element Zr appeared to catalyze hydrogen absorption in Ti. ► Surface roughness was significantly increased for the TiZr alloy over Ti. ► TiZr alloy revealed nanostructures not observed for Ti.

Carbonitriding of low alloy steels: Mechanical and metallurgical responses

Energy Technology Data Exchange (ETDEWEB)

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

2017-05-02

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

Zirconium-made equipment for the new La Hague reprocessing plants

International Nuclear Information System (INIS)

Decours, J.; Demay, R.; Bernard, C.; Mouroux, J.P.; Simonnet, J.

1991-01-01

The use of zirconium was developed to solve some problems of severe corrosion in boiling nitric medium, and to guarantee the service life of the equipment concerned. The paper presents the experience gained since the early 1970s, when the first units made of zirconium were used in French reprocessing plants. For the new La Hague UP3 and UP2 800 plants, it was decided to extend the use of zirconium to make large-scale equipment and, to do so, a major R and D program was implemented, of which the main results are presented

In-situ stabilization of radioactive zirconium swarf

Science.gov (United States)

Hess, Clay C.

1999-01-01

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

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

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

Energy Technology Data Exchange (ETDEWEB)

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

1963-05-01

Zirconium phosphate has been studied with a view to using it as an ion exchanger: the first objective was to develop a method of preparation easy to apply and also reproducible. To this end, several tests were carried out varying the molar ratios of phosphorus and of zirconium. Some physical properties such as the diffraction of X-rays were examined. The work then involved certain chemical properties, particularly the percentages of free water and structural water given by the loss on calcination, the Karl-Fisher method and the weight losses by thermogravimetry. Finally an attempts was made to apply the exchanger to the separation of alkaline ions. The static tests showed that the order of fixation of these ions was Cs{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Tests with columns showed that Na{sup +} and K{sup +} were easily separable, as was the Rb{sup +}-Cs{sup +} mixture, this last pair being fairly difficult to dissociate. (author) [French] Le phosphate de zirconium a ete etudie en vue de son utilisation comme echangeur d'ions: le premier but a atteindre a ete de mettre au point une preparation pouvant se reveler facilement utilisable ainsi qu'aisement reproductible. A cet effet, plusieurs essais ont ete effectues en faisant varier les rapports molaires du phosphore et du zirconium. Quelques proprietes physiques, telle la diffraction des rayons X, ont ete abordees. Ensuite, l'etude a porte sur certaines proprietes chimiques, particulierement les pourcentages d'eau libre et d'eau de structure par des pertes au feu, utilisation de la methode de Karl-Fisher, ainsi que des pertes de poids a la thenmobalance. Enfin, on a tente d'utiliser l'echangeur a la separation des ions alcalins. Les etudes statiques ont permis de constater que l'ordre de fixation de ces ions etait Cs{sup +} > Rb{sup +} >> K{sup +} > Na{sup +}. Les essais effectues en colonne ont montre que Na{sup +} et K{sup +} etaient aisement separables entre eux, ainsi que du couple Rb{sup +}-Cs{sup +}, ce

Towards in-situ tem analysis of PLD Pb(Zr,Ti)O3 thin film membranes

NARCIS (Netherlands)

Sardan Sukas, Ö.; Berenschot, Johan W.; de Boer, Meint J.; Nguyen, Duc Minh; van Zalk, M.; Abelmann, Leon

2011-01-01

In this paper, a novel technique for fabricating Transmission Electron Microscopy (TEM) chips for investigating structural and piezoelectric properties of Pulse Laser Deposited (PLD) Lead Zirconium Titanate (PZT) thin films is presented. The method involves silicon-on-insulator (SOI) wafer

Concept Feasibility Report for Electroplating Zirconium onto Uranium Foil - Year 2

Energy Technology Data Exchange (ETDEWEB)

Coffey, Greg W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Meinhardt, Kerry D. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Joshi, Vineet V. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Pederson, Larry R. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lavender, Curt A. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Burkes, Douglas [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

2015-03-01

The Fuel Fabrication Capability within the U.S. High Performance Research Reactor Conversion Program is funded through the National Nuclear Security Administration (NNSA) NA-26 (Office of Material Management and Minimization). An investigation was commissioned to determine the feasibility of using electroplating techniques to apply a coating of zirconium onto depleted uranium/molybdenum alloy (U-10Mo). Electroplating would provide an alternative method to the existing process of hot roll-bonding zirconium foil onto the U-10Mo fuel foil during the fabrication of fuel elements for high-performance research reactors. The objective of this research was to develop a reproducible and scalable plating process that will produce a uniform, 25 μm thick zirconium metal coating on U-10Mo foil. In previous work, Pacific Northwest National Laboratory (PNNL) established a molten salt electroplating apparatus and protocol to plate zirconium metal onto molybdenum foil (Coffey 2015). During this second year of the research, PNNL furthered this work by moving to the U-10Mo alloy system (90 percent uranium:10 percent molybdenum). The original plating apparatus was disassembled and re-assembled in a laboratory capable of handling low-level radioactive materials. Initially, the work followed the previous year’s approach, and the salt bath composition was targeted at the eutectic composition (LiF:NaF:ZrF4 = 26:37:37 mol%). Early results indicated that the formation of uranium fluoride compounds would be problematic. Other salt bath compositions were investigated in order to eliminate the uranium fluoride production (LiF:NaF = 61:39 mol% and LiF:NaF:KF = 46.5:11.5:42 mol% ). Zirconium metal was used as the crucible for the molten salt. Three plating methods were used—isopotential, galvano static, and pulsed plating. The molten salt method for zirconium metal application provided high-quality plating on molybdenum in PNNL’s previous work. A key advantage of this approach is that

Zirconium elasticity modules

International Nuclear Information System (INIS)

Vavra, G.

1978-01-01

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

Highly corrosion resistant zirconium based alloy for reactor structural material

International Nuclear Information System (INIS)

Ito, Yoichi.

1996-01-01

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

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

International Nuclear Information System (INIS)

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

1985-01-01

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

History of the development of zirconium alloys for use in nuclear reactors

International Nuclear Information System (INIS)

Rickover, H.G.; Geiger, L.D.; Lustman, B.

1975-01-01

The technical problems and the major decisions made during the early development of zirconium alloys for use in naval reactors are outlined. A summary is given of the development of commercial sources of supply for zirconium and hafnium metal over the period 1950 to 1965, and the problems encountered in obtaining zirconium needed for early naval prototype and shipboard reactors are identified. Steps taken in the Government procurement process are described and statistics on production amounts, prices, and inventory are included. Also included are the technical aspects associated with the development of zirconium for water-cooled nuclear reactors, beginning in early 1949 when the Bettis Atomic Power Laboratory was established as a part of the Naval Reactors Program. While in the course of the next 25 years, small-scale investigations were performed on other potential core structural materials such as stainless steel, niobium, aluminum, and beryllium, the pressure for continual development, improvement, and application of zirconium was predominant and unrelenting. (U.S.)

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

Temperature dependence of the optical properties of ion-beam sputtered ZrN films

Energy Technology Data Exchange (ETDEWEB)

Larijani, M.M. [NSTRI, AEOI, Radiation Applications Research School, Karaj (Iran, Islamic Republic of); Kiani, M. [Azad University, South Tehran Branch, Department of Physics, Tehran (Iran, Islamic Republic of); Jafari-Khamse, E. [NSTRI, AEOI, Radiation Applications Research School, Karaj (Iran, Islamic Republic of); University of Kashan, Department of Physics, Kashan (Iran, Islamic Republic of); Fathollahi, V. [Nuclear Science Research School, NSTRI, Tehran (Iran, Islamic Republic of)

2014-11-15

The reflectivity of sputtered Zirconium nitride films on glass substrate has been investigated in the spectral energy range of 0.8-6.1 eV as a function of deposition temperature varying between 373 and 723 K. Optical constants of the prepared films have been determined using the Drude analysis. Experimental results showed strong dependency of optical properties of the films, such as optical resistivity on the substrate temperature. The temperature increase of the substrate has shown an increase in both the plasmon frequency and electron scattering time. The electrical behavior of the films showed a good agreement between their optical and electrical resistivity. (orig.)

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

Development of zirconium alloy tube manufacturing technology

International Nuclear Information System (INIS)

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

2009-01-01

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

Lithium aluminate/zirconium material useful in the production of tritium

Science.gov (United States)

Cawley, W.E.; Trapp, T.J.

A composition is described useful in the production of tritium in a nuclear reactor. Lithium aluminate particles are dispersed in a matrix of zirconium. Tritium produced by the reactor of neutrons with the lithium are absorbed by the zirconium, thereby decreasing gas pressure within capsules carrying the material.

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

Science.gov (United States)

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

2018-05-01

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

Effects of bias voltage and annealing on the structure and mechanical properties of WC0.75N0.25 thin films

International Nuclear Information System (INIS)

Su, Y.D.; Hu, C.Q.; Wen, M.; Wang, C.; Liu, D.S.; Zheng, W.T.

