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Sample records for situ oxide sintering

  1. Sintering of oxide-supported Pt and Pd nanoparticles in air studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose

    This thesis presents a fundamental study of the sintering of supported nanoparticles in relation to diesel oxidation catalysts. The sintering of supported nanoparticles is an important challenge in relation to this catalyst, as well as many other catalyst systems, and a fundamental understanding...... of Pt, Pd and bimetallic Pt-Pd nanoparticles supported on a flat and homogeneous Al2O3 or SiO2 surface. By using in situ TEM on the planar model catalysts it was possible to directly monitor the detailed dynamical changes of the individual nanoparticles during exposure to oxidizing conditions...

  2. Sintering of beryllium oxide

    International Nuclear Information System (INIS)

    Caillat, R.; Pointud, R.

    1955-01-01

    This study had for origin to find a process permitting to manufacture bricks of beryllium oxide of pure nuclear grade, with a density as elevated as possible and with standardized shape. The sintering under load was the technique kept for the manufacture of the bricks. Because of the important toxicity of the beryllium oxide, the general features for the preliminary study of the sintering, have been determined while using alumina. The obtained results will be able to act as general indication for ulterior studies with sintering under load. (M.B.) [fr

  3. Novel approaches for the in situ study of the sintering of nuclear oxide fuel materials and their surrogates

    Energy Technology Data Exchange (ETDEWEB)

    Clavier, Nicolas; Nkou Bouala, Galy Ingrid; Dacheux, Nicolas; Podor, Renaud [Montpellier Univ., Bagnols sur Ceze (France). ICSM - UMR 5257 CEA/CNRS/ENSCM; Lechelle, Jacques [CEA, DNE, DEC, SESC, LLCC, St-Paul lez Durance (France); Martinez, Julien [CEA, DEN, DTEC, SECA, LFC, Bagnols sur Ceze (France)

    2017-07-01

    Sintering is one of the key-points of the processing of ceramic materials. It is then of primary interest for the nuclear fuel cycle, in which it constitutes an important step in the fabrication of either UO{sub 2} or (U,Pu)O{sub 2} pellets used in current PWR reactors. The sintering of actinides oxides not only drives the final density and microstructure of the fuels, but also several characteristics that can impact significantly their behavior in the reactor. Dedicated tools are then needed to monitor the microstructure of such materials and forecast their evolution. In this frame, this paper presents the new potentialities offered by the use of environmental scanning electron microscope at high temperature (HT-ESEM) for the study of nuclear ceramics sintering. First, the results obtained from bulk pellets are detailed, either regarding original fundamental data at the grain level (such as grain boundaries and pores motion), or design of dedicated microstructures through the assessment of grain growth kinetics. Acquisition of sintering maps thanks to the combination of HT-ESEM observations and classical dilatometric measurements are also addressed. In a second part, observations undertaken at the 2-grain scale to monitor the first stage of sintering, dedicated to neck elaboration, are presented, and compared to the results currently provided by numerical models.

  4. Study of the oxide reduction and interstitial contents during sintering of different plain carbon steels by in situ mass spectrometry in nitrogen atmosphere

    International Nuclear Information System (INIS)

    Momeni, Mohammad; Gierl, Christian; Danninger, Herbert

    2011-01-01

    Highlights: → Degassing phenomenon was studied in plain steels with different iron base powders. → The integrated area below the MS m12 graph can be used as an indicator of formed CO. → The integrated area is an indicator for in situ carbon loss in the specimen. → Carbon loss and area below the m12 graph can be correlated. - Abstract: Reduction of oxides covering powder particles is an important process during sintering and a prerequisite to form sintering contacts in PM parts. In the present research, degassing and reduction phenomena during sintering of plain carbon steels prepared from different atomised and sponge iron powders were studied by mass spectrometry (MS) in the dilatometer under protective N 2 atmosphere. Interstitial constituents were measured by carbon and oxygen analysis. According to the results, the major part of CO 2 is formed during carbothermic reduction of surface oxides in the low to moderate temperature range ( 600 deg. C, the main product of carbothermic reduction is CO and not CO 2 , but the former cannot be detected by MS in N 2 atmosphere. Signals m44 (CO 2 ) and m12 (C) were however found to be reliable indicators for CO. Similar intensity of mass 12 signals for both ASC and SC up to 1000 deg. C is consistent with equal carbon loss through carbothermic reaction. The integrated areas below the MS signal graphs, and thus the areas of the different degassing peaks obtained in the MS, were used as at least semi-quantitative estimation of the amount of gases formed, bearing in mind that MS is not really a quantitative analytical tool. Although a clearly defined relationship is not visible between oxygen loss and area below the m16 graph, the area for m12 can be used as an indicator for in situ carbon loss in the specimen. Increasing integrated areas for m12 and 16 between 800 and 1300 deg. C with only marginal enhancement of m44 indicates that the major part of oxides are removed as CO, in agreement with Boudouard equilibrium, at

  5. Effect of low temperature in-situ sintering on the impedance and the performance of intermediate temperature solid oxide fuel cell cathodes

    DEFF Research Database (Denmark)

    Nielsen, Jimmi; Hjalmarsson, Per; Hansen, Martin Hangaard

    2014-01-01

    The effect of in-situ sintering temperature and time on the electronic conductivity, impedance and performance of IT-SOFC cathodes were studied. The studied cathodes were for comparison (La0.6Sr0.4)0.99CoO3 (LSC), (La0.6Sr0.4)0.99CoO3:Ce0.9Gd0.1O1.95 (LSC:CGO), La0.58Sr0.4Co0.2Fe0.8O3 (LSCF) and La......0.58Sr0.4Co0.2Fe0.8O3:Ce0.9Gd0.1O1.95 (LSCF:CGO). The LSCF-based cathodes showed poor sintering capabilities compared to the LSC-based cathodes in the studied temperature range of 650–950 °C. The poor necking between individual LSCF grains lower the electronic conductivity. Furthermore, poor cathode....../electrolyte adhesion was seen as an additional high frequency impedance arc, which gradually disappeared as the LSCF cathodes were sintered at increasing temperature. Effects on the impedance shape from poor cathode grain connectivity was shown through impedance simulations to result in a possible increase in the high...

  6. SINTERING OF NASCENT CALCIUM OXIDE

    Science.gov (United States)

    The paper discusses the measurement of the sintering rate of CaO in a nitrogen atmosphere at temperatures of 700-1100 C. CaO prepared from ultrapure CaCO3 was compared with an impure CaO derived from limestone. Both materials yielded an initial surface area of 104 sq m/g. The rat...

  7. In situ Transmission Electron Microscopy of catalyst sintering

    DEFF Research Database (Denmark)

    DeLaRiva, Andrew T.; Hansen, Thomas Willum; Challa, Sivakumar R.

    2013-01-01

    Recent advancements in the field of electron microscopy, such as aberration correctors, have now been integrated into Environmental Transmission Electron Microscopes (TEMs), making it possible to study the behavior of supported metal catalysts under operating conditions at atomic resolution. Here......, we focus on in situ electron microscopy studies of catalysts that shed light on the mechanistic aspects of catalyst sintering. Catalyst sintering is an important mechanism for activity loss, especially for catalysts that operate at elevated temperatures. Literature from the past decade is reviewed...... along with our recent in situ TEM studies on the sintering of Ni/MgAl2O4 catalysts. These results suggest that the rapid loss of catalyst activity in the earliest stages of catalyst sintering could result from Ostwald ripening rather than through particle migration and coalescence. The smallest...

  8. Integrated analysis of oxide nuclear fuel sintering

    International Nuclear Information System (INIS)

    Baranov, V.; Kuzmin, R.; Tenishev, A.; Timoshin, I.; Khlunov, A.; Ivanov, A.; Petrov, I.

    2011-01-01

    Dilatometric and thermal-gravimetric investigations have been carried out for the sintering process of oxide nuclear fuel in gaseous Ar - 8% H 2 atmosphere at temperatures up to 1600 0 C. The pressed compacts were fabricated under real production conditions of the OAO MSZ with application of two different technologies, so called 'dry' and 'wet' technologies. Effects of the grain size growth after the heating to different temperatures were observed. In order to investigate the effects produced by rate of heating on properties of sintered fuel pellets, the heating rates were varied from 1 to 8 0 C per minute. Time of isothermal overexposure at maximal temperature (1600 0 C) was about 8 hours. Real production conditions were imitated. The results showed that the sintering process of the fuel pellets produced by two technologies differs. The samples sintered under different heating rates were studied with application of scanning electronic microscopy analysis for determination of mean grain size. A simulation of heating profile for industrial furnaces was performed to reduce the beam cycles and estimate the effects of variation of the isothermal overexposure temperatures. Based on this data, an optimization of the sintering conditions was performed in operations terms of OAO MSZ. (authors)

  9. Sintering uranium oxide using a preheating step

    International Nuclear Information System (INIS)

    Jensen, N.J.; Nivas, Y.; Packard, D.R.

    1977-01-01

    Compacted pellets of uranium oxide or uranium oxide with one or more additives are heated in a kiln in a process having a preheating step, a sintering step, a reduction step, and a cooling step in a controlled atmosphere. The process is practiced to give a range of temperature and atmosphere conditions for obtaining optimum fluoride removal from the compacted pellets along with optimum sintering in a single process. The preheating step of this process is conducted in a temperature range of about 600 0 to about 900 0 C and the pellets are held for at least twenty min, and preferably about 60 min, in an atmosphere having a composition in the range of about 10 to about 75 vol % hydrogen with the balance being carbon dioxide. The sintering step is conducted at a temperature in the range of about 900 0 C to 1500 0 C in the presence of an atmosphere having a composition in the range of about 0.5 to about 90 vol % hydrogen with the balance being carbon dioxide. The reduction step reduces the oxygen to metal ratio of the pellets to a range of about 1.98 to 2.10:1 and this is accomplished by gradually cooling the pellets for about 30 to about 120 min from the temperature of the sintering step to about 1100 0 C in an atmosphere of about 10 to 90 vol % hydrogen with the balance being carbon dioxide. Thereafter the pellets are cooled to about 100 0 C under a protective atmosphere, and in one preferred practice the same atmosphere used in the reduction step is used in the cooling step. The preheating, sintering and reduction steps may also be conducted with their respective atmospheres having an initial additional component of water vapor and the water vapor can comprise up to about 20 vol %

  10. Boric oxide or boric acid sintering aid for sintering ceramics

    International Nuclear Information System (INIS)

    Lawler, H.A.

    1979-01-01

    The invention described relates to the use of liquid sintering aid in processes involving sintering of ceramic materials to produce dense, hard articles having industrial uses. Although the invention is specifically discussed in regard to compositions containing silicon carbide as the ceramic material, other sinterable carbides, for example, titanium carbide, may be utilized as the ceramic material. A liquid sintering aid for densifying ceramic material is selected from solutions of H 3 BO 3 , B 2 O 3 and mixtures of these solutions. In sintering ceramic articles, e.g. silicon carbide, a shaped green body is formed from a particulate ceramic material and a resin binder, and the green body is baked at a temperature of 500 to 1000 0 C to form a porous body. The liquid sintering aid of B 2 O 3 and/or H 3 BO 3 is then dispersed through the porous body and the treated body is sintered at a temperature of 1900 to 2200 0 C to produce the sintered ceramic article. (U.K.)

  11. Sintering of dioxide pellets in an oxidizing atmosphere (CO2)

    International Nuclear Information System (INIS)

    Santos, G.R.T.

    1992-01-01

    This work consists in the study of the sintering process of U O 2 pellets in an oxidizing atmosphere. Sintering tests were performed in an CO 2 atmosphere and the influence of temperature and time on the pellets density and microstructure were verified. The results obtained were compared to those from the conventional sintering process and its efficiency was confirmed. (author)

  12. The role of the native oxide shell on the microwave sintering of copper metal powder compacts

    International Nuclear Information System (INIS)

    Mahmoud, Morsi M.; Link, Guido; Thumm, Manfred

    2015-01-01

    Highlights: • Thin oxide native layer had a critical role on microwave sintering of copper. • Explain why microwaves interact with copper powder differently than its bulk. • Abnormal expansion in copper is due to the plastic deformation and crack formation. • In-situ setup gives important insight about the microwave sintering of metals. • Microwave sintering is a promising candidate technology in powder metallurgy. - Abstract: Successful microwave sintering of several metal powders had been reported by many researchers with remarkable improvements in the materials properties and/or in the overall process. However, the concept behind microwave heating of metal powders has not been fully understood till now, as it is well known that bulk metals reflect microwaves. The progress of microwave sintering of copper metal powder compacts was investigated via combining both in-situ electrical resistivity and dilatometry measurements that give important information about microstructural changes with respect to the inter-particle electrical contacts during sintering. The sintering behavior of copper metal powders was depending on the type of the gas used, particle size, the initial green density, the soaking sintering time and the thin oxide layer on the particles surfaces. The thin copper oxide native layer (ceramics) that thermodynamically formed on the particles surfaces under normal handling and ambient environmental conditions had a very critical and important role in the microwave absorption and interaction, the sintering behavior and the microstructural changes. This finding could help to have a fundamental understanding of why MW’s interact with copper metal powder in a different way than its bulk at room temperature, i.e. why a given metal powder could be heated using microwaves while its bulk reflects it

  13. Microstructure evolution during pressureless sintering of bulk oxide ceramics

    Directory of Open Access Journals (Sweden)

    Karel Maca

    2009-06-01

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

  14. Laser-Induced Reductive Sintering of Nickel Oxide Nanoparticles under Ambient Conditions

    KAUST Repository

    Paeng, Dongwoo; Lee, Daeho; Yeo, Junyeob; Yoo, Jae-Hyuck; Allen, Frances I.; Kim, Eunpa; So, Hongyun; Park, Hee K.; Minor, Andrew M.; Grigoropoulos, Costas P.

    2015-01-01

    © 2015 American Chemical Society. This work is concerned with the kinetics of laser-induced reductive sintering of nonstoichiometric crystalline nickel oxide (NiO) nanoparticles (NPs) under ambient conditions. The mechanism of photophysical reductive sintering upon irradiation using a 514.5 nm continuous-wave (CW) laser on NiO NP thin films has been studied through modulating the laser power density and illumination time. Protons produced due to high-temperature decomposition of the solvent present in the NiO NP ink, oxygen vacancies in the NiO NPs, and electronic excitation in the NiO NPs by laser irradiation all affect the early stage of the reductive sintering process. Once NiO NPs are reduced by laser irradiation to Ni, they begin to coalesce, forming a conducting material. In situ optical and electrical measurements during the reductive sintering process take advantage of the distinct differences between the oxide and the metallic phases to monitor the transient evolution of the process. We observe four regimes: oxidation, reduction, sintering, and reoxidation. A characteristic time scale is assigned to each regime.

  15. Laser-Induced Reductive Sintering of Nickel Oxide Nanoparticles under Ambient Conditions

    KAUST Repository

    Paeng, Dongwoo

    2015-03-19

    © 2015 American Chemical Society. This work is concerned with the kinetics of laser-induced reductive sintering of nonstoichiometric crystalline nickel oxide (NiO) nanoparticles (NPs) under ambient conditions. The mechanism of photophysical reductive sintering upon irradiation using a 514.5 nm continuous-wave (CW) laser on NiO NP thin films has been studied through modulating the laser power density and illumination time. Protons produced due to high-temperature decomposition of the solvent present in the NiO NP ink, oxygen vacancies in the NiO NPs, and electronic excitation in the NiO NPs by laser irradiation all affect the early stage of the reductive sintering process. Once NiO NPs are reduced by laser irradiation to Ni, they begin to coalesce, forming a conducting material. In situ optical and electrical measurements during the reductive sintering process take advantage of the distinct differences between the oxide and the metallic phases to monitor the transient evolution of the process. We observe four regimes: oxidation, reduction, sintering, and reoxidation. A characteristic time scale is assigned to each regime.

  16. Manufacture of sintered bricks of high density from beryllium oxide

    International Nuclear Information System (INIS)

    Pointud, R.; Rispal, Ch.; Le Garec, M.

    1959-01-01

    Beryllium oxide bricks of nuclear purity 100 x 100 x 50 and 100 x 100 x 100 mm of very high density (between 2.85 and 3.00) are manufactured by sintering under pressure in graphite moulds at temperatures between 1,750 and 1,850 deg. C, and under a pressure of 150 kg/cm 2 . The physico-chemical state of the saw material is of considerable importance with regard to the success of the sintering operation. In addition, a study of the sintering of a BeO mixture with 3 to 5 per cent of boron introduced in the form of boric acid, boron carbide or elementary boron shows that high densities can only be obtained by sintering under pressure. For technical reasons of manufacture, only the mixture based on boron carbide is used. The sintering is carried out in graphite moulds at 1500 deg. C under 150 kg/cm 2 pressure, and bricks can be obtained with density between 2,85 and 2,90. Laboratory studies and the industrial manufacture of various sinters are described in detail. (author) [fr

  17. Report on in-situ studies of flash sintering of uranium dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Raftery, Alicia Marie [Los Alamos National Lab. (LANL), Los Alamos, NM (United States)

    2017-01-24

    Flash sintering is a novel type of field assisted sintering that uses an electric field and current to provide densification of materials on very short time scales. The potential for field assisted sintering techniques to be used in producing nuclear fuel is gaining recognition due to the potential economic benefits and improvements in material properties. The flash sintering behavior has so far been linked to applied and material parameters, but the underlying mechanisms active during flash sintering have yet to be identified. This report summarizes the efforts to investigate flash sintering of uranium dioxide using dilatometer studies at Los Alamos National Laboratory and two separate sets of in-situ studies at Brookhaven National Laboratory’s NSLS-II XPD-1 beamline. The purpose of the dilatometer studies was to understand individual parameter (applied and material) effects on the flash behavior and the purpose of the in-situ studies was to better understand the mechanisms active during flash sintering. As far as applied parameters, it was found that stoichiometry, or oxygen-to-metal ratio, has a significant effect on the flash behavior (time to flash and speed of flash). Composite systems were found to have degraded sintering behavior relative to pure UO2. The critical field studies are complete for UO2.00 and will be analyzed against an existing model for comparison. The in-situ studies showed that the strength of the field and current are directly related to the sample temperature, with temperature-driven phase changes occurring at high values. The existence of an ‘incubation time’ has been questioned, due to a continuous change in lattice parameter values from the moment that the field is applied. Some results from the in-situ experiments, which should provide evidence regarding ion migration, are still being analyzed. Some preliminary conclusions can be made from these results with regard to using field assisted sintering to

  18. Ferritic oxide dispersion strengthened alloys by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Allahar, Kerry N., E-mail: KerryAllahar@boisestate.edu [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Burns, Jatuporn [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Jaques, Brian [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Wu, Y.Q. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States); Charit, Indrajit [Department of Chemical and Materials Engineering, University of Idaho, McClure Hall Room 405D, Moscow, ID 83844 (United States); Cole, James [Idaho National Laboratory, Idaho Falls, ID 83401 (United States); Butt, Darryl P. [Materials and Science Engineering Department, Boise State University, 1910 University Blvd., Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd., Idaho Falls, ID 83401 (United States)

    2013-11-15

    Spark plasma sintering (SPS) was used to consolidate a Fe–16Cr–3Al (wt.%) powder that was mechanically alloyed with Y{sub 2}O{sub 3} and Ti powders to produce 0.5 Y{sub 2}O{sub 3} and 0.5 Y{sub 2}O{sub 3}–1Ti powders. The effects of mechanical alloying and sintering conditions on the microstructure, relative density and hardness of the sintered oxide dispersion strengthened (ODS) alloys are presented. Scanning electron microscopy indicated a mixed fine-grain and coarse-grain microstructure that was attributed to recrystallization and grain growth during sintering. Analysis of the transmission electron microscopy (TEM) and atom probe tomography (APT) data identified Y–O and Y–O–Ti nanoclusters. Elemental ratios of these nanoclusters were consistent with that observed in hot-extruded ODS alloys. The influence of Ti was to refine the grains as well as the nanoclusters with there being greater number density and smaller sizes of the Y–O–Ti nanoclusters as compared to the Y–O nanoclusters. This resulted in the Ti-containing samples being harder than the Ti-free alloys. The hardness of the alloys with the Y–O–Ti nanoclusters was insensitive to sintering time while smaller hardness values were associated with longer sintering times for the alloys with the Y–O nanoclusters. Pressures greater than 80 MPa are recommended for improved densification as higher sintering temperatures and longer sintering times at 80 MPa did not improve the relative density beyond 97.5%.

  19. Sintering of uranium oxide of high specific surface area

    International Nuclear Information System (INIS)

    Bel, Alain; Francois, Bernard; Delmas, Roger; Caillat, Roger

    1959-01-01

    The extent to which a uranium oxide powder deriving from ammonium uranate or uranium peroxide lends itself to the sintering process depends largely on its specific surface area. When this is greater than 5 m 2 / g there is an optimum temperature for sintering in hydrogen. This temperature becomes less as the specific area of the powder is greater. Reprint of a paper published in Comptes rendus des seances de l'Academie des Sciences, t. 249, p. 1045-1047, sitting of 21 September 1959 [fr

  20. Sintering process optimization for multi-layer CGO membranes by in situ techniques

    DEFF Research Database (Denmark)

    Kaiser, Andreas; Prasad, A.S.; Foghmoes, Søren Preben Vagn

    2013-01-01

    The sintering of asymmetric CGO bi-layers (thin dense membrane on a porous support; Ce0.9Gd0.1O1.95-delta = CGO) with Co3O4 as sintering additive has been optimized by combination of two in situ techniques. Optical dilatometry revealed that bi-layer shape and microstructure are dramatically...... changing in a narrow temperature range of less than 100 degrees C. Below 1030 degrees C, a higher densification rate in the dense membrane layer than in the porous support leads to concave shape, whereas the densification rate of the support is dominant above 1030 degrees C, leading to convex shape. A fiat...... bi-layer could be prepared at 1030 degrees C, when shrinkage rates were similar. In situ van der Pauw measurements on tape cast layers during sintering allowed following the conductivity during sintering. A strong increase in conductivity and in activation energy E-a for conduction was observed...

  1. In-Situ Observation of Sintering Shrinkage of UO2 Compacts Derived from Different Powder Routes

    International Nuclear Information System (INIS)

    Rhee, Young Woo; Oh, Jang Soo; Kim, Dong Joo; Kim, Keon Sik; Kim, Jong Hun; Yang, Jae Ho; Koo, Yang Hyun

    2015-01-01

    In-situ observations on the shrinkage of green pellets with precisely controlled dimensions were carefully conducted by using TOM during H2 atmosphere sintering. The shrinkage retardation in IDR-UO 2 might be attributed to the larger primary particle size of IDRUO 2 than those of ADU- and AUC- UO 2 powders. It would be important to understand the different sintering characteristics of UO 2 powders according to the powder routes, when it comes to designing a new sintering process or choosing a sintering additive for new fuel pellet like PCI (Pellet Cladding Interaction) remedy pellet. In this paper, we have investigated the initial and intermediate sintering shrinkage of UO 2 from different powder routes by in-situ observation of green samples during H2 atmosphere sintering. Effect of powder characteristics of three different UO 2 powders on the initial and intermediate sintering were closely reviewed including crystal structure, powder size, specific surface area, primary crystal size, and O/U ratio

  2. Physical chemistry and modelling of the sintering of actinide oxides

    International Nuclear Information System (INIS)

    Lechelle, Jacques

    2013-01-01

    This report gives a synthesis of the work I have carried out or to which I have numerically contributed to from 1996 up to 2012 in the Department of Plutonium Uranium and minor Actinides in Cadarache CEA Center. Their main goal is the study and the modeling of the sintering process of nuclear fuels which is the unifying thread of this document. Both in order to take into account the physical and chemical features of the actinide bearing oxide material and in order to combine the different transport phenomena leading to sintering, a sub-granular scale model is under development. Extension to a varying chemical composition as well as exchanges with the gaseous phase are foreseen. A simulation on a larger scale (pellet scale) is ongoing in the framework of a PhD thesis. Validation means have been tested with (U,Pu)O 2 material on the scale of the pellet (Small Angle Neutron Diffusion), on the scale of powder granules (X-Ray High Resolution Micro-Tomography) and with CeO 2 at the 'Institut de Chimie Separative' in Marcoule on a single crystal scale (Environmental Scanning Electron Microscope). The required microstructure homogeneity for nuclear fuels has led to a campaign of experimental studies about the role of Cr 2 O 3 as a sintering aid. Whole of these studies improve our understanding of fuel sintering and hence leads to an improved mastering of this process. (author) [fr

  3. Constrained Sintering in Fabrication of Solid Oxide Fuel Cells.

    Science.gov (United States)

    Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

    2016-08-09

    Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs.

  4. Constrained Sintering in Fabrication of Solid Oxide Fuel Cells

    Science.gov (United States)

    Lee, Hae-Weon; Park, Mansoo; Hong, Jongsup; Kim, Hyoungchul; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook

    2016-01-01

    Solid oxide fuel cells (SOFCs) are inevitably affected by the tensile stress field imposed by the rigid substrate during constrained sintering, which strongly affects microstructural evolution and flaw generation in the fabrication process and subsequent operation. In the case of sintering a composite cathode, one component acts as a continuous matrix phase while the other acts as a dispersed phase depending upon the initial composition and packing structure. The clustering of dispersed particles in the matrix has significant effects on the final microstructure, and strong rigidity of the clusters covering the entire cathode volume is desirable to obtain stable pore structure. The local constraints developed around the dispersed particles and their clusters effectively suppress generation of major process flaws, and microstructural features such as triple phase boundary and porosity could be readily controlled by adjusting the content and size of the dispersed particles. However, in the fabrication of the dense electrolyte layer via the chemical solution deposition route using slow-sintering nanoparticles dispersed in a sol matrix, the rigidity of the cluster should be minimized for the fine matrix to continuously densify, and special care should be taken in selecting the size of the dispersed particles to optimize the thermodynamic stability criteria of the grain size and film thickness. The principles of constrained sintering presented in this paper could be used as basic guidelines for realizing the ideal microstructure of SOFCs. PMID:28773795

  5. Sintering of uranium dioxide pellets (UO2) in an oxidizing atmosphere (C O2)

    International Nuclear Information System (INIS)

    Santos, G.R.T.

    1992-01-01

    This work consists in the study of the sintering process of U O 2 pellets in an oxidizing atmosphere. Sintering tests were performed in an CO 2 atmosphere and the influence of temperature and time on the pellets density and microstructure were verified. The results obtained were compared to those from the conventional sintering process and its efficiency was confirmed. (author)

  6. In situ observation and neutron diffraction of NiTi powder sintering

    International Nuclear Information System (INIS)

    Chen, Gang; Liss, Klaus-Dieter; Cao, Peng

    2014-01-01

    This study investigated NiTi powder sintering behaviour from elemental powder mixtures of Ni/Ti and Ni/TiH 2 using in situ neutron diffraction and in situ scanning electron microscopy. The sintered porous alloys have open porosities ranging from 2.7% to 36.0%. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH 2 compact leads to less densification yet higher chemical homogenization only after high-temperature sintering. For the first time, direct evidence of the eutectoid phase transformation of NiTi at 620 °C is reported by in situ neutron diffraction. A comparative study of cyclic stress–strain behaviours of the porous NiTi alloys made from Ni/Ti and Ni/TiH 2 compacts indicate that the samples sintered from the Ni/TiH 2 compact exhibited a much higher porosity, larger pore size, lower fracture strength, lower close-to-overall porosity ratio and lower Young’s modulus. Instead of enhanced densification by the use of TiH 2 as reported in the literature, this study shows an adverse effect of TiH 2 on powder densification in NiTi

  7. An in situ Study of NiTi Powder Sintering Using Neutron Diffraction

    Directory of Open Access Journals (Sweden)

    Gang Chen

    2015-04-01

    Full Text Available This study investigates phase transformation and mechanical properties of porous NiTi alloys using two different powder compacts (i.e., Ni/Ti and Ni/TiH2 by a conventional press-and-sinter means. The compacted powder mixtures were sintered in vacuum at a final temperature of 1373 K. The phase evolution was performed by in situ neutron diffraction upon sintering and cooling. The predominant phase identified in all the produced porous NiTi alloys after being sintered at 1373 K is B2 NiTi phase with the presence of other minor phases. It is found that dehydrogenation of TiH2 significantly affects the sintering behavior and resultant microstructure. In comparison to the Ni/Ti compact, dehydrogenation occurring in the Ni/TiH2 compact leads to less densification, yet higher chemical homogenization, after high temperature sintering but not in the case of low temperature sintering. Moreover, there is a direct evidence of the eutectoid decomposition of NiTi at ca. 847 and 823 K for Ni/Ti and Ni/TiH2, respectively, during furnace cooling. The static and cyclic stress-strain behaviors of the porous NiTi alloys made from the Ni/Ti and Ni/TiH2 compacts were also investigated. As compared with the Ni/Ti sintered samples, the samplessintered from the Ni/TiH2 compact exhibited a much higher porosity, a higher close-to-total porosity, a larger pore size and lower tensile and compressive fracture strength.

  8. In situ process monitoring in selective laser sintering using optical coherence tomography

    Science.gov (United States)

    Gardner, Michael R.; Lewis, Adam; Park, Jongwan; McElroy, Austin B.; Estrada, Arnold D.; Fish, Scott; Beaman, Joseph J.; Milner, Thomas E.

    2018-04-01

    Selective laser sintering (SLS) is an efficient process in additive manufacturing that enables rapid part production from computer-based designs. However, SLS is limited by its notable lack of in situ process monitoring when compared with other manufacturing processes. We report the incorporation of optical coherence tomography (OCT) into an SLS system in detail and demonstrate access to surface and subsurface features. Video frame rate cross-sectional imaging reveals areas of sintering uniformity and areas of excessive heat error with high temporal resolution. We propose a set of image processing techniques for SLS process monitoring with OCT and report the limitations and obstacles for further OCT integration with SLS systems.

  9. Effect of Ca-Fe oxides additives on NOx reduction in iron ore sintering

    Institute of Scientific and Technical Information of China (English)

    Zhi-yuan Yu; Xiao-hui Fan; Min Gan; Xu-ling Chen

    2017-01-01

    As the emission control regulations get stricter, the NOx reduction in the sintering process becomes an important environmental concern owing to its role in the formation of photochemical smog and acid rain. The NOx emissions from the sintering machine account for 48% of total amount from the iron and steel industry.Thus, it is essential to reduce NOx emissions from the sintering machine, for the achievement of clean production of sinter.Ca-Fe oxides, serving as the main binding phase in the sinter, are therefore used as additives into the sintering mixture to reduce NOx emissions.The results show that the NOx re-duction ratio achieves 27.76% with 8% Ca-Fe oxides additives since the Ca-Fe oxides can advance the ig-nition and inhibit the nitrogen oxidation compared with the conventional condition.Meanwhile, the exist-ence of Ca-Fe oxides was beneficial to the sinter quality since they were typical low melting point com-pounds.The optimal mass fraction of Ca-Fe oxides additives should be less than 8% since the permeability of sintering bed was significantly decreased with a further increase of the Ca-Fe oxides fines, inhibiting the mineralization reaction of sintering mixture.Additionally, the appropriate particle size can be obtained when mixing an equal amount of Ca-Fe oxides additives of -0.5 mm and 0.5-3.0 mm in size.