2009-01-01

We investigated the effects of both bias voltage and annealing on the structure and mechanical properties of WC 0.75 N 0.25 thin films, deposited on Si (1 0 0) substrates by a direct current reactive magnetron sputtering system, in which the negative substrate bias voltage (V b ) was varied from floating (-1.6 V) to -200 V, and the deposited films were annealed at 800 deg. C for 2 h. The X-ray photoelectron spectroscopy and selected area electron diffraction analyses, along with the density-functional theory (DFT) calculations on the electronic structure, showed that WC 0.75 N 0.25 films were a single-phase of carbonitrides. After annealing, a significant decrease in hardness for the films was observed, being a result of point-defect annihilation as V b was in the range of floating to -120 V. However, when V b was in the range of -160 to -200 V, the hardness increased from ∼37 GPa for the as-deposited film to a maximum of ∼43 GPa for the annealed one. This increase in hardness after annealing might be attributed to age-hardening.

Thermodynamic Database for Zirconium Alloys

International Nuclear Information System (INIS)

Jerlerud Perez, Rosa

2003-05-01

For many decades zirconium alloys have been commonly used in the nuclear power industry as fuel cladding material. Besides their good corrosion resistance and acceptable mechanical properties the main reason of using these alloys is the low neutron absorption. Zirconium alloys are exposed to a very severe environment during the nuclear fission process and there is a demand for better design of this material. To meet this requirement a thermodynamic database is developed to support material designers. In this thesis some aspects about the development of a thermodynamic database for zirconium alloys are presented. A thermodynamic database represents an important facility in applying thermodynamic equilibrium calculations for a given material providing: 1) relevant information about the thermodynamic properties of the alloys e.g. enthalpies, activities, heat capacity, and 2) significant information for the manufacturing process e.g. heat treatment temperature. The basic information in the database is first the unary data, i.e. pure elements; those are taken from the compilation of the Scientific Group Thermodata Europe (SGTE) and then the binary and ternary systems. All phases present in those binary and ternary systems are described by means of the Gibbs energy dependence on composition and temperature. Many of those binary systems have been taken from published or unpublished works and others have been assessed in the present work. All the calculations have been made using Thermo C alc software and the representation of the Gibbs energy obtained by applying Calphad technique

low dose irradiation growth in zirconium

International Nuclear Information System (INIS)

Fortis, A.M.

1987-01-01

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

Study of zirconium-addition binary systems

International Nuclear Information System (INIS)

Wozniakova, B.; Kuchar, L.

1975-01-01

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

Bioremediation of zirconium from aqueous solution by coriolus versicolor: process optimization

International Nuclear Information System (INIS)

Amin, M.; Bhatti, H. N.; Sadaf, S.

2013-01-01

In the present study the potential of live mycelia of Coriolus versicolor was explored for the removal of zirconium from simulated aqueous solution. Optimum experimental parameters for the bioremediation of zirconium using C. versicolor biomass have been investigated by studying the effect of mycelia dose, concentration of zirconium, contact time and temperature. The isothermal studies indicated that the ongoing bioremediation process was exothermic in nature and obeyed Langmuir adsorption isotherm model. The Gibbs free energy (ΔG), entropy (ΔS) and enthalpy (ΔH) of bioremediation were also determined. The result showed that bioremediation of zirconium by live C. versicolor was feasible and spontaneous at room temperature. The equilibrium data verified the involvement of chemisorption during the bioremediation. The kinetic data indicated the operation of pseudo-second order process during the biosorption of zirconium from aqueous solution. Maximum bioremediation capacity (110.75 mg/g) of C. versicolor was observed under optimum operational conditions: pH 4.5, biomass dose 0.05 mg/100 mL, contact time 6 h and temperature 30 degree C. The results showed that C. versicolor could be used for bioremediation of heavy metal ions from aqueous systems. (author)

Evaluation of a Zirconium Recycle Scrubber System

Energy Technology Data Exchange (ETDEWEB)

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

2017-04-01

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

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

International Nuclear Information System (INIS)

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

1999-01-01

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

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.

Synthesis, characterization and optical properties of novel N donor ligands-chelated zirconium(IV) complexes

Science.gov (United States)

Shahroosvand, Hashem; Nasouti, Fahimeh; Mohajerani, Ezeddin; Khabbazi, Amir

2012-11-01

Novel zirconium complexes have been synthesized by using a mixture of zirconium nitrate, 1,2,4,5-benzen tetracarboxylic acid (H4btec), 1,10-phenanthroline(phen) and potassium thiocyanate. Monodentate coordination mode of btec acid for all complexes was investigated by FT-IR spectroscopy. The complexes were also characterized by UV-Vis, 1H NMR, CHN, ICP-AES. The reaction details and features were described and discussed. The photoluminescence emission of seven zirconium complexes was shown two series peaks: first, sharp and intense bands from 300 to 500 nm and broadened with less intensity from 650 to 750 nm for the second bands. Each of the zirconium compounds were doped in PVK:PBD blend as host. The ratio of zirconium complexes for each type were modified 8 wt.% in PVK:PBD(100:40). The electroluminescence spectra of zirconium complexes were indicated a red shift rather than PVK:PBD blend. We suggest that the electroplex occurring at PVK-Zr complex interface.

Data on physicochemical properties of active films derived from plantain flour/PCL blends developed under reactive extrusion conditions

Directory of Open Access Journals (Sweden)

Tomy J. Gutiérrez

2017-12-01

Full Text Available The data given below relates to the research paper entitled: “Eco-friendly films prepared from plantain flour/PCL blends under reactive extrusion conditions using zirconium octanoate as a catalyst”, recently published by our research group [1]. This article provides information concerning the physicochemical properties of the above-mentioned film systems: thickness, density, opacity, moisture content and surface moisture. Keywords: Active films, Antimicrobial properties, Cross-linking, Poly(ε-caprolactone, Starchy

An evaluated neutronic data file for elemental zirconium

International Nuclear Information System (INIS)

Smith, A.B.; Chiba, S.

1994-09-01

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

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

Indian Academy of Sciences (India)

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

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

International Nuclear Information System (INIS)

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

1994-01-01

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

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

Development of tantalum–zirconium alloy for hydrogen purification

Energy Technology Data Exchange (ETDEWEB)

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

2016-11-01

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

Zirconium determination in refractories (gravimetric method)

International Nuclear Information System (INIS)

Capiotto, N.; Narahashi, Y.; Perish, P.G.; Souza, J.R. de

1991-01-01

A gravimetric method for zirconium determination in refractories is described. X-ray fluorescence analysis is also employed in this experiment and considerations about interfering elements are presented. (M.V.M.)

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

Fluorimetric determination of uranium in zirconium and zircaloy alloys

International Nuclear Information System (INIS)

Acosta L, E.

1991-05-01

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

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

Preparation of zirconium molybdate gel generator

International Nuclear Information System (INIS)

Charoen, S.; Aungurarat, G.; Laohawilai, S.; Sukontpradit, W.; Jingjit, S.

1994-01-01

A procedure for preparation of 99mTc generator based on conversion to zirconium molybdate gel of 99Mo produced by neutron activation was reported. The gel was prepared from zirconium oxychloride solution pH 1.6, ammonium molybdate solution pH 3-5 and mole ratio of Zr:Mo 1:1 which had water content about 7-8%. Small generators containing 1-1.5 g of gel were eluted with average efficiencies of 77% and the activity peak in the first 3 ml of 10 ml of saline solution. The amount of Mo and Zr in eluates were below the acceptance limit. The gel generators of activity about 100 mCi were prepared and had the good performance in elutability and stability

Sorption of Europium in zirconium silicate

International Nuclear Information System (INIS)

Garcia R, G.

2004-01-01

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

Radiochemical determination of zirconium by inductively coupled plasma mass spectrometry (ICPMS)

International Nuclear Information System (INIS)

Oliveira, Thiago C.; Oliveira, Arno Heeren de

2013-01-01

The zirconium isotope 93 Zr is a long-lived pure β-particle-emitting radionuclide thus occurring as one of the radionuclides found in nuclear reactors. It's produced from 235 U fission and from 92 Zr neutron activation. Due to its long half-life, 93 Zr is one of the interest radionuclides for assessment studies performance of waste storage or disposal. Measurement of 93 Zr is difficult owing to its trace level concentration and its low activity in nuclear wastes and further because its certified standards are not frequently available. The aim of this work was to apply a selective radiochemical separation methodology for 93 Zr determination in nuclear waste and analyze it by Inductively Coupled Plasma Mass Spectrometry (ICPMS). To set up the zirconium radiochemical separation procedure, a zirconium tracer solution was used in order to follow the zirconium behavior during the radiochemical separation. A tracer solution containing the main interferences, Ba, Co, Eu, Fe, Mn, Nb, Ni, Sr, and Y was used in order to verify the decontamination factor during separation process. The limit of detection of 0,039 ppb was obtained for zirconium standard solutions by ICPMS. Then, the protocol will be applied to low level waste (LLW) and intermediate level waste (ILW) from nuclear power plants. (author)

Ab initio atomic simulation of hydrogen and iodine effects in zirconium

International Nuclear Information System (INIS)

Domain, Ch.

2002-03-01

In this work we present ab initio atomic simulations concerning the effects of hydrogen and iodine in hexagonal zirconium. We first studied the point defects in the dilute Zr-H (and to a less extend Zr-H-O) systems and concluded that it is better described within the generalised gradient approximation for the exchange and correlation functional. We calculated the hydrogen thermal diffusion coefficient in solid solution that agree very well with the experimental values. The calculated formation energy of different self-interstitial configuration are rather small (around 3 eV) and close to each other indicating the high complexity of these defects. We studied the core structure of the screw dislocation that has a preferential prismatic spreading. We also calculated the gamma surface for different gliding planes. The influence of hydrogen, that induces a significant reduction of the gamma surfaces excess energies, allows to qualitatively explain experimental results regarding some hydrogen effects on hexagonal zirconium plastic deformation. We also discussed the effect of zirconium hydride stoichiometry on gamma surfaces. The results concerning the iodine and oxygen adsorption on zirconium surfaces, inducing the evaluation of the effective surface energy reduction as a function of the iodine partial pressure allow for a better description of iodine induced stress corrosion cracking of zirconium. (author)

Control and monitoring of the localized corrosion of zirconium in acidic chloride solutions

International Nuclear Information System (INIS)

Fahey, J.; Holmes, D.; Yau, T.L.

1995-01-01

Zirconium in acidic chloride solutions which are contaminated with ferric or cupric cations is prone to localized corrosion. This tendency can be reduced by ensuring that the zirconium surface is clean and smooth. In this paper, the effect of surface condition on the localized corrosion of zirconium in acidic chloride solutions is predicted with potentiodynamic scans. These predictions are confirmed by weight loss tests on various combinations of surface finish and acid concentrations. A real time indication of localized corrosion is seen by monitoring the electrochemical noise produced between two similar electrodes immersed in an acidic chloride solutions. Electrochemical noise monitoring correlates well with the predictions from potentiodynamic and weight loss experiments. The electrochemical noise results show that while an elevated (more anodic) potential caused by ferric ion contamination may be a necessary condition for localized corrosion, it is not a sufficient condition: A smooth, clean zirconium surface reduces the localized corrosion of zirconium

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

The role of target-to-substrate distance on the DC magnetron sputtered zirconia thin films' bioactivity

Energy Technology Data Exchange (ETDEWEB)

Thaveedeetrakul, Arisara [Department of Chemical Engineering, King Mongkut' s University of Technology Thonburi, Bangkok (Thailand); Witit-anun, Nirun [Department of Physics, Burapha University, Chon Buri (Thailand); Thailand Center of Excellence in Physics, CHE, Ministry of Education, Bangkok (Thailand); Boonamnuayvitaya, Virote, E-mail: virote.boo@kmutt.ac.th [Department of Chemical Engineering, King Mongkut' s University of Technology Thonburi, Bangkok (Thailand)

2012-01-15

Zirconium dioxide thin films were deposited on 316L-stainless steel type substrates using DC unbalanced magnetron sputtering. The process parameter of this work was the target-to-substrate distance (d{sub t-s}), which was varied from 60 to 120 mm. The crystal structure and surface topography of zirconium dioxide thin films were characterized by X-ray diffraction (XRD) and atomic force microscopy (AFM). The results demonstrate that all of the ZrO{sub 2} thin films are composed monoclinic phase. The film sputtered at short d{sub t-s} (60 mm) shows a rather heterogeneous, uneven surface. The grain size, roughness, and thickness of thin films were decreased by increasing d{sub t-s}. The bioactivity was assessed by investigating the formation of hydroxyapatite (Ca{sub 10}(PO{sub 4}){sub 6}(OH){sub 2}) on the thin film surface soaked in simulated body fluids (SBF) for 7 days. XRD and scanning electron microscopy (SEM) were used to verify the formation of apatite layers on the samples. Bone-like apatites were formed on the surface of the ZrO{sub 2} thin film in SBF immersion experiments. A nanocrystalline hydroxyapatite (HA) with a particle size of 2-4 {mu}m was deposited. Higher crystallinity of HA on the surface was observed when the distance d{sub t-s} increased to more than 80 mm. Therefore, it seems that a d{sub t-s} greater than 80 mm is an important sputtering condition for inducing HA on the zirconia film.

Electrochemical formation of uranium-zirconium alloy in LiCl-KCl melts

Energy Technology Data Exchange (ETDEWEB)

Murakami, Tsuyoshi, E-mail: m-tsuyo@criepi.denken.or.j [Central Research Institute of Electric Power Industry (CRIEPI), Komae-shi, Tokyo 201-8511 (Japan); Kato, Tetsuya; Kurata, Masaki [Central Research Institute of Electric Power Industry (CRIEPI), Komae-shi, Tokyo 201-8511 (Japan); Yamana, Hajimu [Research Reactor Institute, Kyoto University, Kumatori-cho, Sennan-gun, Osaka 590-0494 (Japan)

2009-11-15

Since zirconium is considered an electrochemically active species under practical conditions of the electrorefining process, it is crucial to understand the electrochemical behavior of zirconium in LiCl-KCl melts containing actinide ions. In this study, the electrochemical codeposition of uranium and zirconium on a solid cathode was performed. It was found that the delta-(U, Zr) phase, which is the only intermediate phase of the uranium-zirconium binary alloy system, was deposited on a tantalum substrate by potentiostatic electrolysis at -1.60 V (vs. Ag{sup +}/Ag) in LiCl-KCl melts containing 0.13 in mol% UCl{sub 3} and 0.23 in mol% ZrCl{sub 4} at 773 K. To our knowledge, this is the first report on the electrochemical formation of the delta-(U, Zr) phase. The relative partial molar properties of uranium in the delta-(U, Zr) phase were evaluated by measuring the open-circuit-potentials of the electrochemically prepared delta-phase electrode.

Electrochemical formation of uranium-zirconium alloy in LiCl-KCl melts

International Nuclear Information System (INIS)

Murakami, Tsuyoshi; Kato, Tetsuya; Kurata, Masaki; Yamana, Hajimu

2009-01-01

Since zirconium is considered an electrochemically active species under practical conditions of the electrorefining process, it is crucial to understand the electrochemical behavior of zirconium in LiCl-KCl melts containing actinide ions. In this study, the electrochemical codeposition of uranium and zirconium on a solid cathode was performed. It was found that the δ-(U, Zr) phase, which is the only intermediate phase of the uranium-zirconium binary alloy system, was deposited on a tantalum substrate by potentiostatic electrolysis at -1.60 V (vs. Ag + /Ag) in LiCl-KCl melts containing 0.13 in mol% UCl 3 and 0.23 in mol% ZrCl 4 at 773 K. To our knowledge, this is the first report on the electrochemical formation of the δ-(U, Zr) phase. The relative partial molar properties of uranium in the δ-(U, Zr) phase were evaluated by measuring the open-circuit-potentials of the electrochemically prepared δ-phase electrode.

Arc melting in inert gas atmosphere of zirconium sponge

International Nuclear Information System (INIS)

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

1991-01-01

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

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)

Elastic properties of amorphous thin films studied by Rayleigh waves

International Nuclear Information System (INIS)

Schwarz, R.B.; Rubin, J.B.

1993-01-01

Physical vapor deposition in ultra-high vacuum was used to co-deposit nickel and zirconium onto quartz single crystals and grow amorphous Ni 1-x Zr x (0.1 < x < 0.87) thin film. A high-resolution surface acoustic wave technique was developed for in situ measurement of film shear moduli. The modulus has narrow maxima at x = 0. 17, 0.22, 0.43, 0.5, 0.63, and 0.72, reflecting short-range ordering and formation of aggregates in amorphous phase. It is proposed that the aggregates correspond to polytetrahedral atom arrangements limited in size by geometrical frustration

Hydrolysis of TBF and TiAP in presence of zirconium

International Nuclear Information System (INIS)

Vladimirova, M.V.; Kulikov, I.A.; Kuprij, A.A.