  10. Method of manufacturing gadolinium oxide-incorporated nuclear fuel sintering products

    International Nuclear Information System (INIS)

    Komono, Akira; Seki, Makoto; Omori, Sadayuki.

    1987-01-01

    Purpose: To manufacture nuclear fuel sintering products excellent in burning property and mechanical property. Constitution: In the manufacturing step for nuclear fuel sintering products, specific metal oxides are added for promoting the growth of crystal grains in the sintering. Those metal oxides melted at a temperature lower than the sintering temperature of a mixture of nuclear fuel oxide powder and oxide power, or those metal oxides causing eutectic reaction are used as the metal oxide. Particularly, those compounds having oxygen atom - metal atom ratio (O/M) of not less than 2 are preferably used. As such metal oxides usable herein transition metal oxides, e.g., Nb 2 O 5 , TiO 2 , MoO 3 and WO 3 are preferred, with Nb 2 O 3 and TiO 2 being preferred particularly. (Seki, T.)

  11. Standard specification for sintered gadolinium oxide-uranium dioxide pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2008-01-01

    1.1 This specification is for finished sintered gadolinium oxide-uranium dioxide pellets for use in light-water reactors. It applies to gadolinium oxide-uranium dioxide pellets containing uranium of any 235U concentration and any concentration of gadolinium oxide. 1.2 This specification recognizes the presence of reprocessed uranium in the fuel cycle and consequently defines isotopic limits for gadolinium oxide-uranium dioxide pellets made from commercial grade UO2. Such commercial grade UO2 is defined so that, regarding fuel design and manufacture, the product is essentially equivalent to that made from unirradiated uranium. UO2 falling outside these limits cannot necessarily be regarded as equivalent and may thus need special provisions at the fuel fabrication plant or in the fuel design. 1.3 This specification does not include (1) provisions for preventing criticality accidents or (2) requirements for health and safety. Observance of this specification does not relieve the user of the obligation to be aw...

  12. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    International Nuclear Information System (INIS)

    Majidi, Hasti; Holland, Troy B.; Benthem, Klaus van

    2015-01-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior

  13. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, Hasti [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States); Holland, Troy B. [Department of Mechanical Engineering, Colorado State University, Fort Collins, CO 80523 (United States); Benthem, Klaus van, E-mail: benthem@ucdavis.edu [Department of Chemical Engineering and Materials Science, University of California, Davis, CA 95616 (United States)

    2015-05-15

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior.

  14. Quantitative analysis for in situ sintering of 3% yttria-stablized zirconia in the transmission electron microscope.

    Science.gov (United States)

    Majidi, Hasti; Holland, Troy B; van Benthem, Klaus

    2015-05-01

    Studying particle-agglomerate systems compared to two-particle systems elucidates different stages of sintering by monitoring both pores and particles. We report on in situ sintering of 3% yttria-stablized zirconia particle agglomerates in the transmission electron microscope (TEM). Real-time TEM observations indicate neck formation and growth, particle coalescence and pore closure. A MATLAB-based image processing tool was developed to calculate the projected area of the agglomerate with and without internal pores during in situ sintering. We demonstrate the first densification curves generated from sequentially acquired TEM images. The in situ sintering onset temperature was then determined to be at 960 °C. Densification curves illustrated that the agglomerate projected area which excludes the internal observed pores also shrinks during in situ sintering. To overcome the common projection problem for TEM analyses, agglomerate mass-thickness maps were obtained from low energy-loss analysis combined with STEM imaging. The decrease in the projected area was directly related to the increase in mass-thickness of the agglomerate, likely caused by hidden pores existing in the direction of the beam. Access to shrinkage curves through in situ TEM analysis provides a new avenue to investigate fundamental mechanisms of sintering through directly correlating microstructural changes during consolidation with mesoscale densification behavior. Copyright © 2014 Elsevier B.V. All rights reserved.

  15. Cermet sintering on the oase of molybdenum, nickel, aluminium oxide in dry and wet hydrogen medium

    International Nuclear Information System (INIS)

    Fedotov, A.V.; Lutskaya, E.Eh.

    1985-01-01

    Cermet sintering on the base of molybdenum, nickel and aluminium oxide in dry and wer hydrogen medium is studied. It is stated that presence of water vapours permits to decrease sintering temperature of molybdenum containing cermets and to prepare dense nickeliferous cermets. Cermet density can he rather high at final stages of sintering that is probably conditioned by decrease of growth rate of corundum crystals. Pressing pressure activates cermet siptering at intermediate stages and it is low effective at finite stages of condensation. Constancy of relative reduction of void volume is preserved only at final stages of sintering

  16. In-Situ Observation of Sintering Shrinkage of UO{sub 2} Compacts Derived from Different Powder Routes

    Energy Technology Data Exchange (ETDEWEB)

    Rhee, Young Woo; Oh, Jang Soo; Kim, Dong Joo; Kim, Keon Sik; Kim, Jong Hun; Yang, Jae Ho; Koo, Yang Hyun [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2015-10-15

    In-situ observations on the shrinkage of green pellets with precisely controlled dimensions were carefully conducted by using TOM during H2 atmosphere sintering. The shrinkage retardation in IDR-UO{sub 2} might be attributed to the larger primary particle size of IDRUO{sub 2} than those of ADU- and AUC- UO{sub 2} powders. It would be important to understand the different sintering characteristics of UO{sub 2} powders according to the powder routes, when it comes to designing a new sintering process or choosing a sintering additive for new fuel pellet like PCI (Pellet Cladding Interaction) remedy pellet. In this paper, we have investigated the initial and intermediate sintering shrinkage of UO{sub 2} from different powder routes by in-situ observation of green samples during H2 atmosphere sintering. Effect of powder characteristics of three different UO{sub 2} powders on the initial and intermediate sintering were closely reviewed including crystal structure, powder size, specific surface area, primary crystal size, and O/U ratio.

  17. CALCIUM OXIDE SINTERING IN ATMOSPHERES CONTAINING WATER AND CARBON DIOXIDE

    Science.gov (United States)

    The paper gives results of measurements of the effects of water vapor and CO2 on the sintering rate of nascent CaO, as a function of partial pressure and temperature using CaO prepared by rapid decomposition of CaCO3 and CA(OH)2. Each gas strongly catalyzed the sintering process ...

  18. Effect of process parameters on surface oxides on chromium-alloyed steel powder during sintering

    International Nuclear Information System (INIS)

    Chasoglou, D.; Hryha, E.; Nyborg, L.

    2013-01-01

    The use of chromium in the PM steel industry today puts high demands on the choice and control of the atmosphere during the sintering process due to its high affinity to oxygen. Particular attention is required in order to control the surface chemistry of the powder which in turn is the key factor for the successful sintering and production of PM parts. Different atmosphere compositions, heating rates and green densities were employed while performing sintering trials on water atomized steel powder pre-alloyed with 3 wt.% Cr in order to evaluate the effect on surface chemical reactions. Fracture surfaces of sintered samples were examined using high resolution scanning electron microscopy combined with X-ray microanalysis. The investigation was complemented with thermogravimetric (TG) studies. Reaction products in particulate form containing strong-oxide forming elements such as Cr, Si and Mn were formed during sintering for all conditions. Processing in vacuum results in intensive inter-particle neck development during the heating stage and consequently in the excessive enclosure of surface oxide which is reflected in less good final mechanical properties. Enhanced oxide reduction was observed in samples processed in hydrogen-containing atmospheres independent of the actual content in the range of 3–10 vol.%. An optimum heating rate was required for balancing reduction/oxidation processes. A simple model for the enclosure and growth of oxide inclusions during the sinter-neck development is proposed. The obtained results show that significant reduction of the oxygen content can be achieved by adjusting the atmosphere purity/composition. - Highlights: ► A local atmosphere microclimate is very important for sintering of PM steels. ► High risk of surface oxide enclosure between 800 and 1000 °C. ► Coalescence and agglomeration of enclosed oxides take place during sintering. ► The effect of different process parameters on the oxide reduction is examined. ► A

  19. Effect of Sintering Temperature on the Properties of Aluminium-Aluminium Oxide Composite Materials

    Directory of Open Access Journals (Sweden)

    Dewan Muhammad Nuruzzaman

    2016-12-01

    Full Text Available In this study, aluminium-aluminium oxide (Al-Al2O3 metal matrix composites of different weight percentage reinforcements of aluminium oxide were processed at different sintering temperatures. In order to prepare these composite specimens, conventional powder metallurgy (PM method was used. Three types specimens of different compositions such as 95%Al+5%Al2O3, 90%Al+10%Al2O3 and 85%Al+15%Al2O3 were prepared under 20 Ton compaction load. Then, all the specimens were sintered in a furnace at two different temperatures 550oC and 580oC. In each sintering process, two different heating cycles were used. After the sintering process, it was observed that undistorted flat specimens were successfully prepared for all the compositions. The effects of sintering temperature and weight fraction of aluminium oxide particulates on the density, hardness and microstructure of Al-Al2O3 composites were observed. It was found that density and hardness of the composite specimens were significantly influenced by sintering temperature and percentage aluminium oxide reinforcement. Furthermore, optical microscopy revealed that almost uniform distribution of aluminium oxide reinforcement within the aluminium matrix was achieved.

  20. Photoacoustic spectroscopy investigation of sintered zinc-tin-oxide ceramics

    Directory of Open Access Journals (Sweden)

    Ivetić Tamara B.

    2007-01-01

    Full Text Available In this paper the changes that occurred in differently activated ZnO-SnO2 and sintered samples were investigated using photoacoustic spectroscopy. ZnO and SnO2 powders, mixed in the molar ratio 2:1, were mechanically activated in a planetary ball mill for 10-160 min. The mixtures were pres­sed and isothermally sintered at 1300°C for two hours. X-ray diffraction analysis of the obtained sintered samples was performed in order to investigate changes of the phase composition and confirmed only the presence of a pure zinc stannate (Zn2SnO4 phase in all the sintered samples as a result of the solid state reaction and reaction sintering between the starting ZnO and SnO2 powders. The microstructure of the sintered sam­ples was examined by scanning electron microscopy and showed that mechanical activation leads to the formation of a structure with reduced particle size which accelerates spinel formation. Grain growth of the spinel phase slows down the densification process and together with the agglomerates formed during mechanical activation causes the appearance of a porous microstructure. The photoacoustic (PA phase and amplitude spectra of the sintered samples were recorded as a function of the chopped frequency of the laser beam used (red laser with a power of 25 mW, λ=632 nm in a thermal-transmission detection configuration. PA experimental data were analyzed using the Rosenzweig-Gersho thermal-piston model, which enabled determination of the thermal diffusivity, ZT (m2s-1, diffusion coefficient of the minority free carriers D (m2s-1 and the optical absorption coefficient (m-1. The detected differences of the measured thermal-electrical properties of the obtained Zn2SnO4 ceramics indicate changes in the material induced by the different preparation procedure of the starting powders before the sintering process.

  1. In situ formation of sintered cordierite–mullite nano–micro composites by utilizing of waste silica fume

    International Nuclear Information System (INIS)

    Khattab, R.M.; EL-Rafei, A.M.; Zawrah, M.F.

    2012-01-01

    Highlights: ► We succeeded to obtain in situ formed sintered cordierite–mullite nano–macro composites from waste and pure materials at 1400 °C. ► Their sinterability was greatly dependent on both firing temperature and composition. ► XRD patterns showed that the optimum temperature required for formation of sintered cordierite–mullite nano–macro composites was achieved at 1400 °C. ► The batch containing 70 wt.% cordierite and 30 wt.% mullite exhibited the best properties. ► Microstructures of the densified composites were composed of nano–macro cordierite–mullite structures. -- Abstract: This study aims at in situ formation of sintered cordierite–mullite nano–macro composites having high technological properties using waste silica fume, calcined ball clay, calcined alumina, and magnesia as starting materials. The starting materials were mixed in different ratios to obtain different cordierite–mullite composite batches in which the cordierite contents ranged from 50 to 100 wt.%. The batches were uni-axially pressed at 100 MPa and sintered at 1350, 1400 and 1450 °C to select the optimum temperature required for cordierite–mullite nano–macro composites formation. The formed phases were identified by X-ray diffraction (XRD) pattern. The sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined. The microstructure of composites has been investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered batches was evaluated. The result revealed that the cordierite–mullite nano–macro composites were in-situ formed at 1400 °C. The batch containing 70 wt.% cordierite showed good physical and mechanical properties.

  2. ADVANTAGES/DISADVANTAGES FOR ISCO METHODS IN-SITU FENTON OXIDATION IN-SITU PERMANGANATE OXIDATION

    Science.gov (United States)

    The advantages and disadvantages of in-situ Fenton oxidation and in-situ permanganate oxidation will be presented. This presentation will provide a brief overview of each technology and a detailed analysis of the advantages and disadvantages of each technology. Included in the ...

  3. Laser sintering of magnesia with nanoparticles of iron oxide and aluminum oxide

    International Nuclear Information System (INIS)

    García, L.V.; Mendivil, M.I.; Roy, T.K. Das; Castillo, G.A.; Shaji, S.

    2015-01-01

    Highlights: • Laser sintered MgO pellets with nanoparticles of Al 2 O 3 and Fe 2 O 3 . • Characterized these pellets by XRD, SEM and XPS. • Spinel formations were observed in both cases. • Changes in morphology and structure were analyzed. - Abstract: Nanoparticles of iron oxide (Fe 2 O 3 , 20–40 nm) and aluminum oxide (Al 2 O 3 , 50 nm) were mixed in different concentrations (3, 5 and 7 wt%) in a magnesium oxide (MgO) matrix. The mixture pellet was irradiated with 532 nm output from a Q-switched Nd:YAG laser using different laser fluence and translation speed for sintering. The refractory samples obtained were analyzed using X-ray diffraction technique, scanning electron microscopy and X-ray photoelectron spectroscopy. The results showed that the samples irradiated at translation speed of 110 μm/s and energy fluence of 1.7 J/cm 2 with a concentration of 5 and 7 wt% of Fe 2 O 3 presented the MgFe 2 O 4 spinel-type phase. With the addition of Al 2 O 3 nanoparticles, at a translation speed of 110 μm/s and energy fluence of 1.7 J/cm 2 , there were the formations of MgAl 2 O 4 spinel phase. The changes in morphologies and microstructure due to laser irradiation were analyzed

  4. Nanocrystalline NdFeB magnet prepared by mechanically activated disproportionation and desorption-recombination in-situ sintering

    International Nuclear Information System (INIS)

    Xiaoya, Liu; Yuping, Li; Lianxi, Hu

    2013-01-01

    The process of mechanically activated disproportionation and desorption-recombination in-situ sintering was proposed to synthesize highly densified nanocrystalline NdFeB magnet, and its validity was demonstrated by experimental investigation with the use of a Nd 16 Fe 76 B 8 (atomic ratio) alloy. Firstly, the as-cast alloy was disproportionated by mechanical milling in hydrogen, with the starting micron-sized Nd 2 Fe 14 B phase decomposed into an intimate mixture of nano-structured NdH 2.7 , Fe 2 B and α-Fe phases. The as-disproportionated alloy powders were compacted by cold pressing and then subjected to desorption-recombination in-situ sintering. The microstructure of both the as-disproportionated and the subsequently sintered samples was characterized by X-ray diffraction and electron transmission microscopy, respectively. The magnetic properties of the sintered samples were measured by using vibrating sample magnetometer. The results showed that, by vacuum sintering, not only was the powder compact consolidated, but also the as-disproportionated microstucture transformed into nanocrystalline Nd 2 Fe 14 B phase via the well-known desorption-recombination reaction, thus giving rise to nanocrystalline NdFeB magnet. In the present study, the optimal sintering parameters were found to be 780 °C×30 min. In this case, the coercivity, the remanence, and maximum energy product of the magnet sample achieved 0.8 T, 635.3 kA/m, and 106.3 kJ/m 3 , respectively. - Highlights: ► Nano-structured disproportionated NdFeB alloy powders by mechanical milling in hydrogen. ► Highly densified green magnet compact by cold pressing of as-disproportionated NdFeB alloy powders. ► Nanocrystalline NdFeB magnets by desorption-recombination in-situ sintering under vacuum. ► Magnetic properties significantly improved by relative density enhancement and nanocrystallization of Nd 2 Fe 14 B phase. ► The effects of sintering parameters on magnetic properties and the underlying

  5. Nanocrystalline NdFeB magnet prepared by mechanically activated disproportionation and desorption-recombination in-situ sintering

    Energy Technology Data Exchange (ETDEWEB)

    Xiaoya, Liu; Yuping, Li [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China); Lianxi, Hu, E-mail: hulx@hit.edu.cn [School of Materials Science and Engineering, Harbin Institute of Technology, Harbin 150001 (China)

    2013-03-15

    The process of mechanically activated disproportionation and desorption-recombination in-situ sintering was proposed to synthesize highly densified nanocrystalline NdFeB magnet, and its validity was demonstrated by experimental investigation with the use of a Nd{sub 16}Fe{sub 76}B{sub 8} (atomic ratio) alloy. Firstly, the as-cast alloy was disproportionated by mechanical milling in hydrogen, with the starting micron-sized Nd{sub 2}Fe{sub 14}B phase decomposed into an intimate mixture of nano-structured NdH{sub 2.7}, Fe{sub 2}B and {alpha}-Fe phases. The as-disproportionated alloy powders were compacted by cold pressing and then subjected to desorption-recombination in-situ sintering. The microstructure of both the as-disproportionated and the subsequently sintered samples was characterized by X-ray diffraction and electron transmission microscopy, respectively. The magnetic properties of the sintered samples were measured by using vibrating sample magnetometer. The results showed that, by vacuum sintering, not only was the powder compact consolidated, but also the as-disproportionated microstucture transformed into nanocrystalline Nd{sub 2}Fe{sub 14}B phase via the well-known desorption-recombination reaction, thus giving rise to nanocrystalline NdFeB magnet. In the present study, the optimal sintering parameters were found to be 780 Degree-Sign C Multiplication-Sign 30 min. In this case, the coercivity, the remanence, and maximum energy product of the magnet sample achieved 0.8 T, 635.3 kA/m, and 106.3 kJ/m{sup 3}, respectively. - Highlights: Black-Right-Pointing-Pointer Nano-structured disproportionated NdFeB alloy powders by mechanical milling in hydrogen. Black-Right-Pointing-Pointer Highly densified green magnet compact by cold pressing of as-disproportionated NdFeB alloy powders. Black-Right-Pointing-Pointer Nanocrystalline NdFeB magnets by desorption-recombination in-situ sintering under vacuum. Black-Right-Pointing-Pointer Magnetic properties significantly

  6. In-Situ Chemical Oxidation

    Science.gov (United States)

    2006-08-01

    wells at a bioremediation field site (Weisner et al., 1996). Colloidal clay particles mobilized during injec- tion have resulted in permeability losses...phase material. Nevertheless, O3 was readily delivered and transported through unsaturated porous media where phenanthrene and diesel range...tion, but is not currently a well-developed technology. Bioremediation : Sequencing oxidation and reduction reactions may be achieved through

  7. Optimization of thorium oxalate precipitation conditions relative to thorium oxide sinterability

    International Nuclear Information System (INIS)

    White, G.D.; Bray, L.A.; Hart, P.E.

    1980-01-01

    The effect of thorium oxalate precipitation conditions on derived oxide sinterability was investigated with the objective of producing ThO 2 powder that could be sintered to high density without premilling. Precipitation conditions examined were temperature, digestion time and agitation method which were employed in a two-level factorial experimental design to delineate their effects. The two levels for each of the factors, respectively, were 10 0 C and 70 0 C, 15 min and 360 min, and mechanical stirrer and a homogenizer that imparted both mechanical and ultrasonic agitation. The ThO 2 derived from each of the precipitation trials was characterized with respect to morphology, surface area, and crystallite size as well as sinterability. Only precipitation temperature had a significant effect upon all the properties of the derived oxide powders

  8. Formation of peripheral porosity regions around urania in zirconia-urania mixed oxide powder compact sintering

    International Nuclear Information System (INIS)

    Das, P.; Choudhury, R.

    1992-01-01

    Sintering studies of zirconia-urania mixed oxide powder compacts (in stages of 5% urania up to a maximum of 20% addition) were carried out at temperatures between 1000-1400deg C for various soaking periods. The formation of a peripheral porosity region around comparatively coarser urania particle was a characteristic feature in this mixed oxide sintered compact. At even a higher sintering temperature (1800deg C), where extensive solid solution formation takes place, this porosity region demarcates the solutionized particles from the host zirconia apparently acting as a discontinuity in the system. Relative shrinkage difference between the dissimilar particles probably contributes to the porosity regions around the minor second phase at a lower temperature while at higher temperature generation of 'Kirkendall porosity' may be responsible for such an effect. (orig.)

  9. Preparation of a sinterable beryllium oxide through decomposition of beryllium hydroxide (1963)

    International Nuclear Information System (INIS)

    Bernier, M.

    1963-01-01

    In the course of the present study, we have attempted to precise the factors which among the ones effective in the course of the preparation of the beryllium hydroxide and oxide and during the sintering have an influence on the final result: the density and homogeneity of the sintered body. Of the several varieties of hydroxides precipitated from a sulfate solution the β-hydroxide only is always contaminated with beryllium sulfate and cannot be purified even by thorough washing. We noticed that those varieties of the hydroxide (gel, α, β) have different decomposition rates; this behaviour is used to identify and even to dose the different species in (α, β) mixtures. The various hydroxides transmit to the resulting oxides the shape they had when precipitated. Accordingly the history of the oxide is revealed by its behaviour during its fabrication and sintering. By comparing the results of the sintering operation with the various measurements performed on the oxide powders we are led to the conclusion that an oxide obtained from beryllium hydroxide is sinterable under vacuum if the following conditions are fulfilled: the particle size must lie between 0.1 and 0.2 μ and the BeSO 4 content of the powder must be less than 0.25 per cent wt (expressed as SO 3 /BeO). The best fitting is obtained with the oxide issued from an α-hydroxide precipitated as very small aggregates and with a low sulfur-content. We have observed that this is also the case for the oxide obtained by direct calcination of beryllium sulfate. (author) [fr

  10. Laser sintering of magnesia with nanoparticles of iron oxide and aluminum oxide

    Energy Technology Data Exchange (ETDEWEB)

    García, L.V.; Mendivil, M.I.; Roy, T.K. Das; Castillo, G.A. [Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Pedro de Alba s/n, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66451 (Mexico); Shaji, S., E-mail: sshajis@yahoo.com [Facultad de Ingenieria Mecanica y Electrica, Universidad Autonoma de Nuevo Leon, Av. Pedro de Alba s/n, Cd. Universitaria, San Nicolas de los Garza, Nuevo Leon 66451 (Mexico); CIIDIT, Universidad Autonoma de Nuevo Leon, Apodaca, Nuevo Leon (Mexico)

    2015-05-01

    Highlights: • Laser sintered MgO pellets with nanoparticles of Al{sub 2}O{sub 3} and Fe{sub 2}O{sub 3}. • Characterized these pellets by XRD, SEM and XPS. • Spinel formations were observed in both cases. • Changes in morphology and structure were analyzed. - Abstract: Nanoparticles of iron oxide (Fe{sub 2}O{sub 3}, 20–40 nm) and aluminum oxide (Al{sub 2}O{sub 3}, 50 nm) were mixed in different concentrations (3, 5 and 7 wt%) in a magnesium oxide (MgO) matrix. The mixture pellet was irradiated with 532 nm output from a Q-switched Nd:YAG laser using different laser fluence and translation speed for sintering. The refractory samples obtained were analyzed using X-ray diffraction technique, scanning electron microscopy and X-ray photoelectron spectroscopy. The results showed that the samples irradiated at translation speed of 110 μm/s and energy fluence of 1.7 J/cm{sup 2} with a concentration of 5 and 7 wt% of Fe{sub 2}O{sub 3} presented the MgFe{sub 2}O{sub 4} spinel-type phase. With the addition of Al{sub 2}O{sub 3} nanoparticles, at a translation speed of 110 μm/s and energy fluence of 1.7 J/cm{sup 2}, there were the formations of MgAl{sub 2}O{sub 4} spinel phase. The changes in morphologies and microstructure due to laser irradiation were analyzed.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2018-02-02

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

  12. Effect of High Speed Sintering on the Properties of Zirconia Oxide Materials

    Science.gov (United States)

    2018-03-22

    12. REPORT TYPE 22/03/2018 Poster 4. TITLE AND SUBTITLE Effect of High-Speed Sintering on the Properties ofZirconia-Oxide Materials 6. AUTHOR(S...2018-03/24/2018 Sa. CONTRACT NUMBER Sb. GRANT NUMBER Sc. PROGRAM ELEMENT NUMBER Sd. PROJECT NUMBER Se. TASK NUMBER Sf. WORK UNIT NUMBER 8

  13. Metallographic preparation of sintered oxides, carbides and nitrides of uranium and plutonium

    International Nuclear Information System (INIS)

    Martin, A.; Arles, L.

    1967-12-01

    We describe the methods of polishing, attack and coloring used at the section of plutonium base ceramics studies. These methods have stood the test of experience on the uranium and plutonium carbides, nitrides and carbonitrides as well on the mixed uranium and plutonium oxides. These methods have been particularly adapted to fit to the low dense and sintered samples [fr

  14. Evaluation of thermal properties of sintered beryllium oxide produced from Indian beryl ore

    International Nuclear Information System (INIS)

    Nair, Sathi R.; Ghanwat, S.J.; Patro, P.K.; Syambabu, M.; Mawal, N.E.; Mahata, T.; Sinha, P.K.

    2014-01-01

    Beryllium oxide (BeO) ceramics possess many interesting properties such as good thermal conductivity, high electrical resistivity, high chemical and thermal stability, low dielectric constant, low dielectric loss and low neutron absorption coefficient. These properties lead to its wide use in vacuum electronics technology, nuclear technology, microelectronics and photoelectron technology. The above properties depend on the purity of the material as well as density and microstructure of the sintered body. For high temperature application thermal conductivity and thermal expansion are two important parameters. In the present study, high purity fine BeO powder has been prepared by beryllate route starting with crude beryllium hydroxide. The powder has been sintered at 1550℃ and sintered samples have been evaluated for its thermal properties

  15. Spark Plasma Sintering and Densification Mechanisms of Antimony-Doped Tin Oxide Nanoceramics

    Directory of Open Access Journals (Sweden)

    Junyan Wu

    2013-01-01

    Full Text Available Densification of antimony-doped tin oxide (ATO ceramics without sintering aids is very difficult, due to the volatilization of SnO2, formation of deleterious phases above 1000°C, and poor sintering ability of ATO particles. In this paper, monodispersed ATO nanoparticles were synthesized via sol-gel method, and then ATO nanoceramics with high density were prepared by spark plasma sintering (SPS technology using the as-synthesized ATO nanoparticles without the addition of sintering aids. The effect of Sb doping content on the densification was investigated, and the densification mechanisms were explored. The results suggest that ATO nanoparticles derived from sol-gel method show good crystallinity with a crystal size of 5–20 nm and Sb is incorporated into the SnO2 crystal structure. When the SPS sintering temperature is 1000°C and the Sb doping content is 5 at.%, the density of ATO nanoceramics reaches a maximum value of 99.2%. Densification mechanisms are explored in detail.

  16. In situ transmission electron microscopy and scanning transmission electron microscopy studies of sintering of Ag and Pt nanoparticles

    International Nuclear Information System (INIS)

    Asoro, M.A.; Ferreira, P.J.; Kovar, D.

    2014-01-01

    Transmission electron microscopy and scanning transmission electron microscopy studies were conducted in situ on 2–5 nm Pt and 10–40 nm Ag nanoparticles to study mechanisms for sintering and to measure relevant sintering kinetics in nanoscale particles. Sintering between two separated particles was observed to initiate by either (1) diffusion of the particles on the sample support or (2) diffusion of atoms or small clusters of atoms to the neck region between the two particles. After particle contact, the rate of sintering was controlled by atomic surface diffusivity. The surface diffusivity was determined as a function of particle size and temperature from experimental measurements of the rate of neck growth of the particles. The surface diffusivities did not show a strong size effect for the range of particle sizes that were studied. The surface diffusivity for Pt nanoparticles exhibited the expected Arrhenius temperature dependence and did not appear to be sensitive to the presence of surface contaminants. In contrast, the surface diffusivity for Ag nanoparticles was affected by the presence of impurities such as carbon. The diffusivities for Ag nanoparticles were consistent with previous measurements of bulk surface diffusivities for Ag in the presence of C, but were significantly slower than those obtained from pristine Ag

  17. Process for obtaining sintered conglomerates with a high density of rare earth oxides and actinides

    International Nuclear Information System (INIS)

    Pasto, A.E.

    1974-01-01

    The invention concerns a method to produce agglomerates of actinide and rare earth oxides possessing a cubic-monoclinic transformation in order to obtain high densities close to the theoretical density, and the articles produced by the method. The process is based on the use of a rare earth or actinide oxide, in particular Eu 2 O 3 , with a cubic-monoclinic phase transformation, the oxide being sintered by hot compression at a temperature 50 deg C to 100 deg C above the transformation temperature. The sintered agglomerates obtained can have a purity of at least 99.9% and a density of practically 100%. These agglomerates are suitable in particular for the formation of nuclear reactor control rods [fr

  18. Chemically produced nanostructured ODS-lanthanum oxide-tungsten composites sintered by spark plasma

    International Nuclear Information System (INIS)

    Yar, Mazher Ahmed; Wahlberg, Sverker; Bergqvist, Hans; Salem, Hanadi G.; Johnsson, Mats; Muhammed, Mamoun

    2011-01-01

    High purity W and W-0.9La 2 O 3 (wt.%) nanopowders were produced by a wet chemical route. The precursor was prepared by the reaction of ammonium paratungstate (APT) with lanthanum salt in aqueous solutions. High resolution electron microscopy investigations revealed that the tungstate particles were coated with oxide precipitates. The precursor powder was reduced to tungsten metal with dispersed lanthanum oxide. Powders were consolidated by spark plasma sintering (SPS) at 1300 and 1400 o C to suppress grain growth during sintering. The final grain size relates to the SPS conditions, i.e. temperature and heating rate, regardless of the starting powder particle size. Scanning electron microscopy revealed that oxide phases were mainly accumulated at grain boundaries while the tungsten matrix constituted of nanosized sub-grains. The transmission electron microscopy revealed that the tungsten grains consist of micron-scale grains and finer sub-grains. EDX analysis confirmed the presence of W in dispersed oxide phases with varying chemical composition, which evidenced the presence of complex oxide phases (W-O-La) in the sintered metals.