1992-01-01

Acid hydrolysis of organic solutions of tributyl phosphate (TBP) and tri-iso-amylphosphate (TiAP) in n-paraffin diluent in the presence of zirconium (0.025-0.1 mole/l) at nitric acid concentration of 0.3-1 mole/l is studied. Hydrolysis of extractants in a two-phase system, modelling conditions of spent fuel reprocessing and consisting of 1.1 mole/l TAP, 3 mole/l nitric acid at zirconium concentration in water phase 0.05-0.11 mole/l, at water-organic phase ratio 10:1 and at 60 deg C is also studied. Constants of TAP hydrolysis in organic and water phases are determined. Mechanism of increasing the TAP hydrolysis rate in zirconium presence is discussed. 5 refs., 2 figs., 5 tabs

Zirconium determination in refractories (gravimetric method)

International Nuclear Information System (INIS)

Capiotto, N.; Narahashi, Y.; Perish, C.G.; Souza, J.R.

1991-01-01

The zirconium determination in refractories is described, consisting in two separation methods for eliminating the interferences. The formatted product is calcined at 1100 0 C and determined gravimetrically as Zr P z 07. (author)

Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility.

Science.gov (United States)

Li, H F; Zhou, F Y; Li, L; Zheng, Y F

2016-04-19

In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are zirconium-ruthenium alloys (1.25 × 10(-6) cm(3)·g(-1)-1.29 × 10(-6) cm(3)·g(-1) for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti-6Al-4V, ~3.5 × 10(-6) cm(3)·g(-1), CP Ti and Ti-6Al-7Nb, ~3.0 × 10(-6) cm(3)·g(-1)), and one-sixth that of Co-Cr alloys (Co-Cr-Mo, ~7.7 × 10(-6) cm(3)·g(-1)). Among the Zr-Ru alloy series, Zr-1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr-Ru alloy system as therapeutic devices under MRI diagnostics environments.

Adsorption of zirconium from nitric acid solutions on hydrated tin dioxide

Energy Technology Data Exchange (ETDEWEB)

Tret' yakov, S Ya; Sharygin, L M; Egorov, Yu V

1977-01-01

Adsorption of zirconium from nitric acid solutions has been studied with the use of the labeled atom method on hydrated tin dioxide depending on the sorbate concentration, pH and prehistory of the solution. It has been found that adsorption behavior of zirconium essentially depends on its state in the solution.

Superconductivity in zirconium-rhodium alloys

Science.gov (United States)

Zegler, S. T.

1969-01-01

Metallographic studies and transition temperature measurements were made with isothermally annealed and water-quenched zirconium-rhodium alloys. The results clarify both the solid-state phase relations at the Zr-rich end of the Zr-Rh alloy system and the influence upon the superconducting transition temperature of structure and composition.

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.

Amine extraction of lead(II) and zirconium(IV) with succinate media

International Nuclear Information System (INIS)

Mahamuni, S.V.; Mane, C.P.; Sargar, B.M.; Rajmane, M.M.; Anuse, M.A.

2004-01-01

Lead is an important constituent of various alloys, which are in increasing demand in manufacture of batteries and nuclear shielding while the use of zirconium in nuclear power plants as entirely cladding uranium fuel is most important. This study was carried out to optimize the extraction conditions for Pb(II) and zirconium(IV)

Phyto-availability of zirconium in relation with initial speciation, solubility and soil characteristics

International Nuclear Information System (INIS)

Ferrand, E.; Benedetti, M.; Dumat, C.; Ferrand, E.; Leclerc-Cessac, E.

2005-01-01

During the last decades, the use of zirconium in industry has been widely developed and there is a potential risk of zirconium contamination. The long half-life isotope 93 Zr (T1/2=10 6 years) is largely observed in radioactive wastes. Therefore, the long-term prediction of the zirconium fate in the environment is essential. Due to its low solubility and strong tendency to polymerize, zirconium is usually considered as immobile, however the evidence of Zr mobility in certain conditions such as tropical weathering has been demonstrated. Soil-plant transfer is an important link in the chain of events which leads to radionuclide entry into the human food chain, but only few studies concern the Zr transfer to plants. The primary aim of this investigation is to verify if zirconium can be absorbed by edible plants (young peas and tomatoes) and to study the influence of Zr speciation on its availability. The second aim is to highlight the potential influence of plants on the Zr solubility in soil from the measurements of K d and with chemical extractions. Two agricultural top soils closed to the underground experimental laboratory (Meuse/Haute Marne, France) of the French National Agency for management of radioactive wastes (ANDRA) were collected: a sandy clayey loamy soil (A) and a clayey calcareous soil (B). The main differences between the two soils are: the pH, the texture and the carbonate content. In order to investigate the influence of the Zr speciation on its plant availability, soils were spiked with different forms of Zr chosen for their natural occurrence in the environment. Soil adsorption of Zr in batch experiments was realized (various initial [Zr], pH and I) in order to determine adsorption isotherms and partition coefficients (K d ). Tomatoes and peas were exposed to Zr by contact with the various soils during 8 days. After acidic digestion of the dried roots and aerial parts, the total Zr concentrations were measured by a quadrupole ICP-MS spectrometer

Fabrication of Pb (Zr, Ti) O3 Thin Film for Non-Volatile Memory Device Application

International Nuclear Information System (INIS)

Mar Lar Win

2011-12-01

Ferroelectric lead zirconate titanate powder was composed of mainly the oxides of titanium, zirconium and lead. PZT powder was firstly prepared by thermal synthesis at different Zr/Ti ratios with various sintering temperatures. PZT thin film was fabricated on SiO2/Si substrate by using thermal evaporation method. Physical and elemental analysis were carried out by using SEM, EDX and XRD The ferroelectric properties and the switching behaviour of the PZT thin films were investigated. The ferroelectric properties and switching properties of the PZT thin film (near morphotropic phase boundary sintered at 800 C) could function as a nonvolatile memory.

On composition and thermal degradation of basic zirconium sulfates

Energy Technology Data Exchange (ETDEWEB)

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

1988-02-01

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

On composition and thermal degradation of basic zirconium sulfates

International Nuclear Information System (INIS)

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

1988-01-01

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

Zirconium molybdate hydrate precipitates in spent nuclear fuel reprocessing

International Nuclear Information System (INIS)

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

2004-01-01

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

Zirconium microstructures: uncharted possibilities

International Nuclear Information System (INIS)

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

2015-01-01

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

Temperature dependence of lattice parameters of alpha-zirconium

International Nuclear Information System (INIS)

Versaci, R.A.; Ipohorski, M.

1991-01-01

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

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

International Nuclear Information System (INIS)

Ramasubramanian, N.

1991-01-01

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

A contribution to the study of arc melting in inert gas atmospheres of zirconium sponge

International Nuclear Information System (INIS)

Julio Junior, O.

1990-01-01

Mettalic zirconium is a material of great interest in the nuclear industry due to its low thermal neutron cross section, high strength and corrosion resistance. The latter permits its use in the chemical industry. In this study, a critical bibliographic revision of the industrial processes used for the melting and consolidation of zirconium sponge has been carried out. A procedure for the melting of zirconium on a laboratory scale, has been established. An nonconsumable-electrode arc furnace have been used. The effect of process variables like atmosphere, melting current and getter, have been showed. The influence of sponge characteristics on the qualities of cast zirconium buttons have been studied. The present study is a contribution towards future investigations to obtain high purity cast zirconium and its alloys commercially known as zircaloy. (author)

Design and development of novel MRI compatible zirconium- ruthenium alloys with ultralow magnetic susceptibility

Science.gov (United States)

Li, H.F.; Zhou, F.Y.; Li, L.; Zheng, Y.F.

2016-01-01

In the present study, novel MRI compatible zirconium-ruthenium alloys with ultralow magnetic susceptibility were developed for biomedical and therapeutic devices under MRI diagnostics environments. The results demonstrated that alloying with ruthenium into pure zirconium would significantly increase the strength and hardness properties. The corrosion resistance of zirconium-ruthenium alloys increased significantly. High cell viability could be found and healthy cell morphology observed when culturing MG 63 osteoblast-like cells and L-929 fibroblast cells with zirconium-ruthenium alloys, whereas the hemolysis rates of zirconium-ruthenium alloys are alloys and Ti-based alloys, the magnetic susceptibilities of the zirconium-ruthenium alloys (1.25 × 10−6 cm3·g−1–1.29 × 10−6 cm3·g−1 for zirconium-ruthenium alloys) are ultralow, about one-third that of Ti-based alloys (Ti–6Al–4V, ~3.5 × 10−6 cm3·g−1, CP Ti and Ti–6Al–7Nb, ~3.0 × 10−6 cm3·g−1), and one-sixth that of Co–Cr alloys (Co–Cr–Mo, ~7.7 × 10−6 cm3·g−1). Among the Zr–Ru alloy series, Zr–1Ru demonstrates enhanced mechanical properties, excellent corrosion resistance and cell viability with lowest magnetic susceptibility, and thus is the optimal Zr–Ru alloy system as therapeutic devices under MRI diagnostics environments. PMID:27090955

Study of solution speciation, soil retention and soil-plant transfer of zirconium

International Nuclear Information System (INIS)

Ferrand, E.