  19. Spark plasma sintering of tungsten-yttrium oxide composites from chemically synthesized nanopowders and microstructural characterization

    International Nuclear Information System (INIS)

    Yar, M.A.; Wahlberg, Sverker; Bergqvist, Hans; Salem, H.G.; Johnsson, Mats; Muhammed, Mamoun

    2011-01-01

    Nano-crystalline W-1%Y 2 O 3 (wt.%) powder was produced by a modified solution chemical reaction of ammonium paratungstate (APT) and yttrium nitrate. The precursor powder was found to consist of particles of bimodal morphology i.e. large APT-like particles up to 20 μm and rectangular yttrium containing ultrafine plates. After thermal processing tungsten crystals were evolved from W-O-Y plate like particles. spark plasma sintering (SPS) was used to consolidate the powder at 1100 and 1200 deg. C for different holding times in order to optimize the sintering conditions to yield high density but with reduced grain growth. Dispersion of yttrium oxide enhanced the sinterability of W powder with respect to lanthanum oxide. W-1%Y 2 O 3 composites with sub-micron grain size showed improved density and mechanical properties as compared to W-La 2 O 3 composites. Sample sintered in two steps showed improved density, due to longer holding time at lower temperature (900 deg. C) and less grain growth due to shorter holding time at higher temperature i.e. 1 min at 1100 deg. C.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2005-07-01

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

  1. Process Developed for Generating Ceramic Interconnects With Low Sintering Temperatures for Solid Oxide Fuel Cells

    Science.gov (United States)

    Zhong, Zhi-Min; Goldsby, Jon C.

    2005-01-01

    Solid oxide fuel cells (SOFCs) have been considered as premium future power generation devices because they have demonstrated high energy-conversion efficiency, high power density, and extremely low pollution, and have the flexibility of using hydrocarbon fuel. The Solid-State Energy Conversion Alliance (SECA) initiative, supported by the U.S. Department of Energy and private industries, is leading the development and commercialization of SOFCs for low-cost stationary and automotive markets. The targeted power density for the initiative is rather low, so that the SECA SOFC can be operated at a relatively low temperature (approx. 700 C) and inexpensive metallic interconnects can be utilized in the SOFC stack. As only NASA can, the agency is investigating SOFCs for aerospace applications. Considerable high power density is required for the applications. As a result, the NASA SOFC will be operated at a high temperature (approx. 900 C) and ceramic interconnects will be employed. Lanthanum chromite-based materials have emerged as a leading candidate for the ceramic interconnects. The interconnects are expected to co-sinter with zirconia electrolyte to mitigate the interface electric resistance and to simplify the processing procedure. Lanthanum chromites made by the traditional method are sintered at 1500 C or above. They react with zirconia electrolytes (which typically sinter between 1300 and 1400 C) at the sintering temperature of lanthanum chromites. It has been envisioned that lanthanum chromites with lower sintering temperatures can be co-fired with zirconia electrolyte. Nonstoichiometric lanthanum chromites can be sintered at lower temperatures, but they are unstable and react with zirconia electrolyte during co-sintering. NASA Glenn Research Center s Ceramics Branch investigated a glycine nitrate process to generate fine powder of the lanthanum-chromite-based materials. By simultaneously doping calcium on the lanthanum site, and cobalt and aluminum on the

  2. The age and significance of in-situ sinter at the Te Kopia thermal area, Taupo Volcanic Zone, New Zealand

    Energy Technology Data Exchange (ETDEWEB)

    Martin, Rod; Rodgers, Kerry A. [Auckland Univ., Dept. of Geology, Auckland (New Zealand); Mildenhall, Dallas C. [Institute of Geological and Nuclear Sciences, Lower Hutt (New Zealand); Browne, Patrick R.L. [Auckland Univ., Dept. of Geology, Auckland (New Zealand); Auckland Univ., Geothermal Inst., Auckland (New Zealand)

    2000-06-01

    One hundred pollen grains and spores, recovered from a single sample of in situ silica sinter from the Te Kopia geothermal field, include some from a podocarp forest that grew in a temperate, frost-free climate, unlike that of today, as indicated by the presence of Ascarina. Also present are pollen from taxa introduced within the last 100 years. Ascarina has been absent from the area since at least 1800 B.P. and its presence in the sinter indicates that alkali chloride waters discharged at the surface of Te Kopia before 1800 B.P., and possibly before 3500 B.P. Although palynology is a powerful tool to place age limits on fluctuations in the shallow hydrology of geothermal fields, interpretation must be moderated by considering the present flora and also changes in both local and regional flora, habitat and climate. (Author)

  3. Electrical sintering of silver nanoparticle ink studied by in-situ TEM probing.

    Directory of Open Access Journals (Sweden)

    Magnus Hummelgård

    Full Text Available Metallic nanoparticle inks are used for printed electronics, but to reach acceptable conductivity the structures need to be sintered, usually using a furnace. Recently, sintering by direct resistive heating has been demonstrated. For a microscopic understanding of this Joule heating sintering method, we studied the entire process in real time inside a transmission electron microscope equipped with a movable electrical probe. We found an onset of Joule heating induced sintering and coalescence of nanoparticles at power levels of 0.1-10 mW/μm³. In addition, a carbonization of the organic shells that stabilize the nanoparticles were found, with a conductivity of 4 10⁵ Sm⁻¹.

  4. Standard test methods for analysis of sintered gadolinium oxide-uranium dioxide pellets

    CERN Document Server

    American Society for Testing and Materials. Philadelphia

    2006-01-01

    1.1 These test methods cover procedures for the analysis of sintered gadolinium oxide-uranium dioxide pellets to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Section Carbon (Total) by Direct CombustionThermal Conductivity Method C1408 Test Method for Carbon (Total) in Uranium Oxide Powders and Pellets By Direct Combustion-Infrared Detection Method Chlorine and Fluorine by Pyrohydrolysis Ion-Selective Electrode Method C1502 Test Method for Determination of Total Chlorine and Fluorine in Uranium Dioxide and Gadolinium Oxide Gadolinia Content by Energy-Dispersive X-Ray Spectrometry C1456 Test Method for Determination of Uranium or Gadolinium, or Both, in Gadolinium Oxide-Uranium Oxide Pellets or by X-Ray Fluorescence (XRF) Hydrogen by Inert Gas Fusion C1457 Test Method for Determination of Total Hydrogen Content of Uranium Oxide Powders and Pellets by Carrier Gas Extraction Isotopic Uranium Composition by Multiple-Filament Surface-Ioni...

  5. Sintering uranium oxide in the reaction product of hydrogen-carbon dioxide mixtures

    International Nuclear Information System (INIS)

    De Hollander, W.R.; Nivas, Y.

    1975-01-01

    Compacted pellets of uranium oxide alone or containing one or more additives such as plutonium dioxide, gadolinium oxide, titanium dioxide, silica, and alumina are heated to 900 to 1599 0 C in the presence of a mixture of hydrogen and carbon dioxide, either alone or with an inert carrier gas and held at the desired temperature in this atmosphere to sinter the pellets. The sintered pellets are then cooled in an atmosphere having an oxygen partial pressure of 10 -4 to 10 -18 atm of oxygen such as dry hydrogen, wet hydrogen, dry carbon monoxide, wet carbon monoxide, inert gases such as nitrogen, argon, helium, and neon and mixtures of ayny of the foregoing including a mixture of hydrogen and carbon dioxide. The ratio of hydrogen to carbon dioxide in the gas mixture fed to the furnace is controlled to give a ratio of oxygen to uranium atoms in the sintered particles within the range of 1.98:1 to about 2.10:1. The water vapor present in the reaction products in the furnace atmosphere acts as a hydrolysis agent to aid removal of fluoride should such impurity be present in the uranium oxide. (U.S.)

  6. Hot-pressed silicon nitride with various lanthanide oxides as sintering additives

    Science.gov (United States)

    Ueno, K.; Toibana, Y.

    1984-01-01

    The effects of addition of various lanthanide oxides and their mixture with Y2O3 on the sintering of Si3N4 were investigated. The addition of simple and mixed lanthanide oxides promoted the densification of Si3N4 in hot-pressing at 1800 C under 300-400kg/ centimeters squared for 60 min. The crystallization of yttrium and lanthanide-silicon oxynitrides which was observed inn the sintered body containing yttrium-lanthanide mixed oxides as additives led to the formation of a highly refractory Si3N4 ceramic having a bending strength of 82 and 84 kg/millimeters squared at room temperature and 1300 C respectively. In a Y2O3+La2O3 system, a higher molar ratio of La2O3 to Y2O3 gave a higher hardness and strength at high temperatures. It was found that 90 min was an optimum sintering time for the highest strength.

  7. In situ oxide dispersion strengthened tungsten alloys with high compressive strength and high strain-to-failure

    International Nuclear Information System (INIS)

    Huang, Lin; Jiang, Lin; Topping, Troy D.; Dai, Chen; Wang, Xin; Carpenter, Ryan; Haines, Christopher; Schoenung, Julie M.

    2017-01-01

    In this work a novel process methodology to concurrently improve the compressive strength (2078 MPa at a strain rate of 5 × 10"−"4 s"−"1) and strain-to-failure (over 40%) of bulk tungsten materials has been described. The process involves the in situ formation of intragranular tungsten oxide nanoparticles, facilitated by the application of a pressure of 1 GPa at a low sintering temperature of 1200 °C during spark plasma sintering (SPS). The results show that the application of a high pressure of 1 GPa during SPS significantly accelerates the densification process. Concurrently, the second phase oxide nanoparticles with an average grain size of 108 nm, which are distributed within the interiors of the W grains, simultaneously provide strengthening and plasticity by inhibiting grain growth, and generating, blocking, and storing dislocations. - Graphical abstract: In this work a novel process methodology to concurrently improve the compressive strength (2078 MPa at a strain rate of 5 × 10"−"4 s"−"1) and strain-to-failure (over 40%) of bulk W materials has been described. The process involves the in situ formation of intragranular tungsten oxide nanoparticles, facilitated by the application of a pressure of 1 GPa at a low sintering temperature of 1200 °C during spark plasma sintering (SPS).

  8. Mechanical properties of thermoelectric n-type magnesium silicide synthesized employing in situ spark plasma reaction sintering

    Science.gov (United States)

    Muthiah, Saravanan; Singh, R. C.; Pathak, B. D.; Dhar, Ajay

    2017-07-01

    Thermoelectric devices employing magnesium silicide (Mg2Si) offer an inexpensive and non-toxic solution for green energy generation compared to other existing conventional thermoelectric materials in the mid-temperature range. However, apart from the thermoelectric performance, their mechanical properties are equally important in order to avoid the catastrophic failure of their modules during actual operation. In the present study, we report the synthesis of Mg2Si co-doped with Bi and Sb employing in situ spark plasma reaction sintering and investigate its broad range of mechanical properties. The mechanical properties of the sintered co-doped Mg2Si suggest a significantly enhanced value of hardness ~5.4  ±  0.2 GPa and an elastic modulus ~142.5  ±  6 GPa with a fracture toughness of ~1.71  ±  0.1 MPa  √m. The thermal shock resistance, which is one of the most vital parameter for designing thermoelectric devices, was found to be ~300 W m-1, which is higher than most of the other existing state-of-the-art mid-temperature thermoelectric materials. The friction and wear characteristics of sintered co-doped Mg2Si have been reported for the first time, in order to realize the sustainability of their thermoelectric modules under actual hostile environmental conditions.

  9. In situ evaluation of supersolidus liquid phase sintering phenomena of stainless steel 316L: Densification and distortion

    Science.gov (United States)

    Bollina, Ravi

    Supersolidus liquid phase sintering (SLPS) is a variant of liquid phase sintering. In SLPS, prealloyed powders are heated between the solidus and liquidus temperature of the alloy. This thesis focuses on processing of stainless steel 316L via SLPS by adding boron. Various amounts of boron were added to study the effect of boron on densification and distortion. The sintering window for water atomized 316L with 0.2% boron ranges from 1430 to 1435°C and 1225 to 1245°C for water atomized 316L with 0.8% boron. The rate of change of liquid content with temperature dVL/dt decreases from 1.5%/°C to 0.1%/°C for in increase in boron content from 0 to 0.8%, giving a wider range and better control during sintering. Further; effect of boron on mechanical properties and corrosion properties was researched. It was possible to achieve tensile strength of 476+/-21 MPa and an yield strength of 250+/-5 MPa with an elongation of 15+/-2 % in water atomized 316L with 0.8% boron. Fracture analysis indicates the presence of a brittle boride phase along the grain boundary causing intergranular fracture resulting in poor ductility. The crux of this thesis discusses the evolution of apparent viscosity and its relation to the microstructure. Beam bending viscometry was successfully used to evaluate the in situ apparent viscosity evolution of water atomized 316L with 0.2 and 0.8% boron additions. The apparent viscosity drops from 174 GPa.s at 1200°C to 4 GPa.s at 1275°C with increasing fractional liquid coverage in the water atomized 316L with 0.8% boron. The apparent viscosity calculated from bending beam and was used as an input into a finite element model (FEM) derived from constitutive equations and gives an excellent, fit between simulation and experiment. The densification behavior of boron doped stainless steel was modelled using Master Sintering Curve (MSC) (based on work of sintering) for the first time. It is proven that MSC can be used to identify change in densification rate

  10. Sintering of beryllium oxide; Frittage de l'oxyde de beryllium

    Energy Technology Data Exchange (ETDEWEB)

    Caillat, R; Pointud, R [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1955-07-01

    This study had for origin to find a process permitting to manufacture bricks of beryllium oxide of pure nuclear grade, with a density as elevated as possible and with standardized shape. The sintering under load was the technique kept for the manufacture of the bricks. Because of the important toxicity of the beryllium oxide, the general features for the preliminary study of the sintering, have been determined while using alumina. The obtained results will be able to act as general indication for ulterior studies with sintering under load. (M.B.) [French] Cette etude a eu pour origine la recherche d'un procede permettant de fabriquer industriellement des briques d'oxyde de beryllium nucleaireraent pures, de densite aussi elevee que possible et de forme standardisee. Le frittage sous charge fut la technique retenue pour la fabrication des briques. En raison de la grande toxicite de l'oxyde de beryllium, les caracteristiques generales du frittage, pour l'etude preliminaire, ont ete determine en utilisant de l'alumine. Les resultats obtenus pourront servir d'indication generale pour des etudes ulterieurs avec frittage sous charge. (M.B.)

  11. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr4+ organic salts

    Science.gov (United States)

    Strini, Alberto; Sanson, Alessandra; Mercadelli, Elisa; Bendoni, Riccardo; Marelli, Marcello; Dal Santo, Vladimiro; Schiavi, Luca

    2015-08-01

    The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr4+ organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr4+ organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500-900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m-3) and low UV-A irradiance (180 μW cm-2). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation.

  12. Study and fabrication of solid oxide fuel cells through tape casting and co-sintering

    International Nuclear Information System (INIS)

    Grosjean, A.

    2004-11-01

    This work is dedicated to the devising of a low-cost fabrication process of solid oxide fuel cells (SOFC). Technical requirements impose the shaping method: stripe casting as well as the materials used: Yttria-stabilized zirconia (YSZ), nickel and lanthanum manganite doped with strontium (LSM). In order to comply with environmental requirements the developed process uses an aqueous barbotine solvent. We get electrodes and the electrolyte separately, the use of an absorbent drying process has enabled us to join 3 layers to form an elementary cell with great interfacial homogeneity. The resistance of the cell to sintering has been improved through the symmetrization of the deformations of the cell. In order to interpret the low electrical properties of the cell and its quick damaging, transmission microscopy studies have been performed. These studies have shown 2 facts. First, 2 isolating phases appear at the cathode (at the LSM/YSZ interface) because of a too high sintering temperature and secondly, a quick clustering of nickel grains appears during cell operation that leads to a local loss of the nickel grid percolation. This problem has been solved by increasing the size of nickel oxide grains from 0.5 μm to 3 μm) to stabilize the microstructure. The issue of the reactivity at the LSM/YSZ interfaces was tackled in 2 different ways, we have tried to lower the sintering temperature by using a zirconia nano-powder first and then by replacing zirconia in the electrolyte by gadolinium-doped ceria. The use of zirconia nano-powder has failed to decrease sintering temperature while preserving the electrolyte density and the use of ceria has triggered instabilities that have not yet been solved. Despite all these drawbacks, this process allows the fabrication of an excellent anode/electrolyte interface. (A.C.)

  13. Immobilization of Radioactive Rare Earth oxide Waste by Solid Phase Sintering

    International Nuclear Information System (INIS)

    Ahn, Byung Gil; Park, Hwan Seo; Kim, Hwan Young; Lee, Han Soo; Kim, In Tae

    2010-01-01

    In the pyroprocessing of spent nuclear fuels, LiCl-KCl waste salt containing radioactive rare earth chlorides are generated. The radioactive rare earth oxides are recovered by co-oxidative precipitation of rare earth elements. The powder phase of rare earth oxide waste must be immobilized to produce a monolithic wasteform suitable for storage and ultimate disposal. The immobilization of these waste developed in this study involves a solid state sintering of the waste with host borosilicate glass and zinc titanate based ceramic matrix (ZIT). And the rare-earth monazite which synthesised by reaction of ammonium di-hydrogen phosphate with the rare earth oxides waste, were immobilized with the borosilicate glass. It is shown that the developed ZIT ceramic wasteform is highly resistant the leaching process, high density and thermal conductivity.

  14. Improved reaction sintered silicon nitride. [protective coatings to improve oxidation resistance

    Science.gov (United States)

    Baumgartner, H. R.

    1978-01-01

    Processing treatments were applied to as-nitrided reaction sintered silicon nitride (RSSN) with the purposes of improving strength after processing to above 350 MN/m2 and improving strength after oxidation exposure. The experimental approaches are divided into three broad classifications: sintering of surface-applied powders; impregnation of solution followed by further thermal processing; and infiltration of molten silicon and subsequent carburization or nitridation of the silicon. The impregnation of RSSN with solutions of aluminum nitrate and zirconyl chloride, followed by heating at 1400-1500 C in a nitrogen atmosphere containing silicon monoxide, improved RSSN strength and oxidation resistance. The room temperature bend strength of RSSN was increased nearly fifty percent above the untreated strength with mean absolute strengths up to 420 MN/m2. Strengths of treated samples that were measured after a 12 hour oxidation exposure in air were up to 90 percent of the original as-nitrided strength, as compared to retained strengths in the range of 35 to 60 percent for untreated RSSN after the same oxidation exposure.

  15. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr{sup 4+} organic salts

    Energy Technology Data Exchange (ETDEWEB)

    Strini, Alberto, E-mail: alberto.strini@itc.cnr.it [Istituto per le Tecnologie della Costruzione (ITC-CNR), via Lombardia, 49, I-20098 San Giuliano Milanese (MI) (Italy); Sanson, Alessandra; Mercadelli, Elisa [Istituto di Scienza e Tecnologia dei Materiali Ceramici (ISTEC-CNR), via Granarolo, 64, I-48018 Faenza (RA) (Italy); Bendoni, Riccardo [Istituto di Scienza e Tecnologia dei Materiali Ceramici (ISTEC-CNR), via Granarolo, 64, I-48018 Faenza (RA) (Italy); Dipartimento di Scienze e Tecnologie Chimiche e Centro NAST - Università di Roma Tor Vergata, via della Ricerca Scientifica, I-00133 Roma (Italy); Marelli, Marcello; Dal Santo, Vladimiro [CNR–Istituto di Scienze e Tecnologie Molecolari, via Golgi, 19, I-20133 Milano (Italy); Schiavi, Luca [Istituto per le Tecnologie della Costruzione (ITC-CNR), via Lombardia, 49, I-20098 San Giuliano Milanese (MI) (Italy)

    2015-08-30

    Graphical abstract: - Highlights: • Existing commercial (P25) anatase was stabilized in-situ with Zr(IV) doping. • Highly active catalytic layers were obtained by screen-printing. • Increased thermal stability was demonstrated up to 200 °C without activity loss. • Enhanced activity was obtained because of the Zr(IV) doping. • Zirconium diffusion was assessed by STEM-EDS analysis. - Abstract: The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr{sup 4+} organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr{sup 4+} organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500–900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m{sup −3}) and low UV-A irradiance (180 μW cm{sup −2}). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation.

  16. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr4+ organic salts

    International Nuclear Information System (INIS)

    Strini, Alberto; Sanson, Alessandra; Mercadelli, Elisa; Bendoni, Riccardo; Marelli, Marcello; Dal Santo, Vladimiro; Schiavi, Luca

    2015-01-01

    Graphical abstract: - Highlights: • Existing commercial (P25) anatase was stabilized in-situ with Zr(IV) doping. • Highly active catalytic layers were obtained by screen-printing. • Increased thermal stability was demonstrated up to 200 °C without activity loss. • Enhanced activity was obtained because of the Zr(IV) doping. • Zirconium diffusion was assessed by STEM-EDS analysis. - Abstract: The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr 4+ organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr 4+ organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500–900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m −3 ) and low UV-A irradiance (180 μW cm −2 ). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation

  17. Microwave assisted sintering of gadolinium doped barium cerate electrolyte for intermediate temperature solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Arumugam Senthil, E-mail: senthu.ramp@gmail.com [Department of Physics, PSG College of Technology, Coimbatore, 641 004, Tamilnadu (India); Balaji, Ramamoorthy [Department of Physics, PSG College of Technology, Coimbatore, 641 004, Tamilnadu (India); Jayakumar, Srinivasalu [Department of Physics, PSG Institute of Technology and Applied Research, Coimbatore, 641 062, Tamilnadu (India); Pradeep, Chandran [Department of Physics, Indian Institute of Technology, Madras, 600 036, Tamilnadu (India)

    2016-10-01

    In Solid Oxide Fuel Cell (SOFC), electrolyte plays a vital role to increase the energy conversion efficiency. The main hurdle of such electrolyte in fuel cell is its higher operating temperature (1000 °C) which results in design limitation and higher fabrication cost. In order to reduce the operating temperature of SOFC, a suitable electrolyte has been prepared through co-precipitation method followed by microwave sintering of solid ceramic. The calcination temperature for the as-prepared powder was identified using Differential Scanning Calorimetry. The crystal structure of the sample was found to exhibit its orthorhombic perovskite structure. The particle size was determined using High-Resolution Transmission Electron Microscope with uniform in shape and size, match with XRD results and confirmed from structural analysis. Thus, the sample prepared via co-precipitation method and the solid ceramic sintered through microwave can be a promising electrolyte for fuel cells operated at intermediate temperature. - Highlights: • To synthesis the composite electrolyte by chemical method and sinter using microwave. • To reduce the operating temperature of electrolyte for high ionic conductivity in SOFC's. • To study the phase purity and to develop nanocomposite at reduced temperature.

  18. Microstructures and mechanical properties of 9Cr oxide dispersion strengthened steel produced by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Rui [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); School of Metallurgy, Northeastern University, Shenyang 110819 (China); Lu, Zheng, E-mail: luz@atm.neu.edu.cn [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Lu, Chenyang; Li, Zhengyuan [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China); Ding, Xueyong [School of Metallurgy, Northeastern University, Shenyang 110819 (China); Liu, Chunming [Key Laboratory for Anisotropy and Texture of Materials (Ministry of Education), School of Materials Science and Engineering, Northeastern University, Shenyang 110819 (China)

    2017-02-15

    Highlights: • A 9Cr-ODS steel was produced by mechanical alloying and spark plasma sintering. • Bimodal grain size distribution was observed. • Formation mechanism of bimodal grain size distribution was discussed. • The size and number density of nanoscale particles were obtained by SAXS and HRTEM. • The contribution of nano-sized particles to yield strength is dominating. - Abstract: 9Cr oxide dispersion strengthened (ODS) steel was fabricated by mechanical alloying (MA) and spark plasma sintering (SPS). The nano-sized particles, grain size distribution and mechanical properties of 9Cr-ODS steel sintered at 950 °C were studied by synchrotron radiation small angle X-ray scattering (SAXS), high-resolution transmission electron microscopy (HRTEM), electron backscatter diffraction (EBSD) and tensile experiment. The results showed that bimodal grain size distribution in the matrix is observed, which is attributed to the heterogeneous recrystallization process during the SPS. High-density nano-sized Y{sub 2}Ti{sub 2}O{sub 7} and some large oxides of Cr{sub 2}Mn(Ti)O{sub 4} are formed in 9Cr-ODS steel. The number density and average size of Y{sub 2}Ti{sub 2}O{sub 7} obtained from SAXS are 4.72 × 10{sup 22}/m{sup 3} and 4.4 nm, respectively. The yield strengths of 9Cr-ODS steel fabricated by SPS are compared with the typical 9Cr-ODS steel produced by HIP.

  19. Guideline tests on the corrosion of sintered uranium oxide by lead and sodium about 450 deg. C

    International Nuclear Information System (INIS)

    Portnoff, A.; Pointud, R.

    1958-05-01

    Within the frame of the investigation of behaviour of a fuel element (such as UO 2 ) under irradiation, the authors report the study of the physical-chemical action of the coolant at different temperatures on the body to be irradiated. Thus, sintered uranium oxide has been submitted to corrosion by lead and by sodium during 250 hours at temperatures between 400 and 500 C. The physical characteristics of the UO 2 powder and of different sintered UO 2 pellets produced from this powder under different sintering processes are indicated, as well as the results of a spectrographic analysis of the sintered UO 2 . Corrosion devices, treatments and obtained results are reported for corrosion by lead and by sodium. In the latter case, extraction processes are discussed (using butyl alcohol, or melting in vaseline oil)

  20. Excimer laser sintering of indium tin oxide nanoparticles for fabricating thin films of variable thickness on flexible substrates

    International Nuclear Information System (INIS)

    Park, Taesoon; Kim, Dongsik

    2015-01-01

    Technology to fabricate electrically-conducting, transparent thin-film patterns on flexible substrates has possible applications in flexible electronics. In this work, a pulsed-laser sintering process applicable to indium tin oxide (ITO) thin-film fabrication on a substrate without thermal damage to the substrate was developed. A nanosecond pulsed laser was used to minimize thermal penetration into the substrate and to control the thickness of the sintered layer. ITO nanoparticles (NPs) of ~ 20 nm diameter were used to lower the process temperature by exploiting their low melting point. ITO thin film patterns were fabricated by first spin coating the NPs onto a surface, then sintering them using a KrF excimer laser. The sintered films were characterized using field emission scanning electron microscopy. The electrical resistivity and transparency of the film were measured by varying the process parameters. A single laser pulse could generate the polycrystalline structure (average grain size ~ 200 nm), reducing the electrical resistivity of the film by a factor of ~ 1000. The sintering process led to a minimum resistivity of 1.1 × 10 −4 Ω·m without losing the transparency of the film. The thickness of the sintered layer could be varied up to 150 nm by adjusting the laser fluence. Because the estimated thermal penetration depth in the ITO film was less than 200 nm, no thermal damage was observed in the substrate. This work suggests that the proposed process, combined with various particle deposition methods, can be an effective tool to form thin-film ITO patterns on flexible substrates. - Highlights: • Excimer laser sintering can fabricate ITO thin films on flexible substrates. • The laser pulse can form a polycrystalline structure without thermal damage. • The laser sintering process can reduce the electrical resistivity substantially. • The thickness of the sintered layer can be varied effectively

  1. Excimer laser sintering of indium tin oxide nanoparticles for fabricating thin films of variable thickness on flexible substrates

    Energy Technology Data Exchange (ETDEWEB)

    Park, Taesoon; Kim, Dongsik, E-mail: dskim87@postech.ac.kr

    2015-03-02

    Technology to fabricate electrically-conducting, transparent thin-film patterns on flexible substrates has possible applications in flexible electronics. In this work, a pulsed-laser sintering process applicable to indium tin oxide (ITO) thin-film fabrication on a substrate without thermal damage to the substrate was developed. A nanosecond pulsed laser was used to minimize thermal penetration into the substrate and to control the thickness of the sintered layer. ITO nanoparticles (NPs) of ~ 20 nm diameter were used to lower the process temperature by exploiting their low melting point. ITO thin film patterns were fabricated by first spin coating the NPs onto a surface, then sintering them using a KrF excimer laser. The sintered films were characterized using field emission scanning electron microscopy. The electrical resistivity and transparency of the film were measured by varying the process parameters. A single laser pulse could generate the polycrystalline structure (average grain size ~ 200 nm), reducing the electrical resistivity of the film by a factor of ~ 1000. The sintering process led to a minimum resistivity of 1.1 × 10{sup −4} Ω·m without losing the transparency of the film. The thickness of the sintered layer could be varied up to 150 nm by adjusting the laser fluence. Because the estimated thermal penetration depth in the ITO film was less than 200 nm, no thermal damage was observed in the substrate. This work suggests that the proposed process, combined with various particle deposition methods, can be an effective tool to form thin-film ITO patterns on flexible substrates. - Highlights: • Excimer laser sintering can fabricate ITO thin films on flexible substrates. • The laser pulse can form a polycrystalline structure without thermal damage. • The laser sintering process can reduce the electrical resistivity substantially. • The thickness of the sintered layer can be varied effectively.

  2. Thermoelectric Properties of Hot-Pressed and PECS-Sintered Magnesium-Doped Copper Aluminum Oxide

    Science.gov (United States)

    Liu, Chang; Morelli, Donald T.

    2011-05-01

    Copper aluminum oxide (CuAlO2) is considered as a potential candidate for thermoelectric applications. Partially magnesium-doped CuAlO2 bulk pellets were fabricated using solid-state reactions, hot-pressing, and pulsed electric current sintering (PECS) techniques. X-ray diffraction and scanning electron microscopy were adopted for structural analysis. High-temperature transport property measurements were performed on hot-pressed samples. Electrical conductivity increased with Mg doping before secondary phases became significant, while the Seebeck coefficient displayed the opposite trend. Thermal conductivity was consistently reduced as the Mg concentration increased. Effects of Mg doping, preparation conditions, and future modification on this material's properties are discussed.

  3. Coupling in-situ X-ray micro- and nano-tomography and discrete element method for investigating high temperature sintering of metal and ceramic powders

    Directory of Open Access Journals (Sweden)

    Yan Zilin

    2017-01-01

    Full Text Available The behaviour of various powder systems during high temperature sintering has been investigated by coupling X-ray microtomography and discrete element method (DEM. Both methods are particularly relevant to analyse particle interactions and porosity changes occurring during sintering. Two examples are presented. The first one deals with a copper powder including artificially created pores which sintering has been observed in situ at the European synchrotron and simulated by DEM. 3D images with a resolution of 1.5 μm have been taken at various times of the sintering cycle. The comparison of the real displacement of particle centers with the displacement derived from the mean field assumption demonstrates significant particle rearrangement in some regions of the sample. Although DEM simulation showed less rearrangement, it has been able to accurately predict the densification kinetics. The second example concerns multilayer ceramic capacitors (MLCCs composed of hundreds of alternated metal electrode and ceramic dielectric layers. The observation of Ni-based MLCCs by synchrotron nanotomography at Argon National Laboratory with a spatial resolution between 10 and 50 nm allowed understanding the origin of heterogeneities formed in Ni layers during sintering. DEM simulations confirmed this analysis and provided clues for reducing these defects.

  4. IN-SITU FENTON OXIDATION: A CRITICAL ANALYSIS

    Science.gov (United States)

    In-situ Fenton oxidation (ISFO) is a rapidly emerging technology which involves the injection of hydrogen peroxide (H2O2) and other chemical reagents into the subsurface for the purpose of oxidizing and transforming contaminants. ISFO is being applied at an increasing number of ...

  5. Discussion on Microwave-Matter Interaction Mechanisms by In Situ Observation of "Core-Shell" Microstructure during Microwave Sintering.

    Science.gov (United States)

    Liu, Wenchao; Xu, Feng; Li, Yongcun; Hu, Xiaofang; Dong, Bo; Xiao, Yu

    2016-02-23

    This research aims to deepen the understanding of the interaction mechanisms between microwave and matter in a metal-ceramic system based on in situ synchrotron radiation computed tomography. A special internal "core-shell" microstructure was discovered for the first time and used as an indicator for the interaction mechanisms between microwave and matter. Firstly, it was proved that the microwave magnetic field acted on metal particles by way of inducing an eddy current in the surface of the metal particles, which led to the formation of a "core-shell" microstructure in the metal particles. On this basis, it was proposed that the ceramic particles could change the microwave field and open a way for the microwave, thereby leading to selective heating in the region around the ceramic particles, which was verified by the fact that all the "core-shell" microstructure was located around ceramic particles. Furthermore, it was indicated that the ceramic particles would gather the microwaves, and might lead to local heating in the metal-ceramic contact region. The focusing of the microwave was proved by the quantitative analysis of the evolution rate of the "core-shell" microstructure in a different region. This study will help to reveal the microwave-matter interaction mechanisms during microwave sintering.

  6. An easily sintered, chemically stable, barium zirconate-based proton conductor for high-performance proton-conducting solid oxide fuel cells

    KAUST Repository

    Sun, Wenping; Shi, Zhen; Liu, Mingfei; Bi, Lei; Liu, Wei

    2014-01-01

    Yttrium and indium co-doped barium zirconate is investigated to develop a chemically stable and sintering active proton conductor for solid oxide fuel cells (SOFCs). BaZr0.8Y0.2-xInxO3- δ possesses a pure cubic perovskite structure. The sintering

  7. Sintering effect on material properties of electrochemical reactors used for removal of nitrogen oxides and soot particles emitted from diesel engines

    DEFF Research Database (Denmark)

    He, Zeming; Andersen, Kjeld Bøhm; Keel, Li

    2010-01-01

    In the present work, 12-layered electrochemical reactors (comprising five cells) with a novel configuration including supporting layer lanthanum strontium manganate (LSM)-yttria stabilised zirconia (YSZ), electrode layer LSM-gadolinia-doped cerium oxide (CGO) and electrolyte layer CGO were...... fabricated via the processes of slurry preparation, tape casting and lamination and sintering. The parameters of porosity, pore size, pore size distribution, shrinkage, flow rate of the sintered reactors and the electrical conductivities of the supporting layer and the electrode in the sintered reactors were...... characterised. The effect of sintering temperature on microstructures and properties of the sintered samples was discussed, and 1,250 °C was determined as the appropriate sintering temperature for reactor production based on the performance requirements for applications. Using the present ceramic processing...

  8. In situ observation techniques of protective oxide layer

    International Nuclear Information System (INIS)

    Doi, Takashi; Adachi, Takeharu; Usuki, Noriaki

    2015-01-01

    In situ analyzing techniques for investigating a surface and interface change during corrosion and oxidation of metals by using Raman scattering spectroscopy (Raman), X-ray diffraction (XRD) and X-ray photoemission spectroscopy (XPS) are present. The Raman spectra revealed that a crystal structure and distribution of corrosion products varied during corrosion progress at elevated temperature and high pressure electrolyte. Time dependent XRD measurements made clear the behavior of the electrochemical reduction of a rust and the iso thermal transformation of a scale on a steel. It was demonstrated that XPS was capable of the in-situ measurements for initial stage of high temperature oxidation. (author)

  9. Phenomenological model of sintering of oxide nuclear fuel with doping admixtures

    Science.gov (United States)

    Baranov, V. G.; Devyatko, Yu. N.; Tenishev, A. V.; Khomyakov, O. V.

    2015-12-01

    It is shown that a change in the linear dimension of compacted UO2 in the sintering process is associated with its plastic yielding under the action of the forces of residual stress and capillary forces. From the curves of sintering of a fuel with doping admixtures in various gaseous media, its rate of creep is reduced.

  10. Assessment of consolidation of oxide dispersion strengthened ferritic steels by spark plasma sintering: from laboratory scale to industrial products

    International Nuclear Information System (INIS)

    Boulnat, X.; Fabregue, D.; Perez, M.; Urvoy, S.; Hamon, D.; Carlan, Y. de

    2014-01-01

    Oxide dispersion strengthened steels are new generation alloys that are usually processed by hot isostatic pressing (HIP). In this study, spark plasma sintering (SPS) was studied as an alternative consolidation technique. The influence of the processing parameters on the microstructure was quantified. The homogeneity of the SPSed materials was characterised by electron microprobe and microhardness. A combination of limited grain growth and minimised porosity can be achieved on semi-industrial compact. Excellent tensile properties were obtained compared to the literature. (authors)

  11. Densification of LSGM electrolytes using activated microwave sintering

    Science.gov (United States)

    Kesapragada, S. V.; Bhaduri, S. B.; Bhaduri, S.; Singh, P.

    Lanthanum gallate doped with alkaline rare earths (LSGM) powders were densified using an activated microwave sintering process for developing a dense stable electrolyte layer for applications in intermediate temperature-solid oxide fuel cells (IT-SOFCs). Due to heat generation in situ, the process of sintering gets activated with faster kinetics compared to a conventional sintering process. The effect of various microwave process parameters on the microstructure and phase formation was studied. The sintered pellets were characterized using scanning electron microscopy-energy dispersive analysis (SEM-EDAX), and X-ray diffraction (XRD). The density of LSGM pellets microwave sintered at 1350 °C for 20 min is greater than 95% theoretical density with a fine grained microstructure (˜2-3 μm) and without the presence of other phase(s).

  12. Improved Understanding of In Situ Chemical Oxidation Contaminant Oxidation Kinetics

    Science.gov (United States)

    2007-12-01

    natural oxidant demand •OH hydroxide radical Ox oxidant O3 ozone PCE perchloroethylene HSO5− peroxymonosulfate PNDA p...properties (e.g., soil mineralogy , natural carbon content) affect oxidant mobility and stability in the subsurface, and develop a standardized natural...chlorinated ethenes For contaminant oxidation by activated S2O82−, it is more difficult to develop a general description of kobs vs. T because there are

  13. Co-sintering of CGO/NIO-CGO bilayers for solid oxide fuel cell

    International Nuclear Information System (INIS)

    Neto, P.P.B.; Grilo, J.P.F.; Souza, G.L.; Macedo, D.A.; Paskocimas, C.A.; Nascimento, R.M.

    2012-01-01

    Reducing the operating temperature of solid oxide fuel cells (SOFC) for the range between 500 and 700°C is one of the challenges which more has aroused the interest of research in SOFC in recent years. In this context, the bilayer anode/electrolyte composed of a porous support based on Ni-doped ceria (anode) and a ceria doped gadolinia (CGO) electrolyte, presents itself as one of the half-cell configurations of the most interest towards the production of electricity in the operating logic of a SOFC. In this work, CGO films were successfully prepared on NiO-CGO substrates using the resources of the screen-printing technique. The bi-layers were co-sintered between 1350 and 1450 ° C for 4 h and then characterized by scanning electron microscopy and energy dispersive X-ray spectroscopy (EDS). The results showed good adhesion at the film/substrate interface and no cracks in the films. (author)

  14. Microscopy of Alloy Formation on Arc Plasma Sintered Oxide Dispersion Strengthen (ODS) Steel

    Science.gov (United States)

    Bandriyana, B.; Sujatno, A.; Salam, R.; Dimyati, A.; Untoro, P.

    2017-07-01

    The oxide dispersed strengthened (ODS) alloys steel developed as structure material for nuclear power plants (NPP) has good resistant against creep due to their unique microstructure. Microscopy investigation on the microstructure formation during alloying process especially at the early stages was carried out to study the correlation between structure and property of ODS alloys. This was possible thanks to the arc plasma sintering (APS) device which can simulate the time dependent alloying processes. The ODS sample with composition of 88 wt.% Fe and 12 wt.% Cr powder dispersed with 1 wt.% ZrO2 nano powder was mixed in a high energy milling, isostatic compressed to form sample coins and then alloyed in APS. The Scanning Electron Microscope (SEM) with X-ray Diffraction Spectroscopy (EDX) line scan and mapping was used to characterize the microstructure and elemental composition distribution of the samples. The alloying process with unification of each Fe and Cr phase continued by the alloying formation of Fe-Cr by inter-diffusion of both Fe and Cr and followed by the improvement of the mechanical properties of hardness.

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

    Science.gov (United States)

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

    2016-01-01

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

  16. Real-Time Observation of Platinum Redispersion on Ceria-Based Oxide by In-situ Turbo-XAS in Fluorescence Mode

    International Nuclear Information System (INIS)

    Nagai, Yasutaka; Dohmae, Kazuhiko; Tanabe, Toshitaka; Shinjoh, Hirofumi; Takagi, Nobuyuki; Ikeda, Yasuo; Guilera, Gemma; Pascarelli, Sakura; Newton, Mark; Matsumoto, Shin'ichi

    2007-01-01

    A real-time observation of the redispersion behavior of sintered Pt on ceria-based oxide was made possible by in-situ time-resolved Turbo-XAS in fluorescence mode. 2 wt% Pt/Ce-Zr-Y mixed oxide samples were prepared, and then treated under an aging condition. The average Pt particle size measured by CO absorption method after aging was 7 nm. Redispersion treatments of the previously aged catalyst were carried out at 600 deg. C within an in-situ XAS cell in a cyclical flow of reducing/oxidizing gases. Pt L3-edge XANES spectra were collected every 1.1 second under in-situ conditions. From a change in the XANES spectra, we observed that the Pt particle size of the aged catalyst decreased from 7 to 5 nm after 60 seconds and then to 3 nm after 1000 seconds

  17. In Situ Atom Probe Deintercalation of Lithium-Manganese-Oxide.

    Science.gov (United States)

    Pfeiffer, Björn; Maier, Johannes; Arlt, Jonas; Nowak, Carsten

    2017-04-01

    Atom probe tomography is routinely used for the characterization of materials microstructures, usually assuming that the microstructure is unaltered by the analysis. When analyzing ionic conductors, however, gradients in the chemical potential and the electric field penetrating dielectric atom probe specimens can cause significant ionic mobility. Although ionic mobility is undesirable when aiming for materials characterization, it offers a strategy to manipulate materials directly in situ in the atom probe. Here, we present experimental results on the analysis of the ionic conductor lithium-manganese-oxide with different atom probe techniques. We demonstrate that, at a temperature of 30 K, characterization of the materials microstructure is possible without measurable Li mobility. Also, we show that at 298 K the material can be deintercalated, in situ in the atom probe, without changing the manganese-oxide host structure. Combining in situ atom probe deintercalation and subsequent conventional characterization, we demonstrate a new methodological approach to study ionic conductors even in early stages of deintercalation.

  18. In Situ Study of Noncatalytic Metal Oxide Nanowire Growth

    DEFF Research Database (Denmark)

    Rackauskas, Simas; Jiang, Hua; Wagner, Jakob Birkedal

    2014-01-01

    a catalyst is still widely disputed and unclear. Here, we show that the nanowire growth during metal oxidation is limited by a nucleation of a new layer. On the basis of in situ transmission electron microscope investigations we found that the growth occurs layer by layer at the lowest specific surface...

  19. Microstructure and Mechanical Properties of Multiphase Strengthened Al/Si/Al_2O_3/SiO_2/MWCNTs Nano composites Sintered by In Situ Vacuum Hot Pressing

    International Nuclear Information System (INIS)

    Li, J.; Jiang, X.; Zhu, D.; Zhu, M.; Shao, Z.; Johnson, S.; Luo, Z.

    2015-01-01

    Eutectic Al/Si binary alloy is technically one of the most important Al casting alloys due to its high corrosion resistance, evident shrinkage reduction, low thermal expansion coefficient, high fluidity, and good weldability. In this work, multi phased Al/Si matrix nano composites reinforced with Al_2O_3 and multi walled carbon nano tubes (MWCNTs) have been sintered by an in situ vacuum hot-pressing method. The alumina Al_2O_3 nanoparticles were introduced by an in situ reaction of Al with SiO_2. Microstructure and mechanical properties of the sintered Al/Si/Al_2O_3/SiO_2/MWCNTs nano composites with different alumina contents were investigated. The mechanical properties were determined by micro-Vickers hardness and compressive and shear strength tests. The results demonstrated that in situ alumina and MWCNTs had impacts on microstructure and mechanical properties of the nano composites. Based on the mechanical properties and microstructure of the nano composites, strengthening and fracture mechanisms by multiple reinforcements were analyzed

  20. Characterization and Electrical Response to Humidity of Sintered Polymeric Electrospun Fibers of Vanadium Oxide-({TiO}_{{2}} /{WO}_{{3}} )

    Science.gov (United States)

    Araújo, E. S.; Libardi, J.; Faia, P. M.; de Oliveira, H. P.

    2018-02-01

    Metal oxide composites have attracted much consideration due to their promising applications in humidity sensors in response to the physical and chemical property modifications of the resulting materials. This work focused on the preparation, microstructural characterization and analysis of humidity-dependent electrical properties of undoped and vanadium oxide (V2O5)-doped titanium oxide/tungsten oxide (TiO2/WO3) sintered ceramic films obtained by electrospinning. The electrical properties were investigated by impedance spectroscopy (400 Hz-40 MHz) as a function of relative humidity (RH). The results revealed a typical transition in the transport mechanisms controlled by the appropriated doping level of V2O5, which introduces important advantages to RH detection due to the atomic substitution of titanium by vanadium atoms in highly doped structures. These aspects are directly related to the microstructure modification and structure fabrication procedure.

  1. Mechanism of mechanochemical synthesis of complex oxides and the peculiarities of their nano-structurization determining sintering

    Directory of Open Access Journals (Sweden)

    Zyryanov V.V.

    2005-01-01

    Full Text Available A mechanism of superfast mechanosynthesis reaction for oxide systems is proposed on the base of a dynamics study. The threshold effect and linear dependence of the chemical response on the effective temperature of the reaction zone are established. Major factors are determined: molecular mass of reagents, enthalpy and difference of reagents in Mohs’s hardness, which also influence the composition of the primary product. Primary acts are characterized by a superfast roller mechanism of mass transfer with the formation of a transient dynamic state (D*. Secondary acts slowly approximate the composition of the product to the composition of the starting mixture by diffusion mass transfer in a deformation mixing regime with a contribution of a rotation (roller mechanism. The list of structure types for complex oxides derived by mechanosynthesis includes perovskites, fluorites, pyrochlors, sheelites, and some other ones. Powders of crystal products display multilevel structurization. In all studied complex oxides strong disordering of the “anti-glass” type was observed. The mechanism of sintering was studied in BaTiO3 powders of different origin and in metastable complex oxides derived by mechanosynthesis. The major contribution in shrinkage belongs to rearrangements of crystalline particles as a whole. Structure transformations accompany, as a rule, sintering of inhomogeneous powders derived by mechanosynthesis.

  2. High Temperature Oxidation of Spark Plasma Sintered and Thermally Sprayed FeAl-Based Iron Aluminides

    Czech Academy of Sciences Publication Activity Database

    Haušild, P.; Karlík, M.; Skiba, T.; Sajdl, P.; Dubský, Jiří; Palm, M.

    2012-01-01

    Roč. 122, č. 3 (2012), s. 465-468 ISSN 0587-4246. [International Symposium on Physics of Materials (ISPMA)/12./. Prague, 04.09.2011-08.09.2011] Institutional support: RVO:61389021 Keywords : thermal spraying * plasma sintering Subject RIV: JH - Ceramics, Fire-Resistant Materials and Glass Impact factor: 0.531, year: 2012

  3. Study of pore closure during pressure-less sintering of advanced oxide ceramics

    Czech Academy of Sciences Publication Activity Database

    Spusta, T.; Svoboda, Jiří; Maca, K.

    2016-01-01

    Roč. 115, AUG (2016), s. 347-353 ISSN 1359-6454 R&D Projects: GA ČR(CZ) GA15-06390S Institutional support: RVO:68081723 Keywords : Ceramic material * Sintering * Porosity * Modelling * Hot isostatic pressing Subject RIV: BJ - Thermodynamics Impact factor: 5.301, year: 2016

  4. In situ Oxidation of Ultrathin Silver Films on Ni(111)

    International Nuclear Information System (INIS)

    Meyer, A.; Flege, I.; Senanayake, S.; Kaemena, B.; Rettew, R.; Alamgir, F.; Falta, J.

    2011-01-01

    Oxidation of silver films of one- and two-monolayer thicknesses on the Ni(111) surface was investigated by low-energy electron microscopy at temperatures of 500 and 600 K. Additionally, intensity-voltage curves were measured in situ during oxidation to reveal the local film structure on a nanometer scale. At both temperatures, we find that exposure to molecular oxygen leads to the destabilization of the Ag film with subsequent relocation of the silver atoms to small few-layer-thick silver patches and concurrent evolution of NiO(111) regions. Subsequent exposure of the oxidized surface to ethylene initiates the transformation of bilayer islands back into monolayer islands, demonstrating at least partial reversibility of the silver relocation process at 600 K.

  5. A study of emission property and microstructure of rare earth oxide-molybdenum cermet cathode materials made by spark plasma sintering

    International Nuclear Information System (INIS)

    Wang Jinshu; Li Hongyi; Yang Sa; Cui Ying; Zhou Meiling

    2004-01-01

    A fast sintering method, spark plasma sintering (SPS) was used for the synthesis of rare earth oxide-molybdenum cathode material. The secondary emission property, microstructure, and phase constitution of materials have been studied in this paper. The experimental results show that the maximum secondary emission coefficient of this material can be high to 3.84, much higher than that of rare earth oxide-molybdenum cathode made by traditional sintering method. The grain size is less than 1 μm and rare earth distributed evenly in the material. After the material was activated at 1600 deg. C, a 4 μm layer of rare earth oxide which leads to the high secondary emission coefficient of the material, is formed on the surface of the cathode

  6. Contribution to the study of the sintering of uranium oxide; Contribution a l'etude du frittage de l'oxyde d'uranium

    Energy Technology Data Exchange (ETDEWEB)

    Bel, A; Carteret, Y [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1958-07-01

    The sintering ofnium oxide has been considered and the following factors have been particularly taken in consideration: - the particle size and the particles in shape of the initial powder, - the specific area of the initial powder, - the chemical composition of the oxide, - and the medium in which the sintering was carried out. A method of sintering uranium oxide on semi-industrial scale is presented. (author)Fren. [French] On xamine l'influence de differents facteurs sur le frittage de l'oxyde d'uranium. Sont particulierement prises en consideration: - la taille et la forme des grains de la poudre initiale, - la surface specifique de la poudre initiale, - la composition chimique de l'oxyde, - ainsi que la nature de l'atmosphere durant le frittage. D'autre part, une technique de frittage de l'oxyde d'uranium a l'echelle semi-industrielle est presentee. (auteur)

  7. Effect of rare earth oxide addition on microstructures of ultra-fine WC-Co particulate reinforced Cu matrix composites prepared by direct laser sintering

    International Nuclear Information System (INIS)

    Gu Dongdong; Shen Yifu; Zhao Long; Xiao Jun; Wu Peng; Zhu Yongbing

    2007-01-01

    This paper presents a detailed investigation into the influence of the rare earth (RE) oxide (La 2 O 3 ) addition upon the densification and the resultant microstructural characteristics of the submicron WC-Co particulate reinforced Cu matrix composites prepared by direct laser sintering. It is found that the relative density of the laser sintered sample with 1 wt.% La 2 O 3 addition increased by 11.5% as compared with the sample without RE addition. The addition of RE element favored the microstructural refinement and improved the particulate dispersion homogeneity and the particulate/matrix interfacial coherence. The metallurgical functions of the RE element in improving the sinterability were also addressed. It shows that due to the unique properties of RE element such as high surface activity and large atomic radius, the addition of trace RE element can decrease the surface tension of the melt, resist the grain growth coarsening and increase the heterogeneous nucleation rate during laser sintering

  8. Effect of different sintering aids on thermo-mechanical properties and oxidation of SiC fibers - Reinforced ZrB{sub 2} composites

    Energy Technology Data Exchange (ETDEWEB)

    Sciti, D., E-mail: diletta.sciti@istec.cnr.it [ISTEC-CNR, Institute of Science and Technology for Ceramics, National Research Council, Via Granarolo 64, I-48018 Faenza (Italy); Silvestroni, L. [ISTEC-CNR, Institute of Science and Technology for Ceramics, National Research Council, Via Granarolo 64, I-48018 Faenza (Italy); Saccone, G.; Alfano, D. [CIRA, Italian Aerospace Research Center, 81043 Capua (Italy)

    2013-01-15

    Reinforced zirconium diboride composites containing 15 vol% of Hi Nicalon SiC chopped fibers were hot pressed with addition of various sintering additives, Si{sub 3}N{sub 4}, ZrSi{sub 2} or MoSi{sub 2}. Depending on the sintering aid, different densification temperatures were set in the range 1650-1750 Degree-Sign C. Temperature and additive strongly influenced the matrix/fiber interface, which in turn had a strong impact on the mechanical properties and the oxidation behavior at 1650 Degree-Sign C. Even the workability, performed either by conventional machining or electro discharge machining, varied depending on the sintering additive and the secondary phases formed in the system. The system containing Si{sub 3}N{sub 4} turned out to have the highest mechanical properties, but intermediate oxidation resistance; the composite containing ZrSi{sub 2} had the lowest sintering temperature, but displayed the worst oxidation resistance, and finally the composite containing MoSi{sub 2} showed intermediate mechanical properties, but the highest oxidation resistance and lowest degree of damage upon machining. Preliminary measurements of thermal shock resistance by the water quenching method were also carried out. -- Highlights: Black-Right-Pointing-Pointer We produced SiC fibers reinforced ZrB{sub 2} using different sintering aids. Black-Right-Pointing-Pointer The sintering additives affected properties, oxidation and machinability. Black-Right-Pointing-Pointer The system containing Si{sub 3}N{sub 4} had the highest mechanical properties. Black-Right-Pointing-Pointer The composite containing MoSi{sub 2} had the highest oxidation resistance. Black-Right-Pointing-Pointer ZrB{sub 2}-SiC fibers have higher thermal shock resistance than ZrB{sub 2}-SiC particles.

  9. Geochemical and Microbiological Characteristics during in Situ Chemical Oxidation and in Situ Bioremediation at a Diesel Contaminated Site

    NARCIS (Netherlands)

    Sutton, N.B.; Kalisz, M.; Krupanek, J.; Marek, J.; Grotenhuis, J.T.C.; Smidt, H.; Weert, de J.; Rijnaarts, H.H.M.; Gaans, van P.; Keijzer, T.

    2014-01-01

    While in situ chemical oxidation with persulfate has seen wide commercial application, investigations into the impacts on groundwater characteristics, microbial communities and soil structure are limited. To better understand the interactions of persulfate with the subsurface and to determine the

  10. Improvement of the electrochromic response of a low-temperature sintered dye-modified porous electrode using low-resistivity indium tin oxide nanoparticles

    International Nuclear Information System (INIS)

    Watanabe, Yuichi; Suemori, Kouji; Hoshino, Satoshi

    2016-01-01

    An indium tin oxide (ITO) nanoparticle-based porous electrode sintered at low temperatures was investigated as a transparent electrode for electrochromic displays (ECDs). The electrochromic (EC) response of the dye-modified ITO porous electrode sintered at 150 °C, which exhibited a generally low resistivity, was markedly superior to that of a conventional dye-modified TiO 2 porous electrode sintered at the same temperature. Moreover, the EC characteristics of the dye-modified ITO porous electrode sintered at 150 °C were better than those of the high-temperature (450 °C) sintered conventional dye-modified TiO 2 porous electrode. These improvements in the EC characteristics of the dye-modified ITO porous electrode are attributed to its lower resistivity than that of the TiO 2 porous electrodes. In addition to its sufficiently low resistivity attained under the sintering conditions required for flexible ECD applications, the ITO porous film had superior visible-light transparency and dye adsorption capabilities. We conclude that the process temperature, resistivity, optical transmittance, and dye adsorption capability of the ITO porous electrode make it a promising transparent porous electrode for flexible ECD applications.

  11. In-Situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes

    Science.gov (United States)

    2010-12-28

    DATES COVERED (From - To) 1/29/10-9/30/10 4. TITLE AND SUBTITLE In situ optical studies of oxidation/reduction kinetics on SOFC cermet anodes 5a...0572 In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Department of Chemistry and Biochemistry Montana State University...of Research In-situ Optical Studies of Oxidation/Reduction Kinetics on SOFC Cermet Anodes Principal Investigator Robert Walker Organization

  12. On bacteria oxidizing enlargement scale test for uranium in-situ leaching at. 381 mine

    International Nuclear Information System (INIS)

    Hu Kaiguang; Wang Qingliang; Liu Yingjiu; Shi Wenge; Hu Shihe; Hu Yincai; Fang Qiu

    1999-01-01

    The results of enlarged scale test of bacteria as oxidizer for uranium in-situ leaching at No 381 mine showed that redox potential of the oxidized absorbed tailing water by bacteria is more than 510 mV, without any effects on after treatments by using bacteria as oxidizer and reduce oxidizer costs 70% compared with H 2 O 2 as oxidizer

  13. Study on the isothermal oxidation behavior in air of Ti3AlC2 sintered by hot pressing

    Institute of Scientific and Technical Information of China (English)

    XU Xuewen; LI Yangxian; MEI Bingchu; ZHU Jiaoqun; LIU Heyan; QU Jingping

    2006-01-01

    The isothermal oxidation behavior at 900―1300℃ for 20 h in air of bulk Ti3AlC2 with 2.8 wt% TiC sintered by means of hot pressing was investigated in the work. The isothermal oxidation behavior generally followed a parabolic rate law. The parabolic rate constants increased from 1.39×10-10 kg2·m-4·s-1 at 900℃ to 5.56×10-9 kg2·m-4·s-1 at 1300℃. The calculated activation energy was 136.45 kJ/mol. It was demonstrated that Ti3AlC2 had excellent oxidation resistance due to the continuous, dense and adhesive protect scales consisted of a mass of α-Al2O3 and a little of TiO2 and/or Al2TiO5. In principle, the oxide scale was grown by the inward diffusion of O2- and the outward diffusion of Ti4+ and Al3+. The rapid outward diffusion of cations usually resulted in the formation of cracks, gaps, and holes.

  14. Determination of rare earth elements, hafnium and cadmium in sintered pellets of mixed thorium and uranium oxides by neutron activation

    International Nuclear Information System (INIS)

    Cardoso, S.N.M.

    1987-01-01

    This work shows the development of a method for determination of the rare-earth elements (Eu, Sm, Dy and Gd), Hf and Cd contents in sinterized U and Th mixed oxides by neutron activation analysis. The sample is dissolved in nitric/fluoridric (0,1% HF) medium, to dryness and redissolved in 6N HCl solution. The Hf is extracted into organic phase (0,5 M TTA/benzene), irradiated and analysed through 181 Hf isotope energy peak. The aqueous phase is treated with NH 4 OH for the precipitation of hidroxides. Then, these are dissolved in 6N HNO 3 solution. The extraction of U and Th is made in two steps, one with TBP/CCl 4 and another with 0,5 M TTA/C 6 H 6 . Then the rare-earth elements and Cd are irradiated and determined by gamma spectrometry. (author) [pt

  15. Reaction and Transport Processes Controlling In Situ Chemical Oxidation of DNAPLs

    National Research Council Canada - National Science Library

    Siegrist, Robert L; Crimi, Michelle; Munakata-Marr, Junko; Illangasekare, Tissa; Dugan, Pamela; Heiderscheidt, Jeff; Jackson, Shannon; Petri, Ben; Sahl, Jason; Seitz, Sarah

    2006-01-01

    In situ chemical oxidation involves the introduction of chemical oxidants into the subsurface to destroy organic contaminants in soil and ground water, with the goal being to reduce the mass, mobility...

  16. The effect of sintering time on synthesis of in situ submicron {alpha}-Al{sub 2}O{sub 3} particles by the exothermic reactions of CuO particles in molten pure Al

    Energy Technology Data Exchange (ETDEWEB)

    Dikici, Burak, E-mail: burakdikici@yyu.edu.tr [Yuzuncu Yil University, Department of Mechanical Engineering, 65080 Van (Turkey); Gavgali, Mehmet [Ataturk University, Department of Mechanical Engineering, 25240 Erzurum (Turkey)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer Al-Cu/Al{sub 2}O{sub 3} composites were prepared successfully by means of hot pressing method. Black-Right-Pointing-Pointer Sintering time of the Al-CuO system effect the reaction rate and formation of Al{sub 2}O{sub 3}. Black-Right-Pointing-Pointer Increase in sintering time accelerates formation of submicron in situ {alpha}-Al{sub 2}O{sub 3} phase. Black-Right-Pointing-Pointer Hardness of the sintered composite for 30 min at 1000 Degree-Sign C increased from 60 to 174 HV. - Abstract: In this study, in situ {alpha}-Al{sub 2}O{sub 3} reinforcing particles have been successfully synthesised in an Al-Cu matrix alloy by means of the conventional Hot Pressing (HP) method. The effect of sintering time on the forming of the {alpha}-Al{sub 2}O{sub 3} phase at 1000 Degree-Sign C was investigated using Differential Thermal Analysis (DTA), X-ray Diffraction (XRD) and a Scanning Electron Microscope (SEM). The sintered composites contained thermodynamically stable {alpha}-Al{sub 2}O{sub 3} particles and {theta}-Al{sub 2}Cu eutectic phases, which were embedded in the Al-Cu matrix. The in situ {alpha}-Al{sub 2}O{sub 3} particles were generally spherical and their mean size was observed to be less than 0.5 {mu}m. The results showed that sintering time influences not only the reaction rate of copper and the formation of Al{sub 2}O{sub 3}. Also, an increase in the sintering time accelerates the formation of submicron in situ {alpha}-Al{sub 2}O{sub 3} particles and decreases the quantity of {theta}-Al{sub 2}Cu intermetallic phase in the liquid aluminium. Additionally, sintering of composite for 30 min at 1000 Degree-Sign C increased the hardness from 60 to 174 HV.