2005-12-01

Within the framework of the risks prevention policy of Andra, the radioactive zirconium introduction ( 93 Zr and 95 Zr) into the environment could be carried out starting from the nuclear waste whose storage is envisaged in deep geological layers. Thus, the goal of this study was to evaluate the parameters and phenomena influencing speciation (various chemical forms) and the soil-plant transfer of zirconium. Experiments of adsorption/desorption of zirconium with different ligands likely to be present in soils (goethite and humic acid) and with two soils, with contrasted characteristics, close to the underground research laboratory of Andra (Meuse) were carried out. These results of adsorption were then confronted with those obtained by the MUSIC and NICA-DONNAN models carried out using the computer code ECOSAT. Zr presents a strong affinity for the two types of soils and the soils constituents. Specific interactions of internal sphere type with the goethite were highlighted using the model. Soil-solution partition coefficients, or K d , values increase with pH and contact time. Various types of edible plants, pea (Pisum sativum L.) and tomato (Lycopersicon esculentum L cv. St Pierre) were cultivated in hydroponic conditions and in soils spiked with various sources of Zirconium. The maximum zirconium contents are mainly measured in the roots of the plants. The soil-plant transfer factors measured during these experiments show a weak bioavailability of zirconium. An influence of speciation on Zr bioavailability is however highlighted. Some chemical forms, such as oxychloride or acetate, are more easily mobilized than others by the plant. (author)

Preparation of zirconium molybdate gel for 99mTc gel generator

International Nuclear Information System (INIS)

Aliludin, Z.; Ohkubo, Masatake; Kushita, Kouhei

1988-09-01

Zirconium molybdate gel has excellent characteristics for use as column matrix material of 99m Tc generators. In this work, zirconium molybdate gels were prepared under different conditions; pH's of molybdate solutions from 2.5 to 7.0, Mo:Zr molar ratios from 0.7:1.0 to 1.3:1.0, drying temperatures from an ambient temperature to 200 deg C, and drying times from 1 h to 25 h. Contents of water, nitrate, molybdenum and zirconium were measured to examine the fundamental conditions in gel preparation. The Mo:Zr molar ratio was 1.0:1.0 for the most of gels obtained. A 99m Tc generator was prepared with an amorphous zirconium molybdate containing a tracer level of 99 Mo as column matrix material. Elution of 99m Tc was rapid and the average elution efficiency was 90 % for 6 ml elutions. Contents of radionuclidic impurities, Zr and Mo in the eluates, were low enough to meet the pharmacopoeia requirements for human use. (author)

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

Energy Technology Data Exchange (ETDEWEB)

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

1976-12-01

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

Fuel assembly and fuel cladding tube

International Nuclear Information System (INIS)

Tsutsumi, Shinro; Ito, Ken-ichi; Inagaki, Masatoshi; Nakajima, Junjiro.

1996-01-01

A fuel cladding tube is a zirconium liner tube formed by lining a pure zirconium layer on the inner side of a zirconium alloy tube. The fuel cladding tube is formed by extrusion molding of a composite billet formed by inserting a pure zirconium billet into a zirconium alloy billet. Accordingly, the pure zirconium layer and the zirconium alloy tube are strongly joined by metal bond. The fuel cladding tube has an external oxide film on the outer surface of the zirconium alloy tube and an internal oxide film on the inner side of the pure zirconium layer. The external oxide film has a thickness preferably of about 1μm. The internal oxide film has a thickness of not more than 10μm, preferably, from 1 to 5μm. With such a constitution, flaws to be formed on both inner and outer surfaces of the cladding tube upon assembling a fuel assembly can be reduced thereby enabling to reduce the amount of hydrogen absorbed to the cladding tube. (I.N.)

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

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.

Studies on inorganic exchanger: zirconium antimonate

International Nuclear Information System (INIS)

Dash, A.; Balasubramanian, K.R.

1992-01-01

The inorganic exchanger zirconium antimonate has been prepared and its characteristics evaluated. A method has been developed for the separation of 90 Sr and 144 Ce from fission products solution using this exchanger. (author). 23 refs., 18 f igs., 9 tabs

Pressure of saturated vapor of yttrium and zirconium acetylacetonates

Energy Technology Data Exchange (ETDEWEB)

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

1984-08-01

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

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

NARCIS (Netherlands)

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

2012-01-01

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

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

Science.gov (United States)

2010-07-01

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

Reduced-Gravity Measurements of the Effect of Oxygen on Properties of Zirconium

Science.gov (United States)

Zhao, J.; Lee, J.; Wunderlich, R.; Fecht, H.-J.; Schneider, S.; SanSoucie, M.; Rogers, J.; Hyers, R.

2016-01-01

The influence of oxygen on the thermophysical properties of zirconium is being investigated using MSL-EML (Material Science Laboratory - Electromagnetic Levitator) on ISS (International Space Station) in collaboration with NASA, ESA (European Space Agency), and DLR (German Aerospace Center). Zirconium samples with different oxygen concentrations will be put into multiple melt cycles, during which the density, viscosity, surface tension, heat capacity, and electric conductivity will be measured at various undercooled temperatures. The facility check-up of MSL-EML and the first set of melting experiments have been successfully performed in 2015. The first zirconium sample will be tested near the end of 2015. As part of ground support activities, the thermophysical properties of zirconium and ZrO were measured using a ground-based electrostatic levitator located at the NASA Marshall Space Flight Center. The influence of oxygen on the measured surface tension was evaluated. The results of this research will serve as reference data for those measured in ISS.

Cluster-assembled cubic zirconia films with tunable and stable nanoscale morphology against thermal annealing

Energy Technology Data Exchange (ETDEWEB)

Borghi, F.; Lenardi, C.; Podestà, A.; Milani, P., E-mail: pmilani@mi.infn.it [CIMAINA and Dipartimento di Fisica, Università degli Studi di Milano, via Celoria 16, 20133 Milano (Italy); Sogne, E. [CIMAINA and Dipartimento di Fisica, Università degli Studi di Milano, via Celoria 16, 20133 Milano (Italy); European School of Molecular Medicine (SEMM), IFOM-IEO, Milano (Italy); Merlini, M. [Dipartimento di Scienze della Terra “Ardito Desio”, Università degli Studi di Milano, via Mangiagalli 32, 20133 Milano (Italy); Ducati, C. [Department of Materials Science and Metallurgy, University of Cambridge, 27 Charles Babbage Road, Cambridge CB3 0FS (United Kingdom)

2016-08-07

Nanostructured zirconium dioxide (zirconia) films are very promising for catalysis and biotechnological applications: a precise control of the interfacial properties of the material at different length scales and, in particular, at the nanoscale, is therefore necessary. Here, we present the characterization of cluster-assembled zirconia films produced by supersonic cluster beam deposition possessing cubic structure at room temperature and controlled nanoscale morphology. We characterized the effect of thermal annealing in reducing and oxidizing conditions on the crystalline structure, grain dimensions, and topography. We highlight the mechanisms of film growth and phase transitions, which determine the observed interfacial morphological properties and their resilience against thermal treatments.

Cluster-assembled cubic zirconia films with tunable and stable nanoscale morphology against thermal annealing

International Nuclear Information System (INIS)

Borghi, F.; Lenardi, C.; Podestà, A.; Milani, P.; Sogne, E.; Merlini, M.; Ducati, C.

2016-01-01

Nanostructured zirconium dioxide (zirconia) films are very promising for catalysis and biotechnological applications: a precise control of the interfacial properties of the material at different length scales and, in particular, at the nanoscale, is therefore necessary. Here, we present the characterization of cluster-assembled zirconia films produced by supersonic cluster beam deposition possessing cubic structure at room temperature and controlled nanoscale morphology. We characterized the effect of thermal annealing in reducing and oxidizing conditions on the crystalline structure, grain dimensions, and topography. We highlight the mechanisms of film growth and phase transitions, which determine the observed interfacial morphological properties and their resilience against thermal treatments.

Cluster-assembled cubic zirconia films with tunable and stable nanoscale morphology against thermal annealing

KAUST Repository

Borghi, F.

2016-08-05

Nanostructured zirconium dioxide (zirconia) films are very promising for catalysis and biotechnological applications: a precise control of the interfacial properties of the material at different length scales and, in particular, at the nanoscale, is therefore necessary. Here, we present the characterization of cluster-assembled zirconia films produced by supersonic cluster beam deposition possessing cubic structure at room temperature and controlled nanoscale morphology. We characterized the effect of thermal annealing in reducing and oxidizing conditions on the crystalline structure, grain dimensions, and topography. We highlight the mechanisms of film growth and phase transitions, which determine the observed interfacial morphological properties and their resilience against thermal treatments. Published by AIP Publishing.

Cluster-assembled cubic zirconia films with tunable and stable nanoscale morphology against thermal annealing

KAUST Repository

Borghi, F.; Sogne, Elisa; Lenardi, C.; Podestà , A.; Merlini, M.; Ducati, C.; Milani, P.

2016-01-01

Nanostructured zirconium dioxide (zirconia) films are very promising for catalysis and biotechnological applications: a precise control of the interfacial properties of the material at different length scales and, in particular, at the nanoscale, is therefore necessary. Here, we present the characterization of cluster-assembled zirconia films produced by supersonic cluster beam deposition possessing cubic structure at room temperature and controlled nanoscale morphology. We characterized the effect of thermal annealing in reducing and oxidizing conditions on the crystalline structure, grain dimensions, and topography. We highlight the mechanisms of film growth and phase transitions, which determine the observed interfacial morphological properties and their resilience against thermal treatments. Published by AIP Publishing.

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

Czech Academy of Sciences Publication Activity Database

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

2017-01-01

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

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.

Bayesian model selection validates a biokinetic model for zirconium processing in humans

Science.gov (United States)

2012-01-01

Background In radiation protection, biokinetic models for zirconium processing are of crucial importance in dose estimation and further risk analysis for humans exposed to this radioactive substance. They provide limiting values of detrimental effects and build the basis for applications in internal dosimetry, the prediction for radioactive zirconium retention in various organs as well as retrospective dosimetry. Multi-compartmental models are the tool of choice for simulating the processing of zirconium. Although easily interpretable, determining the exact compartment structure and interaction mechanisms is generally daunting. In the context of observing the dynamics of multiple compartments, Bayesian methods provide efficient tools for model inference and selection. Results We are the first to apply a Markov chain Monte Carlo approach to compute Bayes factors for the evaluation of two competing models for zirconium processing in the human body after ingestion. Based on in vivo measurements of human plasma and urine levels we were able to show that a recently published model is superior to the standard model of the International Commission on Radiological Protection. The Bayes factors were estimated by means of the numerically stable thermodynamic integration in combination with a recently developed copula-based Metropolis-Hastings sampler. Conclusions In contrast to the standard model the novel model predicts lower accretion of zirconium in bones. This results in lower levels of noxious doses for exposed individuals. Moreover, the Bayesian approach allows for retrospective dose assessment, including credible intervals for the initially ingested zirconium, in a significantly more reliable fashion than previously possible. All methods presented here are readily applicable to many modeling tasks in systems biology. PMID:22863152

The technologies of zirconium production for nuclear fuel components in Ukraine

International Nuclear Information System (INIS)

Semenov, G.R.

2000-01-01

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

Arsenic removal from aqueous solutions by sorption onto zirconium- and titanium-modified sorbents

Directory of Open Access Journals (Sweden)

Ignjatović Ljubiša

2011-01-01

Full Text Available Arsenic reduction in drinking water can include treatment by adsorption, switching to alternative water sources, or blending with water that has a lower arsenic concentration. Commercial sorbents MTM, Greensand and BIRM (Clack Corporation were modified with zirconium and titanium after activation. The modifications were performed with titanium tetrachloride and zirconium tetrachloride. The modified sorbents were dried at different temperatures. The sorption of arsenate and arsenite dissolved in drinking water (200μg L-1 onto the sorbents were tested using a batch procedure. After removal of the sorbent, the concentration of arsenic was determined by HG-AAS. Zirconium-modified BIRM showed the best performance for the removal of both arsenite and arsenate. Modification of the greensand did not affect arsenic sorption ability. Zirconium-modified BIRM diminished the concentration of total As to below 5 μg L-1.

OPTIMIZATION OF COMPLEX MINERAL TANNING MATERIAL ON THE BASIS OF ALUMINIUM AND ZIRCONIUM

Directory of Open Access Journals (Sweden)

K. Toguzbaev

2012-01-01

Full Text Available Influence of acetate ion on stability of alumina-zirconium tanning to alkalization has been investigated in the paper. The investigation results have shown that at the ratio of Al3+:Zr4+:CH3COO = 1:1:1 it  is  possible  to  prepare  a  solution  of  masking   alumina-zirconium  tanning  (АЦД-М   with  high stability and low consumption of aluminum sulfate. The paper reveals that masking of alumina-zirconium tanning by natrium acetate allows to increase stability to alkalization and improve tanning properties. It has been established that for a stable increase of fatty matter viscosity and improvement of  leather water-resistant properties it is necessary to use water-insoluble aluminum and zirconium soaps of carboxylic acids.

Photometric determination of yttrium in zirconium-containing materials

International Nuclear Information System (INIS)

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

1984-01-01

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

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)

High temperature evaporation of titanium, zirconium and hafnium carbides

International Nuclear Information System (INIS)

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

1991-01-01

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

Study of point defect clustering in electron and ion irradiated zirconium alloys

International Nuclear Information System (INIS)

Hellio, C.; Boulanger, L.

1986-09-01

Dislocation loops created by 500 keV Zr + ions and 1 MeV electrons in zirconium have a/3 type Burgers vectors, and in ion irradiated samples, loops lie preferentially on planes close to (1010). From in-situ observations of loop growth under 1 MeV electron irradiation in zirconium and dilute Zr (Nb,O) alloys, a strong increase of the vacancy migration energy with oxygen concentration was observed, from 0.72 eV for pure zirconium to 1.7 eV for Zr and Zr-1% Nb doped with 1800 ppm weight oxygen, indicating large trapping of vacancies by O single interstitials or clusters

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.

Adsorption Isotherms of Cs+, Co2+, Zn2+ and Eu3+ on Zirconium Vanadate Ion-Exchanger

International Nuclear Information System (INIS)

Shady, S.A.; El-Ashery, S.M.; El-Naggar, I.M.

2009-01-01

Zirconium vanadate had been prepared by the dropwise addition of 0.1 M sodium vanadate and 0.1 M zirconyl chloride by molar ratio of zirconium/vanadium 2. Exchange isotherms for Cs + /H + , Co 2+ /H + ,Zn 2+ /H + and Eu 3+ /H + have been determined at 25, 40 and 60 degree C. Besides, it was proved that cesium, cobalt, zinc and europium are chemically adsorbed. Moreover, the heat of adsorption of these ions on zirconium vanadate had been calculated and indicated that zirconium vanadate is of endothermic behavior towards these ions

Neutronographic Texture Analysis of Zirconium Based Alloys

International Nuclear Information System (INIS)

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

2012-01-01

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

Development of Zirconium alloys (for pressure tubes)

Energy Technology Data Exchange (ETDEWEB)

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

1997-09-01

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

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

Science.gov (United States)

Al-Thobity, Ahmad M

2016-06-01

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

Five year survival analysis of an oxidised zirconium total knee arthroplasty.

Science.gov (United States)

Holland, Philip; Santini, Alasdair J A; Davidson, John S; Pope, Jill A

2013-12-01

Zirconium total knee arthroplasties theoretically have a low incidence of failure as they are low friction, hard wearing and hypoallergenic. We report the five year survival of 213 Profix zirconium total knee arthroplasties with a conforming all polyethylene tibial component. Data was collected prospectively and multiple strict end points were used. SF12 and WOMAC scores were recorded pre-operatively, at three months, at twelve months, at 3 years and at 5 years. Eight patients died and six were "lost to follow-up". The remaining 199 knees were followed up for five years. The mean WOMAC score improved from 56 to 35 and the mean SF12 physical component score improved from 28 to 34. The five year survival for failure due to implant related reasons was 99.5% (95% CI 97.4-100). This was due to one tibial component becoming loose aseptically in year zero. Our results demonstrate that the Profix zirconium total knee arthroplasty has a low medium term failure rate comparable to the best implants. Further research is needed to establish if the beneficial properties of zirconium improve long term implant survival. Copyright © 2012 Elsevier B.V. All rights reserved.

Modified lead titanate thin films for pyroelectric infrared detectors on gold electrodes

Science.gov (United States)

Ahmed, Moinuddin; Butler, Donald P.

2015-07-01

Pyroelectric infrared detectors provide the advantage of both a wide spectral response and dynamic range, which also has enabled systems to be developed with reduced size, weight and power consumption. This paper demonstrates the deposition of lead zirconium titanate (PZT) and lead calcium titanate (PCT) thin films for uncooled pyroelectric detectors with the utilization of gold electrodes. The modified lead titanate thin films were deposited by pulsed laser deposition on gold electrodes. The PZT and PCT thins films deposited and annealed at temperatures of 650 °C and 550 °C respectively demonstrated the best pyroelectric performance in this work. The thin films displayed a pyroelectric effect that increased with temperature. Poling of the thin films was carried out for a fixed time periods and fixed dc bias voltages at elevated temperature in order to increase the pyroelectric coefficient by establishing a spontaneous polarization of the thin films. Poling caused the pyroelectric current to increase one order of magnitude.

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.

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

Science.gov (United States)

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

2013-01-01

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

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.

Ferrier rearrangement promoted by an electrochemically generated zirconium catalyst.