  17. Quantification of the effect of in-situ generated uranium metal on the experimentally determined O/U ratio of a sintered uranium dioxide fuel pellet

    International Nuclear Information System (INIS)

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

    2005-01-01

    This paper describes quantitatively the effect of in-situ generated uranium metal (that could be formed due to the conducive manufacturing conditions) in a sintered uranium dioxide fuel pellet on the experimentally determined O/U ratio using analytical methods involving dissolution of the pellet material. To quantify the effect of in-situ generated uranium metal in the fuel pellet, a mathematical expression is derived for the actual O/U ratio in terms of the O/U ratio as determined by an experiment involving dissolution of the material and the quantity of uranium metal present in the uranium dioxide pellet. The utility of this derived mathematical expression is demonstrated by tabulating the calculated actual O/U ratios for varying amounts of uranium metal (from 5 to 95% in 5% intervals) and different O/U ratio values (from 2.001 to 2.015 in 0.001 intervals). This paper brings out the necessity of care to be exercised while interpreting the experimentally determined O/U ratio and emphasizes the fact that it is always safer to produce the nuclear fuel with oxygen to uranium ratios well below the specified maximum limit of 2.015. (author)

  18. In situ tribochemical sulfurization of molybdenum oxide nanotubes.

    Science.gov (United States)

    Rodríguez Ripoll, Manel; Tomala, Agnieszka; Gabler, Christoph; DraŽić, Goran; Pirker, Luka; Remškar, Maja

    2018-02-15

    MoS 2 nanoparticles are typically obtained by high temperature sulfurization of organic and inorganic precursors under a S rich atmosphere and have excellent friction reduction properties. We present a novel approach for making the sulfurization unnecessary for MoO 3 nanotubes during the synthesis process for friction and wear reduction applications while simultaneously achieving a superb tribological performance. To this end, we report the first in situ sulfurization of MoO 3 nanotubes during sliding contact in the presence of sulfur-containing lubricant additives. The sulfurization leads to the tribo-chemical formation of a MoS 2 -rich low-friction tribofilm as verified using Raman spectroscopy and can be achieved both during sliding contact and under extreme pressure conditions. Under sliding contact conditions, MoO 3 nanotubes in synergy with sulfurized olefin polysulfide and pre-formed zinc dialkyl dithiophosphate tribofilms achieve an excellent friction performance. Under these conditions, the tribochemical sulfurization of MoO 3 nanotubes leads to a similar coefficient of friction to the one obtained using a model nanolubricant containing MoS 2 nanotubes. Under extreme pressure conditions, the in situ sulfurization of MoO 3 nanotubes using sulfurized olefin polysulfide results in a superb load carrying capacity capable of outperforming MoS 2 nanotubes. The reason is that while MoO 3 nanotubes are able to continuously sulfurize during sliding contact conditions, MoS 2 nanotubes progressively degrade by oxidation thus losing lubricity.

  19. Influence of sintering atmospheres on the aluminium sintering characteristics

    International Nuclear Information System (INIS)

    Mintzer, S.; Bermudez Belkys, S.

    1993-01-01

    This paper describes the aluminium powder (Al) cool compacted (at 95% from theoretical density) which was sintered at 903 K during 4 hours at different atmospheres; oxidizing (air), inert Argon (Ar), Nitrogen (N) and high vacuum. The results obtained show: a) porosity measurements; greater porosity when sintering in Ar and air. b) Metallographic and Scanning observations: many fine pores (< 1 μm) and pore lines distributed at random, at air sintering and greater pores distributed preferentially near the surface, in Ar and N atmospheres. c) Dimensional changes: tendency to contraction of the samples at N and vacuum sintering and expansion in Ar or air. d) Mechanical properties: greater strength and fluence stresses at air and N sintering. The analysis of the results is performed considering sintering modes in presence of an oxide layer and dropped inert gases. (Author)

  20. High temperature oxidation-sulfidation behavior of Cr-Al2O3 and Nb-Al2O3 composites densified by spark plasma sintering

    International Nuclear Information System (INIS)

    Saucedo-Acuna, R.A.; Monreal-Romero, H.; Martinez-Villafane, A.; Chacon-Nava, J.G.; Arce-Colunga, U.; Gaona-Tiburcio, C.; De la Torre, S.D.

    2007-01-01

    The high temperature oxidation-sulfidation behavior of Cr-Al 2 O 3 and Nb-Al 2 O 3 composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO 2 + 3.6%O 2 + N 2 (balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al 2 O 3 and Nb-Al 2 O 3 composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr 2 O 3 layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al 2 O 3 composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy

  1. Development of an in-situ multi-component reinforced Al-based metal matrix composite by direct metal laser sintering technique — Optimization of process parameters

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Subrata Kumar, E-mail: subratagh82@gmail.com [Department of Mechanical Engineering, National Institute of Technology Agartala, Tripura 799055 (India); Bandyopadhyay, Kaushik; Saha, Partha [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Kharagpur 721302 (India)

    2014-07-01

    In the present investigation, an in-situ multi-component reinforced aluminum based metal matrix composite was fabricated by the combination of self-propagating high-temperature synthesis and direct metal laser sintering process. The different mixtures of Al, TiO{sub 2} and B{sub 4}C powders were used to initiate and maintain the self-propagating high-temperature synthesis by laser during the sintering process. It was found from the X-ray diffraction analysis and scanning electron microscopy that the reinforcements like Al{sub 2}O{sub 3}, TiC, and TiB{sub 2} were formed in the composite. The scanning electron microscopy revealed the distribution of the reinforcement phases in the composite and phase identities. The variable parameters such as powder layer thickness, laser power, scanning speed, hatching distance and composition of the powder mixture were optimized for higher density, lower porosity and higher microhardness using Taguchi method. Experimental investigation shows that the density of the specimen mainly depends upon the hatching distance, composition and layer thickness. On the other hand, hatching distance, layer thickness and laser power are the significant parameters which influence the porosity. The composition, laser power and layer thickness are the key influencing parameters for microhardness. - Highlights: • The reinforcements such as Al{sub 2}O{sub 3}, TiC, and TiB{sub 2} were produced in Al-MMC through SHS. • The density is mainly influenced by the material composition and hatching distance. • Hatching distance is the major influencing parameter on porosity. • The material composition is the significant parameter to enhance the microhardness. • The SEM micrographs reveal the distribution of TiC, TiB{sub 2} and Al{sub 2}O{sub 3} in the composite.

  2. Development of an in-situ multi-component reinforced Al-based metal matrix composite by direct metal laser sintering technique — Optimization of process parameters

    International Nuclear Information System (INIS)

    Ghosh, Subrata Kumar; Bandyopadhyay, Kaushik; Saha, Partha

    2014-01-01

    In the present investigation, an in-situ multi-component reinforced aluminum based metal matrix composite was fabricated by the combination of self-propagating high-temperature synthesis and direct metal laser sintering process. The different mixtures of Al, TiO 2 and B 4 C powders were used to initiate and maintain the self-propagating high-temperature synthesis by laser during the sintering process. It was found from the X-ray diffraction analysis and scanning electron microscopy that the reinforcements like Al 2 O 3 , TiC, and TiB 2 were formed in the composite. The scanning electron microscopy revealed the distribution of the reinforcement phases in the composite and phase identities. The variable parameters such as powder layer thickness, laser power, scanning speed, hatching distance and composition of the powder mixture were optimized for higher density, lower porosity and higher microhardness using Taguchi method. Experimental investigation shows that the density of the specimen mainly depends upon the hatching distance, composition and layer thickness. On the other hand, hatching distance, layer thickness and laser power are the significant parameters which influence the porosity. The composition, laser power and layer thickness are the key influencing parameters for microhardness. - Highlights: • The reinforcements such as Al 2 O 3 , TiC, and TiB 2 were produced in Al-MMC through SHS. • The density is mainly influenced by the material composition and hatching distance. • Hatching distance is the major influencing parameter on porosity. • The material composition is the significant parameter to enhance the microhardness. • The SEM micrographs reveal the distribution of TiC, TiB 2 and Al 2 O 3 in the composite

  3. An easily sintered, chemically stable, barium zirconate-based proton conductor for high-performance proton-conducting solid oxide fuel cells

    KAUST Repository

    Sun, Wenping

    2014-07-25

    Yttrium and indium co-doped barium zirconate is investigated to develop a chemically stable and sintering active proton conductor for solid oxide fuel cells (SOFCs). BaZr0.8Y0.2-xInxO3- δ possesses a pure cubic perovskite structure. The sintering activity of BaZr0.8Y0.2-xInxO3- δ increases significantly with In concentration. BaZr0.8Y0.15In0.05O3- δ (BZYI5) exhibits the highest total electrical conductivity among the sintered oxides. BZYI5 also retains high chemical stability against CO2, vapor, and reduction of H2. The good sintering activity, high conductivity, and chemical stability of BZYI5 facilitate the fabrication of durable SOFCs based on a highly conductive BZYI5 electrolyte film by cost-effective ceramic processes. Fully dense BZYI5 electrolyte film is successfully prepared on the anode substrate by a facile drop-coating technique followed by co-firing at 1400 °C for 5 h in air. The BZYI5 film exhibits one of the highest conductivity among the BaZrO3-based electrolyte films with various sintering aids. BZYI5-based single cells output very encouraging and by far the highest peak power density for BaZrO3-based proton-conducting SOFCs, reaching as high as 379 mW cm-2 at 700 °C. The results demonstrate that Y and In co-doping is an effective strategy for exploring sintering active and chemically stable BaZrO3-based proton conductors for high performance proton-conducting SOFCs. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  4. Polycrystalline oxides formation during transient oxidation of (001) Cu-Ni binary alloys studied by in situ TEM and XRD

    International Nuclear Information System (INIS)

    Yang, J.C.; Li, Z.Q.; Sun, L.; Zhou, G.W.; Eastman, J.A.; Fong, D.D.; Fuoss, P.H.; Baldo, P.M.; Rehn, L.E.; Thompson, L.J.

    2009-01-01

    The nucleation and growth of Cu 2 O and NiO islands due to oxidation of Cu x Ni 1-x (001) films were monitored, at various temperatures, by in situ ultra-high vacuum (UHV) transmission electron microscopy (TEM) and in situ synchrotron X-ray diffraction (XRD). In remarkable contrast to our previous observations of Cu and Cu-Au oxidation, irregular-shaped polycrystalline oxide islands formed with respect to the Cu-Ni alloy film, and an unusual second oxide nucleation stage was noted. In situ XRD experiments revealed that NiO formed first epitaxially, then other orientations appeared, and finally polycrystalline Cu 2 O developed as the oxidation pressure was increased. The segregation of Ni and Cu towards or away, respectively, from the alloy surface during oxidation could disrupt the surface and cause polycrystalline oxide formation.

  5. Special metallurgy - the electrical butt-welding by flashing of sintered magnesium-magnesium oxide composites (1963)

    International Nuclear Information System (INIS)

    Charleux, J.

    1963-01-01

    Electrical resistance welding has become quite important since World War II because of the need of a high yield in aeronautical production. Progress has been due in particular to the improvements made in electronically controlled apparatus making possible the automatic control of welding. For the butt-welding of sections requiring either a high production rate or a high quality weld, the flash butt-welding system has been very much developed these last few years. The use of this welding method is of great importance in the field of the bonding of oxidisable metals such as magnesium or aluminium and its alloys, because the welded joint is free from oxides. This study consists of general considerations on the flash-welding process with regard to temperature distribution in the parts during welding, and to electrical phenomena connected with flashing. Besides this general or theoretical section, we have applied the welding process to the bonding of sintered magnesium, a magnesium-magnesium oxide composite, whose use as a structural element in nuclear reactors is considered. (author) [fr

  6. Cost and Performance Assessment of In-situ Chemical Oxidation for Intermittent and Continuous Oxidant Injection

    Science.gov (United States)

    Kim, U.; Parker, J.; Borden, R. C.

    2015-12-01

    In situ chemical oxidation (ISCO) is a popular remediation technology that involves injection of chemical oxidant into groundwater to destroy dissolved and non-aqueous liquid phase contaminants. Depending on site conditions, oxidant can be injected into the contaminated subsurface periodically (intermittently) or continuously. A common approach is to intermittently inject oxidant into a network of wells over a period long enough to emplace oxidant over a target treatment volume (referred to ISCO-int). The injection phase is followed by a passive phase when the oxidant is allowed to react with contaminants and natural oxygen demand (NOD) and to migrate under natural hydraulic gradients. This process may be repeated multiple times until termination criteria are met. Recently, some practitioners have adopted an alternative approach in which oxidant is injected continuously with extraction wells recovering unreacted oxidant to recycle with additional makeup oxidant to maintain its constant concentration (referred to ISCO-cont). Each method has certain advantages and disadvantages. This study numerically evaluates those two ISCO practices in terms of remediation costs and performance based on multiple equi-probable parameter sets. Stochastic cost optimization toolbox (SCOToolkit) is used for this purpose. SCOToolkit is an integrated semi-analytical model for contaminant transport and remediation (e.g., thermal source treatment, ISCO, electron donor injections, permeable reactive barriers) enabling inverse solution and Monte Carlo simulations. Four different aquifer settings, slow and fast Darcy velocities combined with low and high NOD conditions, are used for the evaluation. Preliminary results showed that ISCO-cont is effective for a full scale application without large investment while ISCO-int is more efficient to utilize oxidant in well-characterized sites. Pros and cons of each approach are discussed for the practical use of ISCO for various site conditions.

  7. In situ chemical synthesis of ruthenium oxide/reduced graphene oxide nanocomposites for electrochemical capacitor applications.

    Science.gov (United States)

    Kim, Ji-Young; Kim, Kwang-Heon; Yoon, Seung-Beom; Kim, Hyun-Kyung; Park, Sang-Hoon; Kim, Kwang-Bum

    2013-08-07

    An in situ chemical synthesis approach has been developed to prepare ruthenium oxide/reduced graphene oxide (RGO) nanocomposites. It is found that as the C/O ratio increases, the number density of RuO2 nanoparticles decreases, because the chemical interaction between the Ru ions and the oxygen-containing functional groups provides anchoring sites where the nucleation of particles takes place. For electrochemical capacitor applications, the microwave-hydrothermal process was carried out to improve the conductivity of RGO in RuO2/RGO nanocomposites. The significant improvement in capacitance and high rate capability might result from the RuO2 nanoparticles used as spacers that make the interior layers of the reduced graphene oxide electrode available for electrolyte access.

  8. Determination of the initial oxidation behavior of Zircaloy-4 by in-situ TEM

    International Nuclear Information System (INIS)

    Harlow, Wayne; Ghassemi, Hessam; Taheri, Mitra L.

    2016-01-01

    The corrosion behavior of Zircaloy-4 (Zry-4), specifically by oxidation, is a problem of great importance as this material is critical for current nuclear reactor cladding. The early formation behavior and structure of the oxide layer during oxidation was studied using in-situ TEM techniques that allowed for Zry-4 to be monitored during corrosion. These environmental exposure experiments were coupled with precession electron diffraction to identify and quantify the phases present in the samples before and after the oxidation. Following short-term, high temperature oxidation, the dominant phase was revealed to be monoclinic ZrO 2 in a columnar structure. These samples oxidized in-situ contained structures that correlated well with bulk Zry-4 subjected to autoclave treatment, which were used for comparison and validation of this technique. By using in-situ TEM the effect of microstructure features, such as grain boundaries, on oxidation behavior of an alloy can be studied. The technique presented herein holds the potential to be applied any alloy system to study these effects. - Highlights: • In-situ TEM was used to oxidize samples of Zircaloy-4. • Similar behavior was found in the in-situ oxidized and autoclave-oxidized samples. • Precession diffraction was used to characterize oxide phase and texture.

  9. 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.

  10. Sintered indium-tin oxide particles induce pro-inflammatory responses in vitro, in part through inflammasome activation.

    Directory of Open Access Journals (Sweden)

    Melissa A Badding

    Full Text Available Indium-tin oxide (ITO is used to make transparent conductive coatings for touch-screen and liquid crystal display electronics. As the demand for consumer electronics continues to increase, so does the concern for occupational exposures to particles containing these potentially toxic metal oxides. Indium-containing particles have been shown to be cytotoxic in cultured cells and pro-inflammatory in pulmonary animal models. In humans, pulmonary alveolar proteinosis and fibrotic interstitial lung disease have been observed in ITO facility workers. However, which ITO production materials may be the most toxic to workers and how they initiate pulmonary inflammation remain poorly understood. Here we examined four different particle samples collected from an ITO production facility for their ability to induce pro-inflammatory responses in vitro. Tin oxide, sintered ITO (SITO, and ventilation dust particles activated nuclear factor kappa B (NFκB within 3 h of treatment. However, only SITO induced robust cytokine production (IL-1β, IL-6, TNFα, and IL-8 within 24 h in both RAW 264.7 mouse macrophages and BEAS-2B human bronchial epithelial cells. Our lab and others have previously demonstrated SITO-induced cytotoxicity as well. These findings suggest that SITO particles activate the NLRP3 inflammasome, which has been implicated in several immune-mediated diseases via its ability to induce IL-1β release and cause subsequent cell death. Inflammasome activation by SITO was confirmed, but it required the presence of endotoxin. Further, a phagocytosis assay revealed that pre-uptake of SITO or ventilation dust impaired proper macrophage phagocytosis of E. coli. Our results suggest that adverse inflammatory responses to SITO particles by both macrophage and epithelial cells may initiate and propagate indium lung disease. These findings will provide a better understanding of the molecular mechanisms behind an emerging occupational health issue.

  11. In Situ Study of Thermal Stability of Copper Oxide Nanowires at Anaerobic Environment

    Directory of Open Access Journals (Sweden)

    Lihui Zhang

    2014-01-01

    Full Text Available Many metal oxides with promising electrochemical properties were developed recently. Before those metal oxides realize the use as an anode in lithium ion batteries, their thermal stability at anaerobic environment inside batteries should be clearly understood for safety. In this study, copper oxide nanowires were investigated as an example. Several kinds of in situ experiment methods including in situ optical microscopy, in situ Raman spectrum, and in situ transmission electron microscopy were adopted to fully investigate their thermal stability at anaerobic environment. Copper oxide nanowires begin to transform as copper(I oxide at about 250°C and finish at about 400°C. The phase transformation proceeds with a homogeneous nucleation.

  12. Pilot-Scale Demonstration of In-Situ Chemical Oxidation ...

    Science.gov (United States)

    A pilot-scale in situ chemical oxidation (ISCO) demonstration, involving subsurface injections of sodium permanganate (NaMnO4), was performed at the US Marine Corp Recruit Depot (MCRD), site 45 (Parris Island (PI), SC). The ground water was originally contaminated with perchloroethylene (PCE) (also known as tetrachloroethylene), a chlorinated solvent used in dry cleaner operations. High resolution site characterization involved multiple iterations of soil core sampling and analysis. Nested micro-wells and conventional wells were also used to sample and analyze ground water for PCE and decomposition products (i.e., trichloroethyelene (TCE), dichloroethylene (c-DCE, t-DCE), and vinyl chloride (VC)), collectively referred to as chlorinated volatile organic compounds (CVOC). This characterization methodology was used to develop and refine the conceptual site model and the ISCO design, not only by identifying CVOC contamination but also by eliminating uncontaminated portions of the aquifer from further ISCO consideration. Direct-push injection was selected as the main method of NaMnO4 delivery due to its flexibility and low initial capital cost. Site impediments to ISCO activities in the source area involved subsurface utilities, including a high pressure water main, a high voltage power line, a communication line, and sanitary and stormwater sewer lines. Utility markings were used in conjunction with careful planning and judicious selection of injection locations. A

  13. Determination of oxygen to metal ratio for varying UO2 content in sintered (U,Th)O2 pellet by oxidation-reduction method using thermo-gravimetric analyser

    International Nuclear Information System (INIS)

    Mahanty, B.N.; Khan, F.A.; Karande, A.P.; Prakash, A.; Afzal, Md.; Panakkal, J.P.

    2009-01-01

    Experiments were carried out to determine oxygen to metal ratio in 4%, 6%, 10%, 20%, 50% and 80% UO 2 in sintered (U, Th) O 2 pellets by oxidation-reduction method using thermo gravimetric analyser. (author)

  14. Liquid phase sintered superconducting cermet

    International Nuclear Information System (INIS)

    Ray, S.P.

    1990-01-01

    This patent describes a method of making a superconducting cermet having superconducting properties with improved bulk density, low porosity and in situ stabilization. It comprises: forming a structure of a superconducting ceramic material having the formula RM 2 Cu 3 O (6.5 + x) wherein R is one or more rare earth elements capable of reacting to form a superconducting ceramic, M is one or more alkaline earth metal elements selected from barium and strontium capable of reacting to form a superconducting ceramic, x is greater than 0 and less than 0.5; and a precious metal compound in solid form selected from the class consisting of oxides, sulfides and halides of silver; and liquid phase sintering the mixture at a temperature wherein the precious metal of the precious metal compound is molten and below the melting point of the ceramic material. The liquid phase sintering is carried out for a time less than 36 hours but sufficient to improve the bulk density of the cermet

  15. Studies on frequency dependent electrical and dielectric properties of sintered zinc oxide pellets: effects of Al-doping

    Science.gov (United States)

    Tewari, S.; Ghosh, A.; Bhattacharjee, A.

    2016-11-01

    Sintered pellets of zinc oxide (ZnO), both undoped and Al-doped are prepared through a chemical process. Dopant concentration of Aluminium in ZnO [Al/Zn in weight percentage (wt%)] is varied from 0 to 3 wt%. After synthesis structural characterisation of the samples are performed with XRD and SEM-EDAX which confirm that all the samples are of ZnO having polycrystalline nature with particle size from 108.6 to 116 nm. Frequency dependent properties like a.c. conductivity, capacitance, impedance and phase angle are measured in the frequency range 10 Hz to 100 kHz as a function of temperature (in the range 25-150 °C). Nature of a.c. conductivity in these samples indicates hopping type of conduction arising from localised defect states. The frequency and temperature dependent properties under study are found to be as per correlated barrier hoping model. Dielectric and impedance properties studied in the samples indicate distributed relaxation, showing decrease of relaxation time with temperature.

  16. Laser sintering of copper nanoparticles

    International Nuclear Information System (INIS)

    Zenou, Michael; Saar, Amir; Ermak, Oleg; Kotler, Zvi

    2014-01-01

    Copper nanoparticle (NP) inks serve as an attractive potential replacement to silver NP inks in functional printing applications. However their tendency to rapidly oxidize has so far limited their wider use. In this work we have studied the conditions for laser sintering of Cu-NP inks in ambient conditions while avoiding oxidation. We have determined the regime for stable, low-resistivity copper (< ×3 bulk resistivity value) generation in terms of laser irradiance and exposure duration and have indicated the limits on fast processing. The role of pre-drying conditions on sintering outcome has also been studied. A method, based on spectral reflectivity measurements, was used for non-contact monitoring of the sintering process evolution. It also indicates preferred spectral regions for sintering. Finally, we illustrated how selective laser sintering can generate high-quality, fine line (<5 µm wide) and dense copper circuits. (paper)

  17. Improved Understanding of In Situ Chemical Oxidation. Technical Objective I: Contaminant Oxidation Kinetics Contaminant Oxidation Kinetics

    Science.gov (United States)

    2009-05-01

    methyl tert butyl ether NAPL non-aqueous phase liquid NOD natural oxidant demand •OH hydroxide radical Ox oxidant O3 ozone PCE...and persulfate; and Technical Objective 2, assess how soil properties (e.g., soil mineralogy , natural carbon content) affect oxidant mobility and...to develop a general description of kobs vs. T because there are many reactions that can contribute to the concentration of the reactive intermediate

  18. Influence of Sintering Temperature on the Microstructure and Mechanical Properties of In Situ Reinforced Titanium Composites by Inductive Hot Pressing

    Directory of Open Access Journals (Sweden)

    Cristina Arévalo

    2016-11-01

    Full Text Available This research is focused on the influence of processing temperature on titanium matrix composites reinforced through Ti, Al, and B4C reactions. In order to investigate the effect of Ti-Al based intermetallic compounds on the properties of the composites, aluminum powder was incorporated into the starting materials. In this way, in situ TixAly were expected to form as well as TiB and TiC. The specimens were fabricated by the powder metallurgy technique known as inductive hot pressing (iHP, using a temperature range between 900 °C and 1400 °C, at 40 MPa for 5 min. Raising the inductive hot pressing temperature may affect the microstructure and properties of the composites. Consequently, the variations of the reinforcing phases were investigated. X-ray diffraction, microstructural analysis, and mechanical properties (Young’s modulus and hardness of the specimens were carried out to evaluate and determine the significant influence of the processing temperature on the behavior of the composites.

  19. Effort to improve coupled in situ chemical oxidation with bioremediation: a review of optimization strategies

    NARCIS (Netherlands)

    Sutton, N.B.; Grotenhuis, J.T.C.; Langenhoff, A.A.M.; Rijnaarts, H.H.M.

    2011-01-01

    Purpose - In order to provide highly effective yet relatively inexpensive strategies for the remediation of recalcitrant organic contaminants, research has focused on in situ treatment technologies. Recent investigation has shown that coupling two common treatments-in situ chemical oxidation (ISCO)

  20. In situ Reduction and Oxidation of Nickel from Solid Oxide Fuel Cells in a Transmission Electron Microscope

    DEFF Research Database (Denmark)

    Faes, Antonin; Jeangros, Quentin; Wagner, Jakob Birkedal

    2009-01-01

    Environmental transmission electron microscopy was used to characterize in situ the reduction and oxidation of nickel from a Ni/YSZ solid oxide fuel cell anode support between 300-500{degree sign}C. The reduction is done under low hydrogen pressure. The reduction initiates at the NiO/YSZ interface...

  1. Alternative materials for solid oxide fuel cells: Factors affecting air-sintering of chromite interconnections

    International Nuclear Information System (INIS)

    Chick, L.A.; Bates, J.L.

    1992-01-01

    The purpose of this research is to develop alternative materials for solid oxide fuel cell (SOFC) interconnections and electrodes with improved electrical, thermal and electrochemical properties. Another objective is to develop synthesis and fabrication processes for these materials whereby they can be consolidated in air into SOFC's. The approach is to (1) develop modifications of the current, state-of-the-art materials used in SOFC's, (2) minimize the number of cations used in the SOFC materials to reduce potential deleterious interactions, (3) improve thermal, electrical, and electrochemical properties, (4) develop methods to synthesize both state-of-the-art and alternative materials for the simultaneous fabrication and consolidation in air of the interconnections and electrodes with the solid electrolyte, and (5) understand electrochemical reactions at materials interfaces and the effects of component compositions and processing on those reactions

  2. Flash sintering of ceramic materials

    Science.gov (United States)

    Dancer, C. E. J.

    2016-10-01

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

  3. In situ synthesis of Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite by vacuum sintering mechanically alloyed TiAl powder coated with CNTs

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jian [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Zhao, Naiqin, E-mail: nqzhao@tju.edu.cn [State Key Laboratory of Hydraulic Engineering Simulation and Safety, Tianjin (China); Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China); Nash, Philip [Thermal Processing Technology Center, Illinois Institute of Technology, IL (United States); Liu, Enzuo; He, Chunnian; Shi, Chunsheng; Li, Jiajun [Department of Materials Science and Engineering of Tianjin University, Tianjin Key Laboratory of Composite and Functional Materials, Tianjin 300072 (China)

    2013-11-25

    Highlights: •Using zwitterionic surfactant to enhance the dispersion of the CNTs on the powder surface. •CNTs as carbon source decreased the formation temperature of Ti{sub 2}AlC. •Al{sub 2}O{sub 3} was generated in situ from the oxygen atoms introduced in the drying procedure. •Nanosized Ti{sub 3}Al was precipitated at 1250 °C and distribute in the TiAl matrix homogeneously. •Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composite was synthesized in situ by sintering pre-alloy Ti–Al coated with CNTs. -- Abstract: Bulk Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were in situ synthesized by vacuum sintering mechanically alloyed Ti–50 at.% Al powders coated with carbon nanotubes (CNTs). The pre-alloyed Ti–50 at.% Al powder was obtained by ball milling Ti and Al powders. The multi-walled carbon nanotubes as the carbon resource were covered on the surface of the pre-alloyed powders by immersing them into a water solution containing the CNTs. A zwitterionic surfactant was used to enhance the dispersion of the CNTs on the powder surface. The samples were cold pressed and sintered in vacuum at temperatures from 950 to 1250 °C, respectively. The results show that the reaction of forming Ti{sub 2}AlC can be achieved below 950 °C, which is 150 °C lower than in the Ti–Al–TiC system and 250 °C lower than for the Ti–Al–C system due to the addition of CNTs. Additionally, the reinforcement of Al{sub 2}O{sub 3} particles was introduced in situ in Ti{sub 2}AlC/TiAl by the drying process and subsequent sintering of the composite powders. Dense Ti{sub 2}AlC–Al{sub 2}O{sub 3}/TiAl composites were obtained by sintering at 1250 °C and exhibited a homogeneous distribution of Ti{sub 2}AlC, Al{sub 2}O{sub 3} and precipitated Ti{sub 3}Al particles and a resulting high hardness.

  4. Sintering of Synroc D

    International Nuclear Information System (INIS)

    Robinson, G.

    1982-01-01

    Sintering has been investigated as a method for the mineralization and densification of high-level nuclear defense waste powder. Studies have been conducted on Synroc D composite powder LS04. Optimal densification has been found to be highly dependent on the characteristics of the starting material. Powder subjected to milling, which was believed to reduce the level of agglomeration and possibly particle size, was found to densify better than powder not subjected to this milling. Densities of greater than 95% of theoretical could be achieved for samples sintered at 1150 to 1200 0 C. Mineralogy was found to be as expected for Synroc D for samples sintered in a CO 2 /CO atmosphere where the Fe +2 /Fe +3 ratio was maintained at 1.0 to 5.75. In a more oxidizing, pure CO 2 atmosphere a new phase, not previously identified in Synroc D, was found

  5. On the oxidation behaviour of a Cu-10 vol% Cr in situ composite

    International Nuclear Information System (INIS)

    Haugsrud, R.; Lee, K.L.

    2005-01-01

    The oxidation behaviour of copper and Cu-10 vol% Cr in situ composite was studied at 400-700 deg. C in air and in argon containing 10 ppm O 2 . Oxidation kinetics was investigated by means of isothermal thermogravimetry and the oxide scales were characterized by scanning electron microscopy (SEM). The presence of the chromium fibres increases the oxidation resistance compared to unalloyed copper up to 600 deg. C. The oxidation mechanism and the influence of the different oxidation phenomena on the creep characteristics of the alloy composite are discussed

  6. In-situ formation of complex oxide precipitates during processing of oxide dispersion strengthened ferritic steels

    International Nuclear Information System (INIS)

    Jayasankar, K.; Pandey, Abhishek; Mishra, B.K.; Das, Siddhartha

    2016-01-01

    Highlights: • Use of dual drive planetary ball mill for Bench scale (>1 kg) production. • X-ray diffraction and TEM were used to study transformations during sintering. • HIPped and rolled samples with nearly 99% density successfully produced. - Abstract: In fusion and fission reactor material development, ODS alloys are the most suitable candidate materials due to its high temperature creep properties and irradiation resistance properties. This paper describes the preparation of oxide dispersion strengthened alloy powder in large quantity (>1 kg batch) in dual drive planetary ball mill using pre-alloyed ferrtic steel powder with nano sized Y_2O_3. The consolidation of the powders was carried out in hot isostatic press (HIP) followed by hot rolling. 99% of the theoretical density was achieved by this method. The vickers hardness values of pressed and rolled samples were in the range of 380 ± 2HV and 719 ± 2HV, respectively. Samples were further investigated using X-ray diffraction particle size analyzer and electron microscope. Initial increase in particle size with milling was observed showing flattening of the particle. It was found that 5 h of milling time is sufficient to reduce the particle size to achieve the desired size. Transmission electron microscopy analysis of milled ODS steel powder revealed a uniform distribution of combustion synthesized nano-Y_2O_3 in ferritic steel matrix after a milling time of 5 h. Preliminary results demonstrated suitability of dual drive planetary ball mill for mass production of alloy within a short time due to various kinds of forces acting at a time during milling process. Fine monoclinic Y_2Si_2O_7 precipitates were also observed in the steel. This study explains the particle characteristics of nano Y_2O_3 dispersed ODS powder and formation of nano clusters in ODS ferritic alloy.