Science.gov (United States)

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

2015-04-30

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

Solid-phase zirconium and fluoride species in alkaline zircaloy cladding waste at Hanford.

Science.gov (United States)

Reynolds, Jacob G; Huber, Heinz J; Cooke, Gary A; Pestovich, John A

2014-08-15

The United States Department of Energy Hanford Site, near Richland, Washington, USA, processed plutonium between 1944 and 1987. Fifty-six million gallons of waste of various origins remain, including waste from removing zircaloy fuel cladding using the so-called Zirflex process. The speciation of zirconium and fluoride in this waste is important because of the corrosivity and reactivity of fluoride as well as the (potentially) high density of Zr-phases. This study evaluates the solid-phase speciation of zirconium and fluoride using X-ray diffraction (XRD) and scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS). Two waste samples were analyzed: one waste sample that is relatively pure zirconium cladding waste from tank 241-AW-105 and another that is a blend of zirconium cladding wastes and other high-level wastes from tank 241-C-104. Villiaumite (NaF) was found to be the dominant fluoride species in the cladding waste and natrophosphate (Na7F[PO4]2 · 19H2O) was the dominant species in the blended waste. Most zirconium was present as a sub-micron amorphous Na-Zr-O phase in the cladding waste and a Na-Al-Zr-O phase in the blended waste. Some zirconium was present in both tanks as either rounded or elongated crystalline needles of Na-bearing ZrO2 that are up to 200 μm in length. These results provide waste process planners the speciation data needed to develop disposal processes for this waste. Copyright © 2014 Elsevier B.V. All rights reserved.

Zirconium-based alloys, nuclear fuel rods and nuclear reactors including such alloys, and related methods

Science.gov (United States)

Mariani, Robert Dominick

2014-09-09

Zirconium-based metal alloy compositions comprise zirconium, a first additive in which the permeability of hydrogen decreases with increasing temperatures at least over a temperature range extending from 350.degree. C. to 750.degree. C., and a second additive having a solubility in zirconium over the temperature range extending from 350.degree. C. to 750.degree. C. At least one of a solubility of the first additive in the second additive over the temperature range extending from 350.degree. C. to 750.degree. C. and a solubility of the second additive in the first additive over the temperature range extending from 350.degree. C. to 750.degree. C. is higher than the solubility of the second additive in zirconium over the temperature range extending from 350.degree. C. to 750.degree. C. Nuclear fuel rods include a cladding material comprising such metal alloy compositions, and nuclear reactors include such fuel rods. Methods are used to fabricate such zirconium-based metal alloy compositions.

Obtention of titanium and zirconium metallic

International Nuclear Information System (INIS)

Santos, P.R.G.; Rover, C.F.S.; Amaral, F.L.L.

1988-01-01

The development works of techniques and equipments for titanium and zirconium sponges obtention are mentioned. The Kroll Process used for the sponges production is described, consisting in the reduction of the metal tetracloride with magnesium in an inert atmosphere of helium or argon. (C.G.C.) [pt

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

Science.gov (United States)

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

2009-01-01

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

Preparation and characterization of very pure zirconium tetrafluoride. Application to fluorinated glass

International Nuclear Information System (INIS)

Bridenne, M.

1986-12-01

The synthesis of anhydrous and very pure zirconium tetrafluoride from zirconium tetraborohydride is studied. Zr F 4 is used for fabrication of fluorozirconate glass. Zr (BH 4 ) 4 is purified by sublimation. Two fluorinating agents F 2 and anhydrous HF are used for fluorination. The apparatus is made of fluorinated polymers and a Kel-F prototype reactor was realized. 20 g of Zr F 4 are obtained in 44 hrs with a yield of 88 %. Purity is characterized by chemical analysis (atomique absorption spectroscopy and spark mass spectroscopy) and absorption of an optical fiber made of zirconium tetrafluoride. Cr, Ni, Co and Cu content is lower than 0.1 ppm. Possibility of pilot scale production is discussed [fr

Study of solution speciation, soil retention and soil-plant transfer of zirconium; Etude de la speciation en solution, de la retention dans les sols et du transfert sol-plante du zirconium

Energy Technology Data Exchange (ETDEWEB)

Ferrand, E

2005-12-15

Within the framework of the risks prevention policy of Andra, the radioactive zirconium introduction ({sup 93}Zr and {sup 95}Zr) into the environment could be carried out starting from the nuclear waste whose storage is envisaged in deep geological layers. Thus, the goal of this study was to evaluate the parameters and phenomena influencing speciation (various chemical forms) and the soil-plant transfer of zirconium. Experiments of adsorption/desorption of zirconium with different ligands likely to be present in soils (goethite and humic acid) and with two soils, with contrasted characteristics, close to the underground research laboratory of Andra (Meuse) were carried out. These results of adsorption were then confronted with those obtained by the MUSIC and NICA-DONNAN models carried out using the computer code ECOSAT. Zr presents a strong affinity for the two types of soils and the soils constituents. Specific interactions of internal sphere type with the goethite were highlighted using the model. Soil-solution partition coefficients, or K{sub d}, values increase with pH and contact time. Various types of edible plants, pea (Pisum sativum L.) and tomato (Lycopersicon esculentum L cv. St Pierre) were cultivated in hydroponic conditions and in soils spiked with various sources of Zirconium. The maximum zirconium contents are mainly measured in the roots of the plants. The soil-plant transfer factors measured during these experiments show a weak bioavailability of zirconium. An influence of speciation on Zr bioavailability is however highlighted. Some chemical forms, such as oxychloride or acetate, are more easily mobilized than others by the plant. (author)

Scandium and zirconium ion complexing with salicylic acid

International Nuclear Information System (INIS)

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

1979-01-01

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

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

International Nuclear Information System (INIS)

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

2009-01-01

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

Deformation mechanisms and irradiation effects in zirconium alloys. A multi-scale study

International Nuclear Information System (INIS)

Onimus, Fabien

2015-01-01

Zirconium alloys have been used for more than 30 years in the nuclear industry as structural materials for the fuel assemblies of pressurized water reactors. In particular, the cladding tube, made of zirconium alloys, constitutes the first barrier against the dissemination of radioactive elements. It is therefore essential to have a good understanding and prediction of the mechanical behavior of these materials in various conditions. The work presented in this dissertation deals with an experimental study and numerical simulations, at several length scales, of the deformation mechanisms and the mechanical behavior of zirconium alloys before irradiation, but also after irradiation and under irradiation. The mechanical behavior of zirconium single crystal has been determined, during an original study, using tensile test specimens containing large grains. Based on this study, crystal plasticity constitutive laws have been proposed. A polycrystalline model has also been developed to simulate the behavior of unirradiated zirconium alloys. A thorough Transmission Electron Microscopy (TEM) study has been able to clarify the deformation mechanisms of zirconium alloys occurring after irradiation. The clearing of loops by gliding dislocations leading to the dislocation channeling mechanism has been studied in details. This phenomenon has also been simulated using a dislocation dynamics code. The macroscopic consequences of this process have also been analyzed. A polycrystalline model taking into account the specificity of this mechanism has eventually been proposed. This approach has then been extended to the post-irradiation creep behavior. The recovery of radiation defects during creep tests has been characterized by TEM and modeled using cluster dynamics method. Deformation modes during creep have also been studied and a simple model for the creep behavior has eventually been proposed. Finally, the mechanism responsible for the acceleration of irradiation growth that

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

Extraction and determination of hydrogen in uranium and zirconium; Extraction et dosage de l'hydrogene dans l'uranium et le zirconium

Energy Technology Data Exchange (ETDEWEB)

Champeix, L; Coblence, G; Darras, R [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

1959-07-01

The method of desorption under vacuum at high temperatures in the solid phase, which gives good results in the case of steels, has been applied to uranium and zirconium. In these two metals hydrogen is found mainly in the form of hydride. It is chiefly a question of determining the most suitable temperature and the heating time necessary to obtain an almost total extraction of hydrogen. Two considerations must be taken into account in the choice of temperature. It should be such that on the one hand the hydride decomposes rapidly and completely at the reduced pressure applied, and on the other hand the diffusion of hydrogen through the metal takes place fairly quickly. The apparatus and the method used are described; systematic tests have led to the adoption of temperatures of 650 deg. C for uranium and 1050 deg. C for zirconium. (author) [French] La methode de desorption sous vide a chaud en phase solide, methode qui donne de bons resultats dans le cas des aciers, a ete appliquee a l'uranium et au zirconium. Dans ces deux metaux, l'hydrogene se trouve surtout a l'etat d'hydrure. Il s'agit essentiellement de determiner la temperature optimum et la duree du chauffage necessaire pour obtenir une extraction d'hydrogene pratiquement complete. Deux considerations interviennent dans le choix de la temperature. Elle doit etre telle que, d'une part la decomposition de l'hydrure se fasse rapidement et completement sous la pression reduite realisee et d'autre part que la diffusion de l'hydrogene a travers le metal soit assez rapide. L'appareil et le mode operatoire utilises sont decrits des essais systematiques ont conduit a adopter une temperature de 650 deg. C pour l'uranium et de 1050 deg. C pour le zirconium. (auteur)

Tracing of salicylic acid additive during precipitation of zirconium

International Nuclear Information System (INIS)

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

2011-01-01

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

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

DEFF Research Database (Denmark)

Sørensen, E.; Bjerre, A.B.

1992-01-01

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

Calcification of MC3T3-E1 cells on titanium and zirconium.

Science.gov (United States)

Umezawa, Takayuki; Chen, Peng; Tsutsumi, Yusuke; Doi, Hisashi; Ashida, Maki; Suzuki, Shoichi; Moriyama, Keiji; Hanawa, Takao

2015-01-01

To confirm similarity of hard tissue compatibility between titanium and zirconium, calcification of MC3T3-E1 cells on titanium and zirconium was evaluated in this study. Mirror-polished titanium (Ti) and zirconium (Zr) disks and zirconium-sputter deposited titanium (Zr/Ti) were employed in this study. The surface of specimens were characterized using scanning electron microscopy and X-ray diffraction. Then, the cellular proliferation, differentiation and calcification of MC3T3-E1 cells on specimens were investigated. The surface of Zr/Ti was much smoother and cleaner than those of Ti and Zr. The proliferation of the cell was the same among three specimens, while the differentiation and calcification on Zr/Ti were faster than those on Ti and Zr. Therefore, Ti and Zr showed the identical hard tissue compatibility according to the evaluation with MC3T3-E1 cells. Sputter deposition may improve cytocompatibility.

The separation of plutonium from uranium and fission products on zirconium phosphate columns

Energy Technology Data Exchange (ETDEWEB)

Gal, I; Ruvarac, A [Institute of Nuclear Sciences Boris Kidric, Laboratorija za visoku aktivnost, Vinca, Beograd (Serbia and Montenegro)

1963-12-15

In recent years special attention has been given to the ion-exchange properties of zirconium phosphate and similar compounds in aqueous solutions. These inorganic cation exchangers are stable in oxidizing media and at elevated temperatures. Their resistance to ionizing radiation makes them particularly suitable for work with radioactive solutions. On account of this we considered ir worthwhile to investigate the separation of plutonium from uranium and fission products on zirconium phosphate columns. We were interested in nitric and solutions containing macro-amounts of uranium (a few grams per litre), and micro-amounts of plutonium and long-lived fission products. To obtain a better insight into the ion-exchange behaviour of the different ionic species towards zirconium phosphate, we first determined the dependence of the distribution coefficients of uranium, plutonium and fission product cations on the aqueous nitric acid concentration. Then, taking the distribution data as a guide, we separated plutonium on small glass columns filled with zirconium phosphate and calculated the decontamination factors (author)

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

Directory of Open Access Journals (Sweden)

Zhang Changrui

2016-07-01

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

Manufacture of titanium and zirconium hydrides

International Nuclear Information System (INIS)

Mares, F.; Hanslik, T.

1973-01-01

A method is described of manufacturing titanium and zirconium hydrides by hydrogenation of said metals characterized by the reaction temperature ranging between 250 to 500 degC, hydrogen pressure of 20 to 300 atm and possibly by the presence of a hydride of the respective metal. (V.V.)

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.

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.

Penetrate-leach dissolution of zirconium-clad uranium and uranium dioxide fuels

International Nuclear Information System (INIS)

Harmon, H.D.

1975-01-01

A new decladding-dissolution process was developed for zirconium-clad uranium metal and UO 2 fuels. The proposed penetrate-leach process consists of penetrating the zirconium cladding with Alniflex solution (2M HF--1M HNO 3 --1M Al(NO 3 ) 3 --0.1M K 2 Cr 2 O 7 ) and of leaching the exposed core with 10M HNO 3 . Undissolved cladding pieces are discarded as solid waste. Periodic HF and HNO 3 additions, efficient agitation, and in-line zirconium analyses are required for successful control of ZrF 4 and/or AlF 3 precipitation during the cladding-penetration step. Preliminary solvent extraction studies indicated complete recovery of uranium with 30 vol. percent tributyl phosphate (TBP) from both Alniflex solution and blended Alniflex-HNO 3 leach solutions. With 7.5 vol. percent TBP, high extractant/feed flow ratios and low scrub flows are required for satisfactory uranium recovery from Alniflex solution. Modified waste-handling procedures may be required for Alniflex waste, because it cannot be evaporated before neutralization and large quantities of solids are generated on neutralization. The effect of unstable UZr 3 (epsilon phase of uranium-zirconium system) on the safety of penetrate-leach dissolution was investigated

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

Towards an understanding of zirconium alloy corrosion

International Nuclear Information System (INIS)

Cox, B.

1976-08-01

A brief historical summary is given of the development of a programme for understanding the corrosion mechanisms operating for zirconium alloys. A general summary is given of the progress made, so far, in carrying through this programme. (author)

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

Science.gov (United States)

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

2013-07-01

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

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.)

Arylimido zirconium and titanium complexes. Characteristic structures and application in ethylene polymerization

Energy Technology Data Exchange (ETDEWEB)

Yuan, Shifang; Zhang, Jing [Shanxi Univ., Taiyuan (China). Inst. of Applied Chemistry; Wang, Lijing [Shanxi Univ., Taiyuan (China). School of Chemistry and Chemical Engineering; Hua, Yupeng [Shanxi Univ., Taiyuan (China). School of Chemistry and Chemical Engineering; Inner Mongolia Univ., Ordos (China). College of Ordos; Sun, Wen-Hua [Chinese Academy of Sciences, Beijing (China). Key Laboratory of Engineering Plastics

2016-07-01

Dimeric anilidolithium (ArHNLi.Et{sub 2}O){sub 2} (Ar=2,6-{sup i}Pr{sub 2}C{sub 6}H{sub 3}) reacted with zirconium tetrachloride in THF to give the heterometallic zirconium-lithium complex [(Et{sub 2}O){sub 2}Li(μ-Cl){sub 2}(ArHN)(ArN=)Zr(μ-Cl)]{sub 2} (C1) and with titanium tetrachloride in toluene to give the titanium complex [(ArN=)TiCl{sub 2}.(Et{sub 2}O){sub 2}] (C2) each in good isolated yields. Their molecular structures in the solid state were confirmed by X-ray diffraction analysis. Upon activation with methylaluminoxane, both arylimido zirconium and titanium complexes exhibited good catalytic activities toward ethylene polymerization.

Production kinetics of zirconium tetrachloride

International Nuclear Information System (INIS)

Sudjoko, D.; Masduki, B.; Sunardjo; Sulistyo, B.

1996-01-01

This research was intended to study the kinetics of zirconium tetrachloride production. The process was carried out in semi continuous reactor, equipped with heater, temperature controller, sublimator and scrubber. The variables investigated were time, temperature and the pellet forming pressure. Within the range of variables studied, the expression of the process in the chemical reaction controller region and diffusion controller region were both presented. (author)

Separation of hafnium from zirconium in sulfuric acid solutions using pressurized ion exchange

International Nuclear Information System (INIS)

Hurst, F.J.

1981-01-01

High-resolution pressurized ion exchange has been used successfully to study and separate hafnium and zirconium sulfate complexes by chromatographic elution from Dowex 50W-X8 (15 to 25 μm) resin with sulfuric acid solutions. Techniques were developed to continuously monitor the column effluents for zirconium and hafnium by reaction with fluorometric and colorimetric reagents. Since neither reagent was specific for either metal ion, peak patterns were initially identified by using the stable isotopes 90 Zr and 180 Hf as fingerprints of their elution position. Distribution ratios for both zirconium and hafnium decrease as the inverse fourth power of the sulfuric acid concentration below 2N and as the inverse second power at higher acid concentration. The hafnium-to-zirconium separation factor is approximately constant (approx. 8) over the 0.5 to 3N range. Under certain conditions, an unseparated fraction was observed that was not retained by the resin. The amount of this fraction which is thought to be a polymeric hydrolysis product appears to be a function of metal and sulfuric acid concentrations. Conditions are being sought to give the highest zirconium concentration and the lowest acid concentration that can be used as a feed material for commercial scale-up in the continuous annular chromatographic (CAC) unit without formation of the polymer

ZIRCONIUM PHOSPHATE ADSORPTION METHOD

Science.gov (United States)

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

1958-11-01

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

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

Control of microstructure during hot working of zirconium alloys

International Nuclear Information System (INIS)

Chakravartty, J.K.; Banerjee, S.

2005-01-01

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

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)

Production, applications and status of zirconium-89 immunoPET agents

International Nuclear Information System (INIS)

Jalilian, A.R.; Osso, Joao Alberto