  7. Recycling of mill scale in sintering process

    Directory of Open Access Journals (Sweden)

    El-Hussiny N.A.

    2011-01-01

    Full Text Available This investigation deals with the effect of replacing some amount of Baharia high barite iron ore concentrate by mill scale waste which was characterized by high iron oxide content on the parameters of the sintering process., and investigation the effect of different amount of coke breeze added on sintering process parameters when using 5% mill scale waste with 95% iron ore concentrate. The results of this work show that, replacement of iron ore concentrate with mill scale increases the amount of ready made sinter, sinter strength and productivity of the sinter machine and productivity at blast furnace yard. Also, the increase of coke breeze leads to an increase the ready made sinter and productivity of the sintering machine at blast furnace yard. The productivity of the sintering machine after 5% decreased slightly due to the decrease of vertical velocity.

  8. Oxidation kinetics of Si and SiGe by dry rapid thermal oxidation, in-situ steam generation oxidation and dry furnace oxidation

    Science.gov (United States)

    Rozé, Fabien; Gourhant, Olivier; Blanquet, Elisabeth; Bertin, François; Juhel, Marc; Abbate, Francesco; Pribat, Clément; Duru, Romain

    2017-06-01

    The fabrication of ultrathin compressively strained SiGe-On-Insulator layers by the condensation technique is likely a key milestone towards low-power and high performances FD-SOI logic devices. However, the SiGe condensation technique still requires challenges to be solved for an optimized use in an industrial environment. SiGe oxidation kinetics, upon which the condensation technique is founded, has still not reached a consensus in spite of various studies which gave insights into the matter. This paper aims to bridge the gaps between these studies by covering various oxidation processes relevant to today's technological needs with a new and quantitative analysis methodology. We thus address oxidation kinetics of SiGe with three Ge concentrations (0%, 10%, and 30%) by means of dry rapid thermal oxidation, in-situ steam generation oxidation, and dry furnace oxidation. Oxide thicknesses in the 50 Å to 150 Å range grown with oxidation temperatures between 850 and 1100 °C were targeted. The present work shows first that for all investigated processes, oxidation follows a parabolic regime even for thin oxides, which indicates a diffusion-limited oxidation regime. We also observe that, for all investigated processes, the SiGe oxidation rate is systematically higher than that of Si. The amplitude of the variation of oxidation kinetics of SiGe with respect to Si is found to be strongly dependent on the process type. Second, a new quantitative analysis methodology of oxidation kinetics is introduced. This methodology allows us to highlight the dependence of oxidation kinetics on the Ge concentration at the oxidation interface, which is modulated by the pile-up mechanism. Our results show that the oxidation rate increases with the Ge concentration at the oxidation interface.

  9. Microbial dynamics during and after in situ chemical oxidation of chlorinated solvents

    NARCIS (Netherlands)

    Sutton, N.B.; Atashgahi, S.; Wal, van der J.; Wijn, G.; Grotenhuis, J.T.C.; Smidt, H.; Rijnaarts, H.

    2015-01-01

    In situ chemical oxidation (ISCO) followed by a bioremediation step is increasingly being considered as an effective biphasic technology. Information on the impact of chemical oxidants on organohalide respiring bacteria (OHRB), however, is largely lacking. Therefore, we used quantitative PCR (qPCR)

  10. Sintering Theory and Practice

    Science.gov (United States)

    German, Randall M.

    1996-01-01

    process all around us--in manufactured objects from metals, ceramics, polymers, and many compounds. From a vast professional literature, Sintering Theory and Practice emerges as the only comprehensive, systematic, and self-contained volume on the subject. Covering all aspects of sintering as a processing topic, including materials, processes, theories, and the overall state of the art, the book Offers numerous examples, illustrations, and tables that detail actual processing cycles, and that stress existing knowledge in the field Uses the specifics of various consolidation cycles to illustrate the basics Leads the reader from the fundamentals to advanced topics, without getting bogged down in various mathematical disputes over treatments and measurements Supports the discussion with critically selected references from thousands of sources Examines the sintering behavior of a wide variety of engineered materials--metals, alloys, oxide ceramics, composites, carbides, intermetallics, glasses, and polymers Guides the reader through the sintering processes for several important industrial materials and demonstrates how to control these processes effectively and improve present techniques Provides a helpful reference for specific information on materials, processing problems, and concepts For practitioners and researchers in ceramics, powder metallurgy, and other areas, and for students and faculty in materials science and engineering, this book provides the know-how and understanding crucial to many industrial operations, offers many ideas for further research, and suggests future applications of this important technology. This book offers an unprecedented opportunity to explore sintering in both practical and theoretical terms, whether at the lab or in real-world applications, and to acquire a broad, yet thorough, understanding of this important technology.

  11. Performance of in situ chemical oxidation field demonstrations at DOE sites

    International Nuclear Information System (INIS)

    Cline, S.R.; West, O.R.; Siegrist, R.L.; Holden, W.L.

    1997-01-01

    Researchers at the Oak Ridge National Laboratory (ORNL) have been investigating the use of in situ chemical oxidation to remediate organic contaminants (VOCs, SVOCs, and PCBs) in soils and groundwater at the laboratory and field scales. Field scale design parameters (e.g., oxidant loading rates and oxidant delivery techniques) are often dictated by site conditions (e.g., soil properties and initial contaminant concentrations). Chemical destruction of organic compounds can be accomplished using a variety of oxidants. Recent research has involved field scale in situ chemical oxidation demonstrations using H 2 O 2 and KMnO 4 in conjunction with soil mixing as the oxidant delivery mechanism. A description of some of these fields activities and future field-scale work is presented here

  12. Characterization of In-Situ Cu–TiH2–C and Cu–Ti–C Nanocomposites Produced by Mechanical Milling and Spark Plasma Sintering

    Directory of Open Access Journals (Sweden)

    Nguyen Thi Hoang Oanh

    2017-03-01

    Full Text Available This study focuses on the fabrication and microstructural investigation of Cu–TiH2–C and Cu–Ti–C nanocomposites with different volume fractions (10% and 20% of TiC. Two mixtures of powders were ball milled for 10 h, consequently consolidated by spark plasma sintering (SPS at 900 and 1000 °C producing bulk materials with relative densities of 95–97%. The evolution process of TiC formation during sintering process was studied by using X-ray diffraction (XRD, scanning electron microscopy (SEM, and high resolution transmission electron microscopy (HRTEM. XRD patterns of composites present only Cu and TiC phases, no residual Ti phase can be detected. TEM images of composites with (10 vol % TiC sintered at 900 °C show TiC nanoparticles about 10–30 nm precipitated in copper matrix, most of Ti and C dissolved in the composite matrix. At the higher sintering temperature of 1000 °C, more TiC precipitates from Cu–TiH2–C than those of Cu–Ti–C composite, particle size ranges from 10 to 20 nm. The hardness of both nanocomposites also increased with increasing sintering temperature. The highest hardness values of Cu–TiH2–C and Cu–Ti–C nanocomposites sintered at 1000 °C are 314 and 306 HV, respectively.

  13. Manufacture of sintered bricks of high density from beryllium oxide; Fabrication de frittes de forte densite a base d'oxyde de beryllium

    Energy Technology Data Exchange (ETDEWEB)

    Pointud, R; Rispal, Ch; Le Garec, M [Commissariat a l' Energie Atomique, Saclay (France).Centre d' Etudes Nucleaires

    1959-07-01

    Beryllium oxide bricks of nuclear purity 100 x 100 x 50 and 100 x 100 x 100 mm of very high density (between 2.85 and 3.00) are manufactured by sintering under pressure in graphite moulds at temperatures between 1,750 and 1,850 deg. C, and under a pressure of 150 kg/cm{sup 2}. The physico-chemical state of the saw material is of considerable importance with regard to the success of the sintering operation. In addition, a study of the sintering of a BeO mixture with 3 to 5 per cent of boron introduced in the form of boric acid, boron carbide or elementary boron shows that high densities can only be obtained by sintering under pressure. For technical reasons of manufacture, only the mixture based on boron carbide is used. The sintering is carried out in graphite moulds at 1500 deg. C under 150 kg/cm{sup 2} pressure, and bricks can be obtained with density between 2,85 and 2,90. Laboratory studies and the industrial manufacture of various sinters are described in detail. (author) [French] La fabrication de briques d'oxyde de beryllium de purete nucleaire de 100 x 100 x 50 et de 100 x 100 x 100 mm de densite tres elevee (comprise entre 2.85 et 3.00) est realisee par frittage sous charge dans des moules en graphite entre 1750 et 1850 deg. C, sous 150 kg/cm{sup 2} de pression. L'etat physico-chimique de la matiere premiere a une importance considerable quant au succes de l'operation de frittage. Par ailleurs, l'etude du frittage du mixte BeO a 3 et 5 pour cent de bore element introduit sous forme d'anhydride borique, soit de carbure de bore ou de bore element, montre que seul le frittage sous charge permet d'obtenir des densites elevees. Pour des raisons techniques de fabrication seul le mixte a base de carbure de bore est retenu. Le frittage s'opere dans des moules de graphite a 1500 deg. C sous 150 kg/cm{sup 2} de pression et permet d'obtenir des briques de densite comprise entre 2.85 et 2.90. Les etudes de laboratoire et la fabrication industrielle des differents

  14. Sintering and Electrical Characterization of La and Nb Co‐doped SrTiO3 Electrode Materials for Solid Oxide Cell Applications

    DEFF Research Database (Denmark)

    Sudireddy, Bhaskar Reddy; Agersted, Karsten

    2014-01-01

    Single‐phase lanthanum and niobium co‐doped strontium titanate (Sr1–3x/2LaxTi0.9Nb0.1O3; x = 0–0.02) ceramics were prepared. Dilatometry in reducing atmosphere showed an increase in the sintering rate and sintered density with an increase in La amount. Microscopy of fractured surfaces of sintered...... samples showed that the average grain size increased drastically in reducing conditions with increasing La content (and associated A‐site vacancies). By incorporating 2 mol.% La, the electronic conductivity significantly improved from 80 to 135 S cm−1 at 1,000 °C, and even larger improvements were...... observed at lower temperatures. These observations demonstrate the flexibility in tailoring the microstructure and electronic transport properties by doping small amounts of La into the Nb‐doped SrTiO3 and show that Sr1–3x/2LaxTi0.9Nb0.1O3 is a potential electrode material for solid oxide cells....

  15. In Situ Raman Spectroscopy of Supported Chromium Oxide Catalysts: Reactivity Studies with Methanol and Butane

    NARCIS (Netherlands)

    Weckhuysen, B.M.; Wachs, I.E.

    1996-01-01

    The interactions of methanol and butane with supported chromium oxide catalysts under oxidizing and reducing conditions were studied by in situ Raman spectroscopy as a function of the specific oxide support (Al2O3, ZrO2, TiO2, SiO2, Nb2O5, 3% SiO2/TiO2, 3% TiO2/SiO2, and a physical mixture of SiO2

  16. In situ deposition of thallium-containing oxides

    International Nuclear Information System (INIS)

    Myers, K.E.

    1996-01-01

    The number and variety of thallium based materials that can be made by in situ methods have grown consistently since the first report of successful thallium cuprate deposition by Face and Nestlerode in 1992. Processes for the deposition of superconductors, normal metals, and insulators have been developed. Most work to date has been done on the Tl-1212 phases, TlBa 2 CaCu 2 O 7 and (Tl,Pb)Sr 2 CaCu 2 O 7 . Recently however, the in situ thallium technique has been extended to other materials. For example, epitaxial thin films of thallium tantalate, an insulator of the pyrochlore structure and a potential buffer layer for thallium cuprate films, have been grown. Multilayers, important in the fabrication of Josephson junctions, have been demonstrated with the thallium lead cuprates. This paper reviews progress in the area of in situ thallium deposition technology which will make more complex thallium cuprate multilayer structures and devices possible

  17. Preparation of a sinterable beryllium oxide through decomposition of beryllium hydroxide (1963); Preparation d'un oxyde de beryllium frittable par decomposition de l'hydiloxyde (1963)

    Energy Technology Data Exchange (ETDEWEB)

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

    1963-07-01

    In the course of the present study, we have attempted to precise the factors which among the ones effective in the course of the preparation of the beryllium hydroxide and oxide and during the sintering have an influence on the final result: the density and homogeneity of the sintered body. Of the several varieties of hydroxides precipitated from a sulfate solution the {beta}-hydroxide only is always contaminated with beryllium sulfate and cannot be purified even by thorough washing. We noticed that those varieties of the hydroxide (gel, {alpha}, {beta}) have different decomposition rates; this behaviour is used to identify and even to dose the different species in ({alpha}, {beta}) mixtures. The various hydroxides transmit to the resulting oxides the shape they had when precipitated. Accordingly the history of the oxide is revealed by its behaviour during its fabrication and sintering. By comparing the results of the sintering operation with the various measurements performed on the oxide powders we are led to the conclusion that an oxide obtained from beryllium hydroxide is sinterable under vacuum if the following conditions are fulfilled: the particle size must lie between 0.1 and 0.2 {mu} and the BeSO{sub 4} content of the powder must be less than 0.25 per cent wt (expressed as SO{sub 3}/BeO). The best fitting is obtained with the oxide issued from an {alpha}-hydroxide precipitated as very small aggregates and with a low sulfur-content. We have observed that this is also the case for the oxide obtained by direct calcination of beryllium sulfate. (author) [French] Au cours de cette etude, nous avons cherche a preciser les facteurs qui, intervenant tout au long de la preparation de l'hydroxyde, puis de l'oxyde de beryllium et enfin du frittage, peuvent avoir une influence sur le resultat final: la densite et l'homogeneite du fritte. Parmi tous les hydroxydes precipites d'une solution de sulfate, seul l'hydroxyde {beta} est toujours fortement pollue par le sulfate

  18. Method of sintering ceramic materials

    Science.gov (United States)

    Holcombe, Cressie E.; Dykes, Norman L.

    1992-01-01

    A method for sintering ceramic materials is described. A ceramic article is coated with layers of protective coatings such as boron nitride, graphite foil, and niobium. The coated ceramic article is embedded in a container containing refractory metal oxide granules and placed within a microwave oven. The ceramic article is heated by microwave energy to a temperature sufficient to sinter the ceramic article to form a densified ceramic article having a density equal to or greater than 90% of theoretical density.

  19. Novel iron oxide-silica coreshell powders compacted by using pulsed electric current sintering: optical and magnetic properties

    Czech Academy of Sciences Publication Activity Database

    Mahmed, N.; Heczko, Oleg; Maki, R.; Söderberg, O.; Haimi, E.; Hannula, S.-P.

    2012-01-01

    Roč. 32, č. 11 (2012), s. 2981-2988 ISSN 0955-2219 Institutional research plan: CEZ:AV0Z10100520 Keywords : sintering * SiO 2 * ferrites * grain growth * transparent Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.360, year: 2012 http://www.sciencedirect.com/science/article/pii/S0955221912001240

  20. Liquid crystalline polymer nanocomposites reinforced with in-situ reduced graphene oxide

    Directory of Open Access Journals (Sweden)

    D. Pedrazzoli

    2015-08-01

    Full Text Available In this work liquid-crystalline polymer (LCP nanocomposites reinforced with in-situ reduced graphene oxide are investigated. Graphene oxide (GO was first synthesized by the Hummers method, and the kinetics of its thermal reduction was assessed. GO layers were then homogeneously dispersed in a thermotropic liquid crystalline polymer matrix (Vectran®, and an in-situ thermal reduction of GO into reduced graphene oxide (rGO was performed. Even at low rGO amount, the resulting nanocomposites exhibited an enhancement of both the mechanical properties and the thermal stability. Improvements of the creep stability and of the thermo-mechanical behavior were also observed upon nanofiller incorporation. Furthermore, in-situ thermal reduction of the insulating GO into the more electrically conductive rGO led to an important surface resistivity decrease in the nanofilled samples.

  1. Mechanical, tribological and biological properties of novel 45S5 Bioglass® composites reinforced with in situ reduced graphene oxide.

    Science.gov (United States)

    Li, Zhong; Khun, Nay Win; Tang, Xiu-Zhi; Liu, Erjia; Khor, Khiam Aik

    2017-01-01

    45S5 Bioglass ® (45S5) is one of the most widely used biomaterials in ceramic-based bone graft substitutes by virtue of its excellent biocompatibility and bioactivity. However, the fracture toughness and wear resistance of 45S5 have to be improved to extend its applications in load bearing orthopedic implants. The current study reports the first use of graphene nanoplatelet (GNP) to enhance the fracture toughness and wear resistance of 45S5. Composite powders with four different loadings of graphene oxide (GO), i.e. 0, 0.1, 0.5 and 1wt%, were sintered by spark plasma sintering (SPS) at a relatively low temperature of 550°C, during which in situ thermal reduction of GO took place. It was found that by adding 0.5wt% GO to the 45S5 powder, the fracture toughness of the sintered pellets was increased by 130.2% while friction coefficient and specific wear rate were decreased by 21.3% and 62.0%, respectively. Furthermore, the viability of MG63 cells grown on the GNP-incorporated pellets was comparably high to that of the cells grown on the pure 45S5 pellets. As compared with the pure 45S5 leachates, the media conditioned by the GNP/45S5 pellets fabricated from the composite powder with 1wt% GO could enhance both the proliferation and viability of MG63 cells. It is thus envisioned that the GNP-reinforced 45S5 is a highly promising material for fabricating mechanically strong and biocompatible load-bearing bone implants. Copyright © 2016 Elsevier Ltd. All rights reserved.

  2. Evidence against the nuclear in situ binding of arsenicals-oxidative stress theory of arsenic carcinogenesis

    International Nuclear Information System (INIS)

    Kitchin, Kirk T.; Wallace, Kathleen

    2008-01-01

    A large amount of evidence suggests that arsenicals act via oxidative stress in causing cancer in humans and experimental animals. It is possible that arsenicals could bind in situ close to nuclear DNA followed by Haber-Weiss type oxidative DNA damage. Therefore, we tested this hypothesis by using radioactive 73 As labeled arsenite and vacuum filtration methodology to determine the binding affinity and capacity of 73 As arsenite to calf thymus DNA and Type 2A unfractionated histones, histone H3, H4 and horse spleen ferritin. Arsenicals are known to release redox active Fe from ferritin. At concentrations up to about 1 mM, neither DNA nor any of the three proteins studied, Type II-A histones, histone H3, H4 or ferritin, bound radioactive arsenite in a specific manner. Therefore, it appears highly unlikely that initial in situ binding of trivalent arsenicals, followed by in situ oxidative DNA damage, can account for arsenic's carcinogenicity. This experimental evidence (lack of arsenite binding to DNA, histone Type II-A and histone H3, H4) does not rule out other possible oxidative stress modes of action for arsenic such as (a) diffusion of longer lived oxidative stress molecules, such as H 2 O 2 into the nucleus and ensuing oxidative damage, (b) redox chemistry by unbound arsenicals in the nucleus, or (c) arsenical-induced perturbations in Fe, Cu or other metals which are already known to oxidize DNA in vitro and in vivo

  3. Ex-Situ and In-Situ Ellipsometric Studies of the Thermal Oxide on InP

    Science.gov (United States)

    1990-12-06

    ion---- Distribution/ Availabilit ? Codes£v l llt Codes Avail and/or Dist| Special Abstract The thermally grown InP oxide as etched by an aqueous...aqueous NH4OH/NH4F, and Law(17) has reported observations of orientational ordering of water and organic solvents on pyrex surfaces by in-situ...minutes, followed by a sequence of acetone, deionized water (d. i. water ) rinse. After being dipped in a concentrated aqueous HF solution for 15 seconds

  4. Freeform Fabrication of Magnetophotonic Crystals with Diamond Lattices of Oxide and Metallic Glasses for Terahertz Wave Control by Micro Patterning Stereolithography and Low Temperature Sintering

    Directory of Open Access Journals (Sweden)

    Maasa Nakano

    2013-04-01

    Full Text Available Micrometer order magnetophotonic crystals with periodic arranged metallic glass and oxide glass composite materials were fabricated by stereolithographic method to reflect electromagnetic waves in terahertz frequency ranges through Bragg diffraction. In the fabrication process, the photo sensitive acrylic resin paste mixed with micrometer sized metallic glass of Fe72B14.4Si9.6Nb4 and oxide glass of B2O3·Bi2O3 particles was spread on a metal substrate, and cross sectional images of ultra violet ray were exposed. Through the layer by layer stacking, micro lattice structures with a diamond type periodic arrangement were successfully formed. The composite structures could be obtained through the dewaxing and sintering process with the lower temperature under the transition point of metallic glass. Transmission spectra of the terahertz waves through the magnetophotonic crystals were measured by using a terahertz time domain spectroscopy.

  5. Brush-Painting and Photonic Sintering of Copper Oxide and Silver Inks on Wood and Cardboard Substrates to Form Antennas for UHF RFID Tags

    Directory of Open Access Journals (Sweden)

    Erja Sipilä

    2016-01-01

    Full Text Available Additive deposition of inks with metallic inclusions provides compelling means to embed electronics into versatile structures. The need to integrate electronics into environmentally friendly components and structures increases dramatically together with the increasing popularity of the Internet of Things. We demonstrate a novel brush-painting method for depositing copper oxide and silver inks directly on wood and cardboard substrates and discuss the optimization of the photonic sintering process parameters for both materials. The optimized parameters were utilized to manufacture passive ultra high frequency (UHF radio frequency identification (RFID tag antennas. The results from wireless testing show that the RFID tags based on the copper oxide and silver ink antennas on wood substrate are readable from ranges of 8.5 and 11 meters, respectively, and on cardboard substrate from read ranges of 8.5 and 12 meters, respectively. These results are well sufficient for many future wireless applications requiring remote identification with RFID.

  6. In-situ oxidation study of Pd(100) by surface x-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Kilic, Volkan; Franz, Dirk; Stierle, Andreas [AG Grenzflaechen, Universitaet Siegen (Germany); Martin, Natalia; Lundgren, Edvin [Department of Synchrotron Radiation Research, Lund University (Sweden); Mantilla, Miguel [MPI fuer Metallforschung, Stuttgart (Germany)

    2011-07-01

    The oxidation of the Pd(100) surface at oxygen pressures in the 10{sup -6} mbar to 10{sup 3} mbar range and temperatures up to 1000 K has been studied in-situ by surface x-ray diffraction (SXRD). The SXRD experiments were performed at the MPI beamline at the Angstrom Quelle Karlsruhe (ANKA). We present the surface and crystal truncation rod (CTR) data from the ({radical}(5) x {radical}(5)) surface layer. We show that the transformation from the surface oxide to PdO bulk oxide can be observed in-situ under specific pressure and temperature conditions. We compare our results with previously proposed structure models based on low energy electron diffraction (LEED) I(V) curves and density functional theory calculations. Finally, we elucidate the question of commensurability of the surface oxide layer with respect to the Pd(100) substrate.

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

    Science.gov (United States)

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

    2009-11-01

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

  8. In Situ Chemical Oxidation Using Potassium Permanganate. Innovative Technology Summary Report

    International Nuclear Information System (INIS)

    1999-01-01

    The In Situ Chemical Oxidation Using Potassium Permanganate [KMnO4] treats soils or groundwater contaminated with a range of organic chemicals, including trichlorethylene. Potential application to metal and radionuclide contaminants, including oxidation/immobilization of uranium, is being investigated. This technology is designed for use with efficient delivery systems, such as the Multi-Point Injection System and Deep Soil Mixing, to treat contaminants in low permeability soils

  9. Heterogeneous burnable poisons. Sinterability study in oxidizing atmosphere of alumina-gadolinia and alumina-boron carbide compounds

    International Nuclear Information System (INIS)

    Agueda, H.C.; Leiva, S.F.; Russo, D.O.

    1990-01-01

    Solid burnable poisons are used in reactors cooled by pressure light water (PLWR) with the purpose of controlling initial reactivity in the first reactor's core. The burnable poisons may be uniformly mixed with the fuel -known as 'homogeneous' poisons-; or constituting separate elements -known as heterogeneous poisons-. The purpose of this work is to present the results of two sinterability studies, performed on Al 2 O 3 -Gd 2 O 3 and Al 2 O 3 -B 4 C, where alumina acts as inert matrix, storing the absorbing elements as Gd 2 O 3 or B 4 C. The elements were sintered at an air atmosphere and additives permitting the obtention of a greater density alumina were tested at lower temperatures than the characteristic for this material, in order to determine its compatibility with the materials dealt with herein. (Author) [es

  10. Discrimination symbol applying method for sintered nuclear fuel product

    International Nuclear Information System (INIS)

    Ishizaki, Jin

    1998-01-01

    The present invention provides a symbol applying method for applying discrimination information such as an enrichment degree on the end face of a sintered nuclear product. Namely, discrimination symbols of information of powders are applied by a sintering aid to the end face of a molded member formed by molding nuclear fuel powders under pressure. Then, the molded product is sintered. The sintering aid comprises aluminum oxide, a mixture of aluminum oxide and silicon dioxide, aluminum hydride or aluminum stearate alone or in admixture. As an applying means of the sintering aid, discrimination symbols of information of powders are drawn by an isostearic acid on the end face of the molded product, and the sintering aid is sprayed thereto, or the sintering aid is applied directly, or the sintering aid is suspended in isostearic acid, and the suspension is applied with a brush. As a result, visible discrimination information can be applied to the sintered member easily. (N.H.)

  11. Influence of sintering parameters in the ferroelectric properties os strontium bismuth tantalate samples obtained by oxide mixture

    International Nuclear Information System (INIS)

    Souza, R.R. de; Pereira, A.S.; Sousa, V.C.; Egea, J.R.J.

    2012-01-01

    The family of compounds layered-type perovskite, know as Aurivilius presents great alternative not only by the absence of lead in the composition, but because the polarization retention, replacing PZT in FeRAM devices. The strontium bismuth tantalate (SrBi 2 Ta 2 O 9 ) or SBT is ferroelectric material that has attracted considerable interest, since it has high fatigue resistance, supporting high hysteresis loops, with the change in polarization.Checking polarization and depolarization currents stimulated by temperature it is possible to obtain, for example, information about the nature of charges and about the activation energy for the process of dielectric relaxation. For analysis of ferroelectric properties of this compound, it is essential to obtain specimens with a relative density around 95%. Thus, it is important the optimization of the sintering process in order to obtain a ceramic body with a high densification. The influence of sintering parameters to obtain SrBi 2 Ta 2 O 9 in the polarization properties and in the microstructure of sintered samples was investigated by thermostimulated currents and electronic microscopy, respectively. Results show that variation of these parameters may cause changes in the ferroelectric properties of the material. (author)

  12. A comparison between different oxide dispersion strengthened ferritic steel ongoing in situ oxide dissolution in High Voltage Electron Microscope

    International Nuclear Information System (INIS)

    Monnet, I.; Van den Berghe, T.; Dubuisson, Ph.

    2012-01-01

    ODS materials are considered for nuclear applications but previous experimental studies have shown a partial dissolution of some oxides under neutron irradiation. In this work, electron irradiations were used to evaluate the stability of the oxides depending on the chemical composition of the oxide dispersion. Four ferritic steels based on EM10 (Fe–9Cr–1Mo) and reinforced respectively by Al 2 O 3 , MgO, MgAl 2 O 4 and Y 2 O 3 , were studied. These materials were irradiated with 1 MeV or 1.2 MeV electrons in a High Voltage Electron Microscope. This technique allows to follow one single oxide and to determine the evolution of its size during the irradiation. In situ HVEM observations indicate that the dissolution rate depends on the chemical composition of the oxide, on the temperature and on the irradiation dose.

  13. Polyacrylamide grafting of modified graphene oxides by in situ free radical polymerization

    International Nuclear Information System (INIS)

    Tang, Mingyi; Xu, Xiaoyang; Wu, Tao; Zhang, Sai; Li, Xianxian; Li, Yi

    2014-01-01

    Highlights: • Graphene oxide (GO) was modified by chemical reactions to functionalized GO (FGO). • The FGOs and the GO were then subjected to in situ free radical polymerization. • Hydroxyl groups of GO were the most reactive grafting sites. - Abstract: Graphene oxide (GO) was modified using chemical reactions to obtain three types of functionalized GO sheets (FGO). The FGO sheets and the GO were then subjected to in situ free radical polymerization in order to study the grafting polymerization. The FGO and grafted-.FGO were analyzed with Fourier transform infrared spectroscopy, scanning electronic microscopy, thermo-gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS). The grafting percentages in the materials were calculated using the TGA and XPS results. The FGO sheets with different functional groups exhibited different grafting abilities, and hydroxyl groups were proven to be the most reactive grafting sites for the in situ free radical grafting polymerization of polyacrylamide

  14. Polyacrylamide grafting of modified graphene oxides by in situ free radical polymerization

    Energy Technology Data Exchange (ETDEWEB)

    Tang, Mingyi [Department of Applied Chemistry, School of Science, Tianjin University of Commerce, Tianjin 300134 (China); Xu, Xiaoyang, E-mail: xiaoyangxu2012@163.com [School of Science, Tianjin University, Tianjin 30072 (China); Wu, Tao [School of Science, Tianjin University, Tianjin 30072 (China); Zhang, Sai; Li, Xianxian [Department of Applied Chemistry, School of Science, Tianjin University of Commerce, Tianjin 300134 (China); Li, Yi, E-mail: liyi@tju.edu.cn [School of Science, Tianjin University, Tianjin 30072 (China)

    2014-12-15

    Highlights: • Graphene oxide (GO) was modified by chemical reactions to functionalized GO (FGO). • The FGOs and the GO were then subjected to in situ free radical polymerization. • Hydroxyl groups of GO were the most reactive grafting sites. - Abstract: Graphene oxide (GO) was modified using chemical reactions to obtain three types of functionalized GO sheets (FGO). The FGO sheets and the GO were then subjected to in situ free radical polymerization in order to study the grafting polymerization. The FGO and grafted-.FGO were analyzed with Fourier transform infrared spectroscopy, scanning electronic microscopy, thermo-gravimetric analysis (TGA) and X-ray photoelectron spectroscopy (XPS). The grafting percentages in the materials were calculated using the TGA and XPS results. The FGO sheets with different functional groups exhibited different grafting abilities, and hydroxyl groups were proven to be the most reactive grafting sites for the in situ free radical grafting polymerization of polyacrylamide.

  15. Guidelines for active spreading during in situ chemical oxidation to remediate contaminated groundwater

    Science.gov (United States)

    The effectiveness of in situ chemical oxidation to remediate contaminated aquifers depends on the extent and duration of contact between the injected treatment chemical and the groundwater contaminant (the reactants). Techniques that inject and extract in the aquifer to ‘ac...

  16. XPERT DESIGN AND DIAGNOSTICS' (XDD) IN-SITU CHEMICAL OXIDATION PROCESS USING POTASSIUM PERMANGANATE (KMNO4)

    Science.gov (United States)

    Xpert Design and Diagnostic's (XDD)potassium permanganate in situ chemical oxidation (ISCO) process was evaluated under the EPA Superfund Innovative Technology Evaluation (SITE) Program at the former MEC Building site located in Hudson, New Hampshire. At this site, both soil and ...

  17. Oriented Arrays of Graphene in a Polymer Matrix by in situ Reduction of Graphite Oxide Nanosheets

    KAUST Repository

    Ansari, Seema; Kelarakis, Antonios; Estevez, Luis; Giannelis, Emmanuel P.

    2010-01-01

    Graphite oxide-Nafion hybrids with a high degree of alignment are cast from aqueous solution in the absence of any external field and reduced in situ by exposure to hydrazine to produce graphene-Nafion hybrids. Dramatic enhancement of electrical

  18. In-situ measurement of the electrical conductivity of aluminum oxide in HFIR

    Energy Technology Data Exchange (ETDEWEB)

    Zinkle, S.J.; White, D.P.; Snead, L.L. [Oak Ridge National Lab., TN (United States)] [and others

    1996-10-01

    A collaborative DOE/Monbusho irradiation experiment has been completed which measured the in-situ electrical resistivity of 12 different grades of aluminum oxide during HFIR neutron irradiation at 450{degrees}C. No evidence for bulk RIED was observed following irradiation to a maximum dose of 3 dpa with an applied dc electric field of 200 V/mm.

  19. In situ hydrogenation of molybdenum oxide nanowires for enhanced supercapacitors

    KAUST Repository

    Shakir, Imran

    2014-01-01

    In situ hydrogenation of orthorhombic molybdenum trioxide (α-MoO 3) nanowires has been achieved on a large scale by introducing alcohol during the hydrothermal synthesis for electrochemical energy storage supercapacitor devices. The hydrogenated molybdenum trioxide (H xMoO3) nanowires yield a specific capacitance of 168 F g-1 at 0.5 A g-1 and maintain 108 F g-1 at 10 A g-1, which is 36-fold higher than the capacitance obtained from pristine MoO3 nanowires at the same conditions. The electrochemical devices made with HxMoO3 nanowires exhibit excellent cycling stability by retaining 97% of their capacitance after 3000 cycles due to an enhanced electronic conductivity and increased density of hydroxyl groups on the surface of the MoO3 nanowires. This journal is © The Royal Society of Chemistry.

  20. Improved Understanding of In Situ Chemical Oxidation Soil Reactivity

    Science.gov (United States)

    2007-12-01

    followed by a mixture of nitric and perchloric acids . This sequence uses precise heat ramping and holding cycles which takes the sample to dryness...release different kinds of products (e.g., benzenepolycarboxylic acids , phenolic acids , and fatty acids ) with varying resistance to the attack of... oxalate might be the only organic product in the oxidation of humic and non-humic soils by permanganate or even hydrogen peroxide (Harada and Inoko

  1. In situ polymerization of highly dispersed polypyrrole on reduced graphite oxide for dopamine detection.

    Science.gov (United States)

    Qian, Tao; Yu, Chenfei; Wu, Shishan; Shen, Jian

    2013-12-15

    A composite consisting of reduced graphite oxide and highly dispersed polypyrrole nanospheres was synthesized by a straightforward technique, by in situ chemical oxidative polymerization. The novel polypyrrole nanospheres can prevent the aggregation of reduced graphite oxide sheets by electrostatic repulsive interaction, and enhance their electrochemical properties in the nano-molar measurement of dopamine in biological systems with a linear range of 1-8000 nM and a detection limit as low as 0.3 nM. © 2013 Elsevier B.V. All rights reserved.

  2. Gas-phase advanced oxidation for effective, efficient in situ control of pollution

    DEFF Research Database (Denmark)

    Johnson, Matthew Stanley; Nilsson, Elna Johanna Kristina; Svensson, Erik Anders

    2014-01-01

    In this article, gas-phase advanced oxidation, a new method for pollution control building on the photo-oxidation and particle formation chemistry occurring in the atmosphere, is introduced and characterized. The process uses ozone and UV-C light to produce in situ radicals to oxidize pollution......, generating particles that are removed by a filter; ozone is removed using a MnO2 honeycomb catalyst. This combination of in situ processes removes a wide range of pollutants with a comparatively low specific energy input. Two proof-of-concept devices were built to test and optimize the process...... particulate mass. Secondary pollution including formaldehyde and ultrafine particles might be generated, depending on the composition of the primary pollution....

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

    International Nuclear Information System (INIS)

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

    2017-01-01

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

  4. Mechanical characteristics of microwave sintered silicon carbide

    Indian Academy of Sciences (India)

    In firing of products by conventionally sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered silicon carbide by such a method is a useful material for a varieties of applications ranging from kiln furniture to membrane material.

  5. The effects of additives on the microstructure and sinterability of molybdenum oxide - study of related solid solutions

    International Nuclear Information System (INIS)

    Kassem, M.

    2006-01-01

    This study focuses on the phase transformation induced during mixing a fixed quantity of MoO 3 with various concentration of V 2 O 5 , Bn 2 O 5 , Al 2 O 3 and pure aluminium. These concentrations are 2, 3, 4, 5, 10, 20, 40 and 50%. Employing several physical techniques such as x-ray powder diffraction, FTIR and DTA, different solid solution were identified. Also the compressibility and sintering of these solid solutions have been studied via the variation of the density of pellets prepared from these solid solutions (Author)

  6. Iron oxide/cassava starch-supported Ziegler-Natta catalysts for in situ ethylene polymerization.

    Science.gov (United States)

    Chancharoenrith, Sittikorn; Kamonsatikul, Choavarit; Namkajorn, Montree; Kiatisevi, Supavadee; Somsook, Ekasith

    2015-03-06

    Iron oxide nanoparticles were used as supporters for in situ polymerization to produce polymer nanocomposites with well-dispersed fillers in polymer matrix. Iron oxide could be sustained as colloidal solutions by cassava starch to produce a good dispersion of iron oxide in the matrix. New supports based on iron oxide/cassava starch or cassava starch for Ziegler-Natta catalysts were utilized as heterogeneous supporters for partially hydrolyzed triethylaluminum. Then, TiCl4 was immobilized on the supports as catalysts for polymerization of ethylene. High-density polyethylene (HDPE) composites were obtained by the synthesized catalysts. A good dispersion of iron oxide/cassava starch particles was observed in the synthesized polymer matrix promoting to good mechanical properties of HDPE. Copyright © 2014 Elsevier Ltd. All rights reserved.

  7. A field-scale test of in situ chemical oxidation through recirculation

    International Nuclear Information System (INIS)

    West, O.R.; Cline, S.R.; Holden, W.L.; Gardner, F.G.; Schlosser, B.M.; Siegrist, R.L.; Houk, T.C.

    1998-01-01

    In situ chemical oxidation is a developing class of remediation technologies in which organic contaminants are degraded in place by powerful oxidants. Successful implementation of this technology requires an effective means for dispersing the oxidant to contaminated regions in the subsurface. An oxidant delivery technique has been developed wherein the treatment solution is made by adding an oxidant to extracted groundwater. The oxidant-laden groundwater is then injected and recirculated into a contaminated aquifer through multiple horizontal and/or vertical wells. This technique, referred to as in situ chemical oxidation through recirculation (ISCOR), can be applied to saturated and hydraulically conductive formations and used with relatively stable oxidants such as potassium permanganate (KMnO 4 ). A field-scale test of ISCOR was conducted at a site (Portsmouth Gaseous Diffusion Plant) where groundwater in a 5-ft thick silty gravel aquifer is contaminated with trichloroethylene (TCE) at levels that indicate the presence of residual dense non-aqueous phase liquids (DNAPLs). The field test was implemented using a pair of parallel horizontal wells with 200-ft screened sections. For approximately one month, groundwater was extracted from one horizontal well, dosed with crystalline KMnO 4 , and re-injected into the other horizontal well 90 ft away. Post-treatment characterization showed that ISCOR was effective at removing TCE in the saturated region. Lateral and vertical heterogeneities within the treatment zone impacted the uniform delivery of the oxidant solution. However, TCE was not detected in groundwater samples collected from monitoring wells and soil samples from borings in locations where the oxidant had permeated

  8. Microstructure and phase analysis of Zirconia-ODS (Oxide Dispersion Strengthen) alloy sintered by APS with milling time variation

    Science.gov (United States)

    Sugeng, Bambang; Bandriyana, B.; Sugeng, Bambang; Salam, Rohmad; Sumariyo; Sujatno, Agus; Dimyati, Arbi

    2018-03-01

    Investigation on the relationship between the process conditions of milling time and the microstructure on the synthesis of the zirconia-ODS steel alloy has been performed. The elemental composition of the alloy was determined on 20 wt% Cr and zirconia dispersoid of 0.50 wt%. The synthesis was carried out by powder metallurgy method with milling time of 3, 5 and 7 hours, static compression of 20 Ton and sintering process for 4 minutes using the APS (Arc Plasma Sintering) equipment. SEM-EDX and XRD test was carried out to characterize the phase and morphology of the alloy and the effect to the mechanical properties was evaluated by the Vickers Hardness testing. The synthesis produced sample of ODS steel with good dense and very little porous with the Fe-Cr phase that clearly observed in the XRD peak pattern. In addition milling time increased the homogeneously of Fe-Cr phase formulation, enhanced the grain refinement of the structure and increase the hardness of the alloy.

  9. Preparation and characterization of amorphous SiO2 coatings deposited by mirco-arc oxidation on sintered NdFeB permanent magnets

    International Nuclear Information System (INIS)

    Xu, J.L.; Xiao, Q.F.; Mei, D.D.; Zhong, Z.C.; Tong, Y.X.; Zheng, Y.F.; Li, L.

    2017-01-01

    Amorphous SiO 2 coatings were prepared on sintered NdFeB magnets by micro-arc oxidation (MAO) in silicate solution. The surface and cross-sectional morphologies, element and phase composition, corrosion resistance and magnetic properties of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization test and physical properties measurements system (PPMS). The results showed that the surface morphologies of the coatings exhibited the “coral reef” like structure, different from the typical MAO porous structure. With increasing the voltages, the thickness of the coatings increased from 12.72 to 19.90 µm, the content of Si element increased, while the contents of Fe, Nd and P elements decreased. The coatings were mainly composed of amorphous SiO 2 and a few amorphous Fe 2 O 3 and Nd 2 O 3 . The amorphous SiO 2 coatings presented excellent thermal shock resistance, while the thermal shock resistance decreased with increasing the voltages. The corrosion resistance of the coatings increased with increasing the voltages, and it could be enhanced by one order of magnitude compared to the uncoated NdFeB magnets. The MAO coatings slightly decreased the magnetic properties of the NdFeB samples in different degrees. - Highlights: • Amorphous SiO 2 coatings were prepared on sintered NdFeB magnets by micro-arc oxidation. • The coatings presented excellent thermal shock resistance. • The corrosion resistance could be enhanced by one order of magnitude. • The MAO coatings slightly decreased the magnetic properties of the NdFeB samples.

  10. Preparation and characterization of amorphous SiO{sub 2} coatings deposited by mirco-arc oxidation on sintered NdFeB permanent magnets

    Energy Technology Data Exchange (ETDEWEB)

    Xu, J.L., E-mail: jlxu@nchu.edu.cn [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Xiao, Q.F.; Mei, D.D. [School of Materials Science and Engineering, Nanchang Hangkong University, Nanchang 330063 (China); Zhong, Z.C., E-mail: zzhong2014@sina.com [The Institute for Rare Earth Magnetic Materials and Devices, Jiangxi University of Science and Technology, Ganzhou 341000 (China); Tong, Y.X. [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); Zheng, Y.F., E-mail: yfzheng@pku.edu.cn [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China); Li, L. [Center for Biomedical Materials and Engineering, Harbin Engineering University, Harbin 150001 (China)

    2017-03-15

    Amorphous SiO{sub 2} coatings were prepared on sintered NdFeB magnets by micro-arc oxidation (MAO) in silicate solution. The surface and cross-sectional morphologies, element and phase composition, corrosion resistance and magnetic properties of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization test and physical properties measurements system (PPMS). The results showed that the surface morphologies of the coatings exhibited the “coral reef” like structure, different from the typical MAO porous structure. With increasing the voltages, the thickness of the coatings increased from 12.72 to 19.90 µm, the content of Si element increased, while the contents of Fe, Nd and P elements decreased. The coatings were mainly composed of amorphous SiO{sub 2} and a few amorphous Fe{sub 2}O{sub 3} and Nd{sub 2}O{sub 3}. The amorphous SiO{sub 2} coatings presented excellent thermal shock resistance, while the thermal shock resistance decreased with increasing the voltages. The corrosion resistance of the coatings increased with increasing the voltages, and it could be enhanced by one order of magnitude compared to the uncoated NdFeB magnets. The MAO coatings slightly decreased the magnetic properties of the NdFeB samples in different degrees. - Highlights: • Amorphous SiO{sub 2} coatings were prepared on sintered NdFeB magnets by micro-arc oxidation. • The coatings presented excellent thermal shock resistance. • The corrosion resistance could be enhanced by one order of magnitude. • The MAO coatings slightly decreased the magnetic properties of the NdFeB samples.

  11. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.; AlYami, Noktan; LLOYD, D.C.; Bakr, Osman; BOYES, E.D.; GAI, P.L.

    2017-01-01

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

  12. In situ oxidation and reduction of triangular nickel nanoplates via environmental transmission electron microscopy

    KAUST Repository

    LAGROW, A.P.

    2017-08-29

    Understanding the oxidation and reduction mechanisms of transition metals, such as nickel (Ni), is important for their use in industrial applications of catalysis. A powerful technique for investigating the redox reactive species is in situ environmental transmission electron microscopy (ETEM), where oxidation and reduction can be tracked in real time. One particular difficulty in understanding the underlying reactions is understanding the underlying morphology of the starting structure in a reaction, in particular the defects contained in the material, and the exposed surface facets. Here-in, we use a colloidal nanoparticle synthesis in a continuous flow reactor to form nanoplates of nickel coated with oleylamine as a capping agent. We utilise an in situ heating procedure at 300 °C in vacuum to remove the oleylamine ligands, and then oxidise the Ni nanoparticles at 25 °C with 2 Pa oxygen, and follow the nanoparticles initial oxidation. After that, the nanoparticles are oxidised at 200 and 300 °C, making the size of the oxide shell increase to ∼4 nm. The oxide shell could be reduced under 2 Pa hydrogen at 500 °C to its initial size of ∼1 nm. High temperature oxidation encouraged the nanoparticles to form pure NiO nanoparticles, which occurred via the Kirkendall effect leading to hollowing and void formation.

  13. Enhanced In Situ Chemical Oxidation Using Surfactants and Shear Thinning Fluids

    Science.gov (United States)

    Hauswirth, S.; Sadeghi, S.; Cerda, C. C.; Espinoza, I.; Schultz, P. B.; Miller, C. T.

    2017-12-01

    In situ chemical oxidation (ISCO) is an attractive approach for the remediation of recalcitrant contaminants, due to the fact that target compounds are degraded in place, precluding the need for ex situ treatment or disposal. However, field applications of ISCO approaches have been plagued by "rebound" of contaminant concentrations in groundwater weeks to months after treatment. The cause of rebound at a given site may vary, but is typically associated with back-diffusion from finer grained, low permeability units or the presence of non-aqueous phase liquids (NAPLs) that are incompletely degraded during treatment. Modifications to traditional ISCO methods have been proposed to overcome these challenges, including the use of shear-thinning polymers to improve delivery of oxidants to low permeability units and the addition of surfactants to improve dissolution of contaminants from NAPLs. In this work, we investigate the application of these approaches to the oxidation of manufactured gas plant (MGP) tars—NAPLs composed primarily of polycyclic aromatic hydrocarbons (PAHs). We conducted experiments to determine the mutual impact of each chemical component on the physical and chemical properties of the overall system. Specifically, experiments were designed to: determine the kinetics and overall effectiveness of contaminant-oxidant reactions for multiple oxidant-activator combinations; screen several common surfactants in terms of their ability to increase MGP tar solubility and their compatibility with oxidant systems; measure the impact of oxidants and surfactants on the rheology of several common polymer additives; and assess the effect of surfactants and polymers on the consumption of oxidants/activators and on the kinetics of contaminant-oxidant reactions. The results of this work provide insight into the chemical and physical mechanisms associated with enhanced ISCO approaches and an improved basis with which to model and design ISCO applications at both the lab

  14. The application of in situ analytical transmission electron microscopy to the study of preferential intergranular oxidation in Alloy 600

    Energy Technology Data Exchange (ETDEWEB)

    Burke, M.G., E-mail: m.g.burke@manchester.ac.uk; Bertali, G.; Prestat, E.; Scenini, F.; Haigh, S.J.

    2017-05-15

    In situ analytical transmission electron microscopy (TEM) can provide a unique perspective on dynamic reactions in a variety of environments, including liquids and gases. In this study, in situ analytical TEM techniques have been applied to examine the localised oxidation reactions that occur in a Ni-Cr-Fe alloy, Alloy 600, using a gas environmental cell at elevated temperatures. The initial stages of preferential intergranular oxidation, shown to be an important precursor phenomenon for intergranular stress corrosion cracking in pressurized water reactors (PWRs), have been successfully identified using the in situ approach. Furthermore, the detailed observations correspond to the ex situ results obtained from bulk specimens tested in hydrogenated steam and in high temperature PWR primary water. The excellent agreement between the in situ and ex situ oxidation studies demonstrates that this approach can be used to investigate the initial stages of preferential intergranular oxidation relevant to nuclear power systems. - Highlights: • In situ analytical TEM has been performed in 1 bar H{sub 2}-H{sub 2}O vapor at 360–480 °C. • Nanoscale GB migration and solute partitioning correlate with ex situ data for Alloy 600 in H{sub 2}-steam. • This technique can provide new insights into localised reactions associated with localised oxidation.

  15. High temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites densified by spark plasma sintering

    Energy Technology Data Exchange (ETDEWEB)

    Saucedo-Acuna, R.A. [Instituto e Ingenieria y Tecnologia, Universidad Autonoma de Cd. Juarez, Av. Del Charro 450 Norte, Col. Partido Romero, C.P. 32310, Cd. Juarez, Chihuahua (Mexico); Monreal-Romero, H.; Martinez-Villafane, A. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Chacon-Nava, J.G. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico)], E-mail: jose.chacon@cimav.edu.mx; Arce-Colunga, U. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); Universidad Autonoma de Tamaulipas, Matamoros 8 y 9 Col. Centro C.P. 87110, Cd. Victoria, Tamaulipas (Mexico); Gaona-Tiburcio, C. [Centro de Investigacion en Materiales Avanzados, Departamento de Fisica de Materiales, Miguel de Cervantes 120, Complejo Industrial Chihuahua, C.P. 31109, Chihuahua (Mexico); De la Torre, S.D. [Centro de Investigacion e Innovacion Tecnologica (CIITEC)-IPN, D.F. Mexico (Mexico)

    2007-12-15

    The high temperature oxidation-sulfidation behavior of Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composites prepared by mechanical alloying (MA) and spark plasma sintering (SPS) has been studied. These composite powders have a particular metal-ceramic interpenetrating network and excellent mechanical properties. Oxidation-sulfidation tests were carried out at 900 deg. C, in a 2.5%SO{sub 2} + 3.6%O{sub 2} + N{sub 2}(balance) atmosphere for 48 h. The results revealed the influence of the sintering conditions on the specimens corrosion resistance, i.e. the Cr-Al{sub 2}O{sub 3} and Nb-Al{sub 2}O{sub 3} composite sintered at 1310 deg. C/4 min showed better corrosion resistance (lower weight gains) compared with those found for the 1440 deg. C/5 min conditions. For the former composite, a protective Cr{sub 2}O{sub 3} layer immediately forms upon heating, whereas for the later pest disintegration was noted. Thus, under the same sintering conditions the Nb-Al{sub 2}O{sub 3} composites showed the highest weight gains. The oxidation products were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy.

  16. Geochemical and microbiological characteristics during in situ chemical oxidation and in situ bioremediation at a diesel contaminated site.

    Science.gov (United States)

    Sutton, Nora B; Kalisz, Mariusz; Krupanek, Janusz; Marek, Jan; Grotenhuis, Tim; Smidt, Hauke; de Weert, Jasperien; Rijnaarts, Huub H M; van Gaans, Pauline; Keijzer, Thomas

    2014-02-18

    While in situ chemical oxidation with persulfate has seen wide commercial application, investigations into the impacts on groundwater characteristics, microbial communities and soil structure are limited. To better understand the interactions of persulfate with the subsurface and to determine the compatibility with further bioremediation, a pilot scale treatment at a diesel-contaminated location was performed consisting of two persulfate injection events followed by a single nutrient amendment. Groundwater parameters measured throughout the 225 day experiment showed a significant decrease in pH and an increase in dissolved diesel and organic carbon within the treatment area. Molecular analysis of the microbial community size (16S rRNA gene) and alkane degradation capacity (alkB gene) by qPCR indicated a significant, yet temporary impact; while gene copy numbers initially decreased 1-2 orders of magnitude, they returned to baseline levels within 3 months of the first injection for both targets. Analysis of soil samples with sequential extraction showed irreversible oxidation of metal sulfides, thereby changing subsurface mineralogy and potentially mobilizing Fe, Cu, Pb, and Zn. Together, these results give insight into persulfate application in terms of risks and effective coupling with bioremediation.

  17. Current state of the Uranium dioxide sintering theory

    International Nuclear Information System (INIS)

    Baranov, V.; Devyatko, Y.; Tenishev, A.; Khlunov, A.; Khomyakov, O.

    2011-01-01

    The basic approaches to the description of the ceramics sintering phenomenon are considered. It is established that diffusive sintering models incorrectly describe an intermediate stage of this process. The physical model of sintering, considering the substance plastic flow of pressing under the influence of internal stress forces and capillary forces, as the basic mechanism defining the shrinkage of sintering oxide nuclear fuel, is offered. (authors)

  18. In Situ Synchrotron X-Ray Diffraction Characterization of the Synthesis of Graphene Oxide and Reduced Graphene Oxide

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2015-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) synthesised from GO, has a promising future in fields ranging from electronics to energy technologies[1]. GO may be synthesized by the modified Hummer’s method[2], where a mixture of potassium permanganate and concentrated sulfuric acid forms...... by placing a mixture of permanganate and sulphuric acid in a capillary next to graphite. The synthesis was then initiated by gently pushing the fluid mixture into the powder with N2 gas. The in situ XRD of the GO synthesis showed how the oxidation reaction proceeds in three separate stages, as seen in Figure...... 1. The first stage was the dissolution of potassium permanganate, followed by an intercalation stage and subsequent formation of crystalline material. The GO 001 diffraction peak was observed early during the synthesis, in the second stage, and the intensity of the 001 diffraction increased during...

  19. Coarsening of Pd nanoparticles in an oxidizing atmosphere studied by in situ TEM

    DEFF Research Database (Denmark)

    Simonsen, Søren Bredmose; Chorkendorff, Ib; Dahl, Søren

    2016-01-01

    The coarsening of supported palladium nanoparticles in an oxidizing atmosphere was studied in situ by means of transmission electron microscopy (TEM). Specifically, the Pd nanoparticles were dispersed on a planar and amorphous Al2O3 support and were observed during the exposure to 10 mbar technical...... for the Ostwald ripening process indicates that the observed change in the particle size distribution can be accounted for by wetting of the Al2O3 support by the larger Pd nanoparticles....

  20. In-situ investigation of the calcination process of mixed oxide xerogels with Raman spectroscopy

    Energy Technology Data Exchange (ETDEWEB)

    Panitz, J C [Paul Scherrer Inst. (PSI), Villigen (Switzerland)

    1997-06-01

    The controlled calcination of materials derived by sol-gel reactions is important for the evolution of the final structure. Raman spectroscopy is an ideal tool for the identification of surface species under in-situ conditions, as demonstrated in the following for the example of a molybdenum oxide-silica xerogel. Raman spectra of this particular sample were recorded at temperatures as high as 1173 K, and compared with those of a reference material.(author) 3 figs., 4 refs.

  1. Oriented Arrays of Graphene in a Polymer Matrix by in situ Reduction of Graphite Oxide Nanosheets

    KAUST Repository

    Ansari, Seema

    2010-01-18

    Graphite oxide-Nafion hybrids with a high degree of alignment are cast from aqueous solution in the absence of any external field and reduced in situ by exposure to hydrazine to produce graphene-Nafion hybrids. Dramatic enhancement of electrical conductivity indicates sufficient accessibility of the inorganic nanosheets to the reducing agent, through the nanochannels formed by the polymeric ionic domains. © 2010 Wiley-VCH Verlag GmbH & Co. KGaA.

  2. In situ measurement of methane oxidation in groundwater by using natural-gradient tracer tests

    International Nuclear Information System (INIS)

    Smith, R.L.; Howes, B.L.; Garabedian, S.P.

    1991-01-01

    Methane oxidation was measured in an unconfined sand and gravel aquifer (Cape Cod, Mass.) by using in situ natural-gradient tracer tests at both a pristine, oxygenated site and an anoxic, sewage-contaminated site. The tracer sites were equipped with multilevel sampling devices to create target grids of sampling points; the injectate was prepared with groundwater from the tracer site to maintain the same geochemical conditions. Methane oxidation was calculated from breakthrough curves of methane relative to halide and inert gas (hexafluoroethane) tracers and was confirmed by the appearance of 13 C-enriched carbon dioxide in experiments in which 13 C-enriched methane was used as the tracer. A V max for methane oxidation could be calculated when the methane concentration was sufficiently high to result in zero-order kinetics throughout the entire transport interval. Methane breakthrough curves could be simulated by modifying a one-dimensional advection-dispersion transport model to include a Michaelis-Menten-based consumption term for methane oxidation. The K m values for methane oxidation that gave the best match for the breakthrough curve peaks were 6.0 and 9.0 μM for the uncontaminated and contaminated sites, respectively. Natural-gradient tracer tests are a promising approach for assessing microbial processes and for testing in situ bioremediation potential in groundwater systems

  3. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  4. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  5. On the sintering kinetics in UO2

    International Nuclear Information System (INIS)

    Marajofsky, A.

    1998-01-01

    The fabrication process of UO 2 pellets from powders involve pressing and a sintering anneal at high temperature (1650 deg. C to 1750 deg. C) during two or more hours in a hydrogen atmosphere. An alternative method is the oxidative sintering, made at lower temperature (1000 deg. C to 1300 deg. C) in a CO 2 or CO/CO 2 atmosphere. The sintering phenomena consist in the densification of the material by a thermal treatment below the fusion point. For a compact made by pressing a powder, sintering is the process of annulation of the porosity present in the compact or pellet. Several theories describe the sintering phenomena dividing it in three stages, initial, intermediate and final: in all of them the densification is a continuous growing function of time. Nevertheless it has been experimentally reported that a reduction of the density occurs in the third step of the sintering. The phenomena has been called solarization. Solarization has been attributed to the effect of the evolved gases from additives or to the CO 2 atmosphere in oxidative sintering. Thus, it is convenient to distinguish between solarization in oxidative or reducing conditions. Reducing solarization is a consequence of the tendency towards equilibrium of intergranular pores. In oxidative sintering it occurs in the reducing anneal after the sintering and is due to the change in the lattice parameter. This work shows examples of both types of solarization and qualitative interpretation of this phenomena. Both situations show the need of strict control of the sintering and powder production conditions. (author)

  6. Sintering and densification; new techniques: sinter forging

    International Nuclear Information System (INIS)

    Winnubst, A.J.A.

    1998-01-01

    In this chapter pressure assisted sintering methods will be described. Attention will mainly be paid to sinter forging as a die-wall free uniaxial pressure sintering technique, where large creep strains are possible. Sinter forging is an effective tool to reduce sintering temperature and time and to obtain a nearly theoretically dense ceramic. In this way grain size in tetragonal zirconia ceramics can be reduced down to 100 nm. Another important phenomenon is the reduction of the number density and size of cracks and flaws resulting in higher strength and improved reliability, which is of utmost importance for engineering ceramics. The creep deformation during sinter forging causes a rearrangement of the grains resulting in a reduction of interatomic spaces between grains, while grain boundary (glassy) phases can be removed. The toughness and in some cases the wear resistance is enhanced after sinter forging as a result of the grain-boundary-morphology improvement. (orig.)

  7. Mechanical characteristics of microwave sintered silicon carbide

    Indian Academy of Sciences (India)

    Unknown

    sintered process, SiC grain gets oxidized producing SiO2 (∼ 32 wt%) and deteriorates the quality of the product substantially. Partially sintered .... product, could be due to oxidation of SiC, e.g. 50% weight gain of a green SiC sample ... because, the charging current is 90° advanced in phase, ideally, with respect to the ...

  8. Method for hot pressing beryllium oxide articles

    Science.gov (United States)

    Ballard, Ambrose H.; Godfrey, Jr., Thomas G.; Mowery, Erb H.

    1988-01-01

    The hot pressing of beryllium oxide powder into high density compacts with little or no density gradients is achieved by employing a homogeneous blend of beryllium oxide powder with a lithium oxide sintering agent. The lithium oxide sintering agent is uniformly dispersed throughout the beryllium oxide powder by mixing lithium hydroxide in an aqueous solution with beryllium oxide powder. The lithium hydroxide is converted in situ to lithium carbonate by contacting or flooding the beryllium oxide-lithium hydroxide blend with a stream of carbon dioxide. The lithium carbonate is converted to lithium oxide while remaining fixed to the beryllium oxide particles during the hot pressing step to assure uniform density throughout the compact.

  9. Microwave sintering of hydroxyapatite-based composites

    International Nuclear Information System (INIS)

    Fang, Y.; Roy, D.M.; Cheng, J.; Roy, R.; Agrawal, D.K.

    1993-01-01

    Composites of hydroxyapatite/partially stabilized zirconia (HAp/PSZ) and hydroxyapatite/silicon carbide whiskers (HAp/SiC) were sintered at 1100-1200 degrees C by microwave at 2.45 GHz. Characterization of the sintered composites was carried out by density, microstructure, phase composition, and fracture toughness measurements. The results show that although not yet fully densified, a much higher sintered density in the HAp/PSZ composite was achieved by microwave sintering than by conventional sintering at the same temperature. A relative density of 93% was achieved by 20 min. microwave processing at 1200 degrees C. Comparatively, 2 h conventional sintering of the same material at 1200 degrees C led to only 75.5% relative density. K IC of this microwave sintered HAp/PSZ of 93% density was found to be 3.88 MPa√m, which is 250% of the value for pure HAp of the same density. A further increase in K IC could be expected if full or nearly full densification was achieved. Sintering of PSZ particles in the HAp/PSZ composite was also observed in the microwave processed sample. Microwave sintering of HAp/SiC was not successful in the current study due to the oxidation of SiC in air at high temperature. 8 refs., 4 figs., 1 tab

  10. Structure and Properties of Nanocomposites based on PTT-block-PTMO Copolymer and Graphene Oxide prepared by in Situ Polymerization

    OpenAIRE

    Paszkiewicz, Sandra; Szymczyk, Anna; Špitalský, Zdenko; Mosnáček, Jaroslav; Kwiatkowski, Konrad; Rosłaniec, Zbigniew

    2014-01-01

    Poly(trimethylene terephthalate-block-tetramethylene oxide) (PTT-PTMO) copolymer/graphene oxide nanocomposites were prepared by in situ polymerization. From the SEM and TEM images of PTT-PTMO/GO nanocomposite, it can be seen that GO sheets are clearly well-dispersed in the PTT-PTMO matrix. TEM images also showed that graphene was well exfoliated into individual sheets, suggesting that in situ polymerization is a highly efficient method for preparing nanocomposites. The influence of GO on the ...

  11. Microstructural comparison of effects of hafnium and titanium additions in spark-plasma-sintered Fe-based oxide-dispersion strengthened alloys

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Yina, E-mail: huangyina1981@hotmail.com [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); School of Electronic Science & Applied Physics, Hefei University of Technology, Hefei, Anhui 230009 (China); Zhang, Hongtao [Department of Materials, Loughborough University, Leicestershire, LE11 3TU (United Kingdom); Auger, Maria A.; Hong, Zuliang [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Ning, Huanpo [School of Engineering of Materials Science, Queen Mary University of London, London, E1 4NS (United Kingdom); Nanoforce Technology Ltd, London, E1 4NS (United Kingdom); Gorley, Michael J. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); CCFE, Culham Science Centre, Abingdon, Oxon, OX14 3DB (United Kingdom); Grant, Patrick S. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); Reece, Michael J.; Yan, Haixue [School of Engineering of Materials Science, Queen Mary University of London, London, E1 4NS (United Kingdom); Nanoforce Technology Ltd, London, E1 4NS (United Kingdom); Roberts, Steve G. [Department of Materials, University of Oxford, Oxford OX1 3PH (United Kingdom); CCFE, Culham Science Centre, Abingdon, Oxon, OX14 3DB (United Kingdom)

    2017-04-15

    Two oxide dispersion strengthened alloys: 14Cr-0.25Y{sub 2}O{sub 3}-0.22Hf (wt.%) and Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.4Ti (wt.%) were fabricated by mechanical alloying and subsequently consolidated by spark plasma sintering (SPS). Electron backscatter diffraction showed grain sizes in the range 0.5–15 μm in both alloys. Transmission electron microscopy and scanning transmission electron microscopy showed a homogeneous distribution of nano-oxides precipitated during SPS. Using high resolution transmission electron microscopy, energy dispersive X-ray spectroscopy and atom probe tomography, several different oxide phases were found in both alloys, but the majority of dispersoids were Y-Hf-O type in Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.22Hf and Y-Ti-O type in Fe-14Cr-0.25Y{sub 2}O{sub 3}-0.4Ti. There were a variety of orientation relationships between the different dispersoids and the ferritic matrix. Both alloys had dispersoid densities of ∼10{sup 23}/m{sup 3}, with average diameters of 4.3 nm and 3.5 nm in the 0.22Hf and 0.4Ti containing alloys, respectively. Per atom added, Hf (0.07 at.%) is suggested to be more potent than Ti (0.46 at.%) in refining the nano-oxides.

  12. In-Situ Growth and Characterization of Indium Tin Oxide Nanocrystal Rods

    Directory of Open Access Journals (Sweden)

    Yan Shen

    2017-11-01

    Full Text Available Indium tin oxide (ITO nanocrystal rods were synthesized in-situ by a vapor-liquid-solid (VLS method and electron beam evaporation technique. When the electron-beam gun bombarded indium oxide (In2O3 and tin oxide (SnO2 mixed sources, indium and tin droplets appeared and acted as catalysts. The nanocrystal rods were in-situ grown on the basis of the metal catalyst point. The nanorods have a single crystal structure. Its structure was confirmed by X-ray diffraction (XRD and transmission electron microscopy (TEM. The surface morphology was analyzed by scanning electron microscopy (SEM. During the evaporation, a chemical process was happened and an In2O3 and SnO2 solid solution was formed. The percentage of doped tin oxide was calculated by Vegard’s law to be 3.18%, which was in agreement with the mixture ratio of the experimental data. The single crystal rod had good semiconductor switch property and its threshold voltage of single rod was approximately 2.5 V which can be used as a micro switch device. The transmission rate of crystalline nanorods ITO film was over 90% in visible band and it was up to 95% in the blue green band as a result of the oxygen vacancy recombination luminescence.

  13. Characterization of subcritical water oxidation with in situ monitoring and self-modeling curve resolution

    International Nuclear Information System (INIS)

    Gemperline, Paul J.; Yang Yu; Bian Zhihui

    2003-01-01

    In this paper, a subcritical water oxidation (SBWO) process was monitored using self-modeling curve resolution (SMCR) of in situ UV-Vis measurements to estimate time-dependant composition profiles of reactants, intermediates and products. A small laboratory scale reactor with UV-Vis fiber-optic probes and a flow cell was used to demonstrate the usefulness of SMCR for monitoring the destruction of model compounds phenol, benzoic acid, and aniline in a dilute aqueous solutions. Hydrogen peroxide was used as the oxidizing reagent at moderate temperature (150-250 deg. C) and pressure (60-90 atm) in a single phase. By use of in situ monitoring, reaction times were easily determined and conditions for efficient oxidations were easily diagnosed without the need for time consuming off-line reference measurements. For selected runs, the destruction of the model compound was confirmed by gas chromatography and chemical oxygen demand (COD) measurements. Suspected intermediate oxidation products were easily detected by the use of UV-Vis spectrometry and self-modeling curve resolution, but could not be detected by gas chromatography

  14. The state of permanganate with relation to in situ chemical oxidation

    International Nuclear Information System (INIS)

    Veronda, Brenda; Dingens, Matthew

    2007-01-01

    In Situ Chemical Oxidation (ISCO) with permanganate had its beginnings over 10 years ago. Since that time, many sites have been successfully treated for organic compounds including chlorinated ethenes (perchloroethylene, trichloroethylene, etc.) phenols, explosives such as RDX, and many other organics. The successful application of ISCO with permanganate requires the integration of many site-specific factors into the remedial design. ISCO with permanganate is an effective technology, not only for its oxidative properties and persistence, but also for its application flexibility to remediate soil and groundwater. The merits of any type of treatment technology can be assessed in terms of effectiveness, ease of use, reaction rate, and cost. The use of permanganate for in situ chemical oxidation results in the complete mineralization of TCE and PCE and can result in treatment levels below detection limits. Permanganate is a single component oxidizer, which is easily handled, mixed and distributed to the subsurface. Permanganate is also inexpensive to design and implement as compared to other technologies. This presentation will provide a general overview of the application and safety aspects of ISCO with permanganate. This paper will discuss the advantages and limitations of this technology, typical cost ranges, site evaluation and application technologies. (authors)

  15. Ex situ integration of iron oxide nanoparticles onto the exfoliated expanded graphite flakes in water suspension

    Directory of Open Access Journals (Sweden)

    Jović Nataša

    2014-01-01

    Full Text Available Hybrid structures composed of exfoliated expanded graphite (EG and iron oxide nanocrystals have been produced by an ex situ process. The iron oxide nanoparticles coated with meso-2,3-dimercaptosuccinic acid (DMSA, or poly(acrylic acid (PAA were integrated onto the exfoliated EG flakes by mixing their aqueous suspensions at room temperature under support of 1-ethyl-3-(3-dimethylaminopropylcarbodiimide (EDC and N-hydroxysuccin-nimide (NHS. EG flakes have been used both, naked and functionalized with branched polyethylenimine (PEI. Complete integration of two constituents has been achieved and mainteined stable for more than 12 months. No preferential spatial distribution of anchoring sites for attachement of iron oxide nanoparticles has been observed, regardless EG flakes have been used naked or functionalized with PEI molecules. The structural and physico-chemical characteristics of the exfoliated expanded graphite and its hybrids nanostructures has been investigated by SEM, TEM, FTIR and Raman techniques. [Projekat Ministarstva nauke Republike Srbije, br. 45015

  16. In situ functionalization and PEO coating of iron oxide nanocrystals using seeded emulsion polymerization.

    Science.gov (United States)

    Kloust, Hauke; Schmidtke, Christian; Feld, Artur; Schotten, Theo; Eggers, Robin; Fittschen, Ursula E A; Schulz, Florian; Pöselt, Elmar; Ostermann, Johannes; Bastús, Neus G; Weller, Horst

    2013-04-16

    Herein we demonstrate that seeded emulsion polymerization is a powerful tool to produce multiply functionalized PEO coated iron oxide nanocrystals. Advantageously, by simple addition of functional surfactants, functional monomers, or functional polymerizable linkers-solely or in combinations thereof-during the seeded emulsion polymerization process, a broad range of in situ functionalized polymer-coated iron oxide nanocrystals were obtained. This was demonstrated by purposeful modulation of the zeta potential of encapsulated iron oxide nanocrystals and conjugation of a dyestuff. Successful functionalization was unequivocally proven by TXRF. Furthermore, the spatial position of the functional groups can be controlled by choosing the appropriate spacers. In conclusion, this methodology is highly amenable for combinatorial strategies and will spur rapid expedited synthesis and purposeful optimization of a broad scope of nanocrystals.

  17. Hydrothermal Cold Sintering

    Science.gov (United States)

    Kang, Xiaoyu

    Solid state sintering transforms particle compact to a physically robust and dense polycrystalline monolith driven by reduction of surface energy and curvature. Since bulk diffusion is required for neck formation and pore elimination, sintering temperature about 2/3 of melting point is needed. It thus places limitations for materials synthesis and integration, and contributes to significant energy consumption in ceramic processing. Furthermore, since surface transport requires lower temperature than bulk processes, grain growth is often rapid and can be undesired for physical properties. For these reasons, several techniques have been developed including Liquid Phase Sintering (LPS), Hot Pressing (HP) and Field Assisted Sintering Technique (FAST), which introduce either viscous melt, external pressure or electric field to speed up densification rates at lower temperature. However, because of their inherent reliability on bulk diffusion, temperatures required are often too high for integrating polymers and non-noble metals. Reduction of sintering temperature below 400 °C would require a different densification mechanism that is based on surface transport with external forces to drive volume shrinkage. Densification method combining uniaxial pressure and solution under hydrothermal condition was first demonstrated by Kanahara's group at Kochi University in 1986 and was brought to our attention by the work of Kahari, etc, from University of Oulu on densification of Li2MoO 4 in 2015. This relatively new process showed promising ultra-low densification temperature below 300 °C, however little was known about its fundamental mechanism and scope of applications, which became the main focus of this dissertation. In this work, a uniaxial hydraulic press, a standard stainless steel 1/2 inch diameter die with heating band were utilized in densifying metal oxides. Applied pressure and sintering temperature were between 100 MPa and 700 MPa and from room temperature to 300

  18. In situ studies of oxide nucleation, growth, and transformation using slow electrons

    Science.gov (United States)

    Flege, Jan Ingo; Grinter, David C.

    2018-05-01

    Surface processes such as metal oxidation and metal oxide growth invariably influence the physical and chemical properties of materials and determine their interaction with their surroundings and hence their functionality in many technical applications. On a fundamental level, these processes are found to be governed by a complex interplay of thermodynamic variables and kinetic constraints, resulting in a rich variety of material-specific phenomena. In this review article, we discuss recent results and insights on transition metal oxidation and rare-earth oxide growth acquired by low-energy electron microscopy and related techniques. We demonstrate that the use of in situ surface sensitive methods is a prerequisite to gaining a deeper understanding of the underlying concepts and the mechanisms responsible for the emerging oxide structure and morphology. Furthermore, examples will be provided on how structural and chemical modifications of the oxide films and nanostructures can be followed in real-time and analyzed in terms of local reactivity and cooperative effects relevant for heterogeneous model catalysis.

  19. Hot water extraction with in situ wet oxidation: Kinetics of PAHs removal from soil

    International Nuclear Information System (INIS)

    Dadkhah, Ali A.; Akgerman, Aydin

    2006-01-01

    Finding environmentally friendly and cost-effective methods to remediate soils contaminated with polycyclic aromatic hydrocarbons (PAHs) is currently a major concern of researchers. In this study, a series of small-scale semi-continuous extractions - with and without in situ wet oxidation - were performed on soils polluted with PAHs, using subcritical water (i.e. liquid water at high temperatures and pressures, but below the critical point) as the removal agent. Experiments were performed in a 300 mL reactor using an aged soil sample. To find the desorption isotherms and oxidation reaction rates, semi-continuous experiments with residence times of 1 and 2 h were performed using aged soil at 250 deg. C and hydrogen peroxide as oxidizing agent. In all combined extraction and oxidation flow experiments, PAHs in the remaining soil after the experiments were almost undetectable. In combined extraction and oxidation no PAHs could be detected in the liquid phase after the first 30 min of the experiments. Based on these results, extraction with hot water, if combined with oxidation, should reduce the cost of remediation and can be used as a feasible alternative technique for remediating contaminated soils and sediments

  20. Study of the Radical Chain Mechanism of Hydrocarbon Oxidation for In Situ Combustion Process

    Directory of Open Access Journals (Sweden)

    Alexandra Ushakova

    2017-01-01

    Full Text Available Despite the abundance of in situ combustion models of oil oxidation, many of the effects are still beyond consideration. For example, until now, initial stages of oxidation were not considered from a position of radical chain process. This is a serious difficulty for the simulation of oil recovery process that involves air injection. To investigate the initial stages of oxidation, the paper considers the sequence of chemical reactions, including intermediate short-living compounds and radicals. We have attempted to correlate the main stages of the reaction with areas of heat release observed in the experiments. The system of differential equations based on the equations of oxidation reactions was solved. Time dependence of peroxides formation and start of heat release is analytically derived for the initial stages. We have considered the inhibition of initial oxidation stages by aromatic oil compounds and have studied the induction time in dependence on temperature. Chain ignition criteria for paraffins and crude oil in presence of core samples were obtained. The calculation results are compared with the stages of oxidation that arise by high-pressure differential scanning calorimetry. According to experimental observations we have determined which reactions are important for the process and which can be omitted or combined into one as insignificant.

  1. Uranium oxidation kinetics monitored by in-situ X-ray diffraction

    Energy Technology Data Exchange (ETDEWEB)

    Zalkind, S., E-mail: shimonzl@nrcn.org.il; Rafailov, G.; Halevy, I.; Livneh, T.; Rubin, A.; Maimon, H.; Schweke, D.

    2017-03-15

    The oxidation kinetics of U-0.1 wt%Cr at oxygen pressures of 150 Torr and the temperature range of 90–150 °C was studied by means of in-situ X-ray diffraction (XRD). A “breakaway” in the oxidation kinetics is found at ∼0.25 μm, turning from a parabolic to a linear rate law. At the initial stage of oxidation the growth plane of UO{sub 2}(111) is the prominent one. As the oxide thickens, the growth rate of UO{sub 2}(220) plane increases and both planes grow concurrently. The activation energies obtained for the oxide growth are Q{sub parabolic} = 17.5 kcal/mol and Q{sub linear} = 19 kcal/mol. Enhanced oxidation around uranium carbide (UC) inclusions is clearly observed by scanning electron microscopy (SEM).

  2. New materials through a variety of sintering methods

    Science.gov (United States)

    Jaworska, L.; Cyboroń, J.; Cygan, S.; Laszkiewicz-Łukasik, J.; Podsiadło, M.; Novak, P.; Holovenko, Y.

    2018-03-01

    New sintering techniques make it possible to obtain materials with special properties that are impossible to obtain by conventional sintering techniques. This issue is especially important for ceramic materials for application under extreme conditions. Following the tendency to limit critical materials in manufacturing processes, the use of W, Si, B, Co, Cr should be limited, also. One of the cheapest and widely available materials is aluminum oxide, which shows differences in phase composition, grain size, hardness, strain and fracture toughness of the same type of powder, sintered via various methods. In this paper the alumina was sintered using the conventional free sintering process, microwave sintering, Spark Plasma Sintering (SPS), high pressure-high temperature method (HP-HT) and High Pressure Spark Plasma Sintering (HP SPS). Phase composition analysis, by X-ray diffraction of the alumina materials sintered using various methods, was carried out. For the conventional sintering method, compacts are composed of α-Al2O3 and θ-Al2O3. For compacts sintered using SPS, microwave and HP-HT methods, χ-Al2O3 and γ-Al2O3 phases were additionally present. Mechanical and physical properties of the obtained materials were compared between the methods of sintering. On the basis of images from scanning electron microscope quantitative analysis was performed to determine the degree of grain growth of alumina after sintering.

  3. Structural Investigation of Sodium Layered Oxides Via in Situ Synchrotron X-Ray Diffraction

    DEFF Research Database (Denmark)

    Jung, Young Hwa; Christiansen, Ane Sælland; Johnsen, Rune

    2015-01-01

    electrochemical reaction is generally considered to be a pivotal feature for understanding the relationship between layered structures and electrochemical properties. Here the structure, phase stability, and electrochemical properties of two kinds of layered oxides, P2 and O3, are investigated through in......-situ synchrotron XRD experiments. A capillary Na-based cell is designed to minimize interference in other substances such as a separator or external battery parts. This approach could give us to obtain clear diffraction patterns with high intensity during electrochemical reaction in a short period of time without...... further relaxation step. We carefully scrutinized reversible structural phase transformations during electrochemical reaction of P2 and O3-layered compounds based on in situ analysis, and detailed results will be discussed....

  4. Gaining electricity from in situ oxidation of hydrogen produced by fermentative cellulose degradation.

    Science.gov (United States)

    Niessen, J; Schröder, U; Harnisch, F; Scholz, F

    2005-01-01

    To exploit the fermentative hydrogen generation and direct hydrogen oxidation for the generation of electric current from the degradation of cellulose. Utilizing the metabolic activity of the mesophilic anaerobe Clostridium cellulolyticum and the thermophilic Clostridium thermocellum we show that electricity generation is possible from cellulose fermentation. The current generation is based on an in situ oxidation of microbially synthesized hydrogen at platinum-poly(tetrafluoroaniline) (Pt-PTFA) composite electrodes. Current densities of 130 mA l(-1) (with 3 g cellulose per litre medium) were achieved in poised potential experiments under batch and semi-batch conditions. The presented results show that electricity generation is possible by the in situ oxidation of hydrogen, product of the anaerobic degradation of cellulose by cellulolytic bacteria. For the first time, it is shown that an insoluble complex carbohydrate like cellulose can be used for electricity generation in a microbial fuel cell. The concept represents a first step to the utilization of macromolecular biomass components for microbial electricity generation.

  5. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    Energy Technology Data Exchange (ETDEWEB)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong, E-mail: hhong@aps.anl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tung, I. C. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Department of Materials Science and Engineering, Northwestern University, Evanston, Illinois 60208 (United States); Chang, S.-H.; Bhattacharya, A.; Fong, D. D. [Materials Science Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

    2016-01-15

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques.

  6. In situ surface/interface x-ray diffractometer for oxide molecular beam epitaxy

    International Nuclear Information System (INIS)

    Lee, J. H.; Freeland, J. W.; Hong, Hawoong; Tung, I. C.; Chang, S.-H.; Bhattacharya, A.; Fong, D. D.

    2016-01-01

    In situ studies of oxide molecular beam epitaxy by synchrotron x-ray scattering has been made possible by upgrading an existing UHV/molecular beam epitaxy (MBE) six-circle diffractometer system. For oxide MBE growth, pure ozone delivery to the chamber has been made available, and several new deposition sources have been made available on a new 12 in. CF (ConFlat, a registered trademark of Varian, Inc.) flange. X-ray diffraction has been used as a major probe for film growth and structures for the system. In the original design, electron diffraction was intended for the secondary diagnostics available without the necessity of the x-ray and located at separate positions. Deposition of films was made possible at the two diagnostic positions. And, the aiming of the evaporation sources is fixed to the point between two locations. Ozone can be supplied through two separate nozzles for each location. Also two separate thickness monitors are installed. Additional features of the equipment are also presented together with the data taken during typical oxide film growth to illustrate the depth of information available via in situ x-ray techniques

  7. In situ observations of oxide fracture on austenitic stainless steels relevant to IASCC

    International Nuclear Information System (INIS)

    Duff, J.; Burke, M.G.; Scenini, F.

    2015-01-01

    Stress Corrosion Cracking (SCC) and Irradiation-Assisted Stress Corrosion Cracking (IASCC) are important failure modes in the nuclear industry, yet the exact mechanism(s) responsible for these complex failure phenomena are not fully understood. In particular, considerable attention is being focused on SCC and IASCC initiation and the behaviour of the oxidised metal surface during straining in a relevant environment. Experimental observations and data for oxide fracture at the grain boundary are limited, but are also required for the development of crack growth models. In this work, the role of strain localization on surface oxide fracture has been examined via: 1) in situ straining experiments using a state-of-the-art imaging autoclave; and 2) ex situ studies using pre-oxidised samples in a FEG-SEM with a micro-tensile stage. The work was conducted using three materials: 1) a non-irradiated archive Type 316 Stainless Steel, 2) a 1 dpa proton-irradiated Type 316 Stainless Steel, and 3) a model alloy designed to simulate the grain boundary composition resulting from radiation induced segregation. The observations were performed on samples pre-oxidized at 320 C. degrees in high purity, water containing 30 cm 3 /kg of dissolved H 2 and 2 ppm Li additions. The samples were strained in tension and the surface deformation measured via Digital Image Correlation. This technique provided quantitative data regarding the intergranular strains associated with oxide fracture. Oxide fracture and strain development were also related to the local irradiation-induced microstructure and grain boundary character. The results from this work contribute to the mechanistic information on the role of strain localization and composition on the incubation stages of IASCC. (authors)

  8. Influence of calcium oxide level and time of exposure to sugarcane on in vitro and in situ digestion kinetics

    Science.gov (United States)

    Experiments were carried out to evaluate, using in vitro and in situ techniques, the effects of three inclusion levels of calcium oxide (0, 5, and 10 g/kg of sugarcane fresh matter) and four exposure times (0, 24, 48, and 72 h) of sugarcane to calcium oxide on the chemical composition and digestive ...

  9. In situ growth of capping-free magnetic iron oxide nanoparticles on liquid-phase exfoliated graphene

    NARCIS (Netherlands)

    Tsoufis, T.; Syrgiannis, Z.; Akhtar, N.; Prato, M.; Katsaros, F.; Sideratou, Z.; Kouloumpis, A.; Gournis, D.; Rudolf, P.

    2015-01-01

    We report a facile approach for the in situ synthesis of very small iron oxide nanoparticles on the surface of high-quality graphene sheets. Our synthetic strategy involved the direct, liquid-phase exfoliation of highly crystalline graphite (avoiding any oxidation treatment) and the subsequent

  10. In Situ Spectroscopy and Mechanistic Insights into CO Oxidation on Transition-Metal-Substituted Ceria Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Elias, Joseph S.; Stoerzinger, Kelsey A.; Hong, Wesley T.; Risch, Marcel; Giordano, Livia [Dipartimento; Mansour, Azzam N. [Naval; Shao-Horn, Yang

    2017-09-12

    Herein we investigate the reaction intermediates formed during CO oxidation on copper-substituted ceria nanoparticles (Cu0.1Ce0.9O2–x) by means of in situ spectroscopic techniques and identify an activity descriptor that rationalizes a trend with other metal substitutes (M0.1Ce0.9O2–x, M = Mn, Fe, Co, Ni). In situ X-ray absorption spectroscopy (XAS) performed under catalytic conditions demonstrates that O2– transfer occurs at dispersed copper centers, which are redox active during catalysis. In situ XAS reveals a dramatic reduction at the copper centers that is fully reversible under catalytic conditions, which rationalizes the high catalytic activity of Cu0.1Ce0.9O2–x. Ambient pressure X-ray photoelectron spectroscopy (AP-XPS) and in situ diffuse reflectance infrared Fourier transform spectroscopy (DRIFTS) show that CO can be oxidized to CO32– in the absence of O2. We find that CO32– desorbs as CO2 only under oxygen-rich conditions when the oxygen vacancy is filled by the dissociative adsorption of O2. These data, along with kinetic analyses, lend support to a mechanism in which the breaking of copper–oxygen bonds is rate-determining under oxygen-rich conditions, while refilling the resulting oxygen vacancy is rate-determining under oxygen-lean conditions. On the basis of these observations and density functional calculations, we introduce the computed oxygen vacancy formation energy (Evac) as an activity descriptor for substituted ceria materials and demonstrate that Evac successfully rationalizes the trend in the activities of M0.1Ce0.9O2–x catalysts that spans three orders of magnitude. The applicability of Evac as a useful design descriptor is demonstrated by the catalytic performance of the ternary oxide Cu0.1La0.1Ce0.8O2–x, which has an apparent activation energy rivaling those of state-of-the-art Au/TiO2 materials. Thus, we suggest that cost-effective catalysts for CO oxidation can be rationally designed by judicious choice of substituting

  11. Field study of nitrous oxide production with in situ aeration in a closed landfill site.

    Science.gov (United States)

    Nag, Mitali; Shimaoka, Takayuki; Nakayama, Hirofumi; Komiya, Teppei; Xiaoli, Chai

    2016-03-01

    Nitrous oxide (N(2)O) has gained considerable attention as a contributor to global warming and depilation of stratospheric ozone layer. Landfill is one of the high emitters of greenhouse gas such as methane and N(2)O during the biodegradation of solid waste. Landfill aeration has been attracted increasing attention worldwide for fast, controlled and sustainable conversion of landfills into a biological stabilized condition, however landfill aeration impel N(2)O emission with ammonia removal. N(2)O originates from the biodegradation, or the combustion of nitrogen-containing solid waste during the microbial process of nitrification and denitrification. During these two processes, formation of N(2)O as a by-product from nitrification, or as an intermediate product of denitrification. In this study, air was injected into a closed landfill site and investigated the major N(2)O production factors and correlations established between them. The in-situ aeration experiment was carried out by three sets of gas collection pipes along with temperature probes were installed at three different distances of one, two and three meter away from the aeration point; named points A-C, respectively. Each set of pipes consisted of three different pipes at three different depths of 0.0, 0.75 and 1.5 m from the bottom of the cover soil. Landfill gases composition was monitored weekly and gas samples were collected for analysis of nitrous oxide concentrations. It was evaluated that temperatures within the range of 30-40°C with high oxygen content led to higher generation of nitrous oxide with high aeration rate. Lower O(2) content can infuse N(2)O production during nitrification and high O(2) inhibit denitrification which would affect N(2)O production. The findings provide insights concerning the production potentials of N(2)O in an aerated landfill that may help to minimize with appropriate control of the operational parameters and biological reactions of N turnover. Investigation of

  12. Preparation and characterization of amorphous SiO2 coatings deposited by mirco-arc oxidation on sintered NdFeB permanent magnets

    Science.gov (United States)

    Xu, J. L.; Xiao, Q. F.; Mei, D. D.; Zhong, Z. C.; Tong, Y. X.; Zheng, Y. F.; Li, L.

    2017-03-01

    Amorphous SiO2 coatings were prepared on sintered NdFeB magnets by micro-arc oxidation (MAO) in silicate solution. The surface and cross-sectional morphologies, element and phase composition, corrosion resistance and magnetic properties of the coatings were investigated by scanning electron microscopy (SEM), energy dispersive X-ray spectrometer (EDS), X-ray photoelectron spectroscopy (XPS), potentiodynamic polarization test and physical properties measurements system (PPMS). The results showed that the surface morphologies of the coatings exhibited the "coral reef" like structure, different from the typical MAO porous structure. With increasing the voltages, the thickness of the coatings increased from 12.72 to 19.90 μm, the content of Si element increased, while the contents of Fe, Nd and P elements decreased. The coatings were mainly composed of amorphous SiO2 and a few amorphous Fe2O3 and Nd2O3. The amorphous SiO2 coatings presented excellent thermal shock resistance, while the thermal shock resistance decreased with increasing the voltages. The corrosion resistance of the coatings increased with increasing the voltages, and it could be enhanced by one order of magnitude compared to the uncoated NdFeB magnets. The MAO coatings slightly decreased the magnetic properties of the NdFeB samples in different degrees.

  13. In Situ Spectroscopic Analysis of the Carbothermal Reduction Process of Iron Oxides during Microwave Irradiation

    Directory of Open Access Journals (Sweden)

    Jun Fukushima

    2018-01-01

    Full Text Available The effects of microwave plasma induction and reduction on the promotion of the carbothermal reduction of iron oxides (α-Fe2O3, γ-Fe2O3, and Fe3O4 are investigated using in situ emission spectroscopy measurements during 2.45 GHz microwave processing, and the plasma discharge (such as CN and N2 is measured during microwave E-field irradiation. It is shown that CN gas or excited CN molecules contribute to the iron oxide reduction reactions, as well as to the thermal reduction. On the other hand, no plasma is generated during microwave H-field irradiation, resulting in thermal reduction. Magnetite strongly interacts with the microwave H-field, and the reduction reaction is clearly promoted by microwave H-field irradiation, as well as thermal reduction reaction.

  14. Magnetization of individual yeast cells by in situ formation of iron oxide on cell surfaces

    Science.gov (United States)

    Choi, Jinsu; Lee, Hojae; Choi, Insung S.; Yang, Sung Ho

    2017-09-01

    Magnetic functionalization of living cells has intensively been investigated with the aim of various bioapplications such as selective separation, targeting, and localization of the cells by using an external magnetic field. However, the magnetism has not been introduced to individual living cells through the in situ chemical reactions because of harsh conditions required for synthesis of magnetic materials. In this work, magnetic iron oxide was formed on the surface of living cells by optimizing reactions conditions to be mild sufficiently enough to sustain cell viability. Specifically, the reactive LbL strategy led to formation of magnetically responsive yeast cells with iron oxide shells. This facile and direct post-magnetization method would be a useful tool for remote manipulation of living cells with magnetic interactions, which is an important technique for the integration of cell-based circuits and the isolation of cell in microfluidic devices.

  15. Enhanced performance of biodegradable poly(butylene succinate)/graphene oxide nanocomposites via in situ polymerization.

    Science.gov (United States)

    Wang, X W; Zhang, C-A; Wang, P L; Zhao, J; Zhang, W; Ji, J H; Hua, K; Zhou, J; Yang, X B; Li, X P

    2012-05-08

    Poly(butylene succinate) (PBS)/graphene oxide (GO) nanocomposites were facilely prepared via in situ polymerization. The properties of the nanocomposites were studied using FTIR, XRD, and (1)H NMR, and the state of dispersion of GO in the PBS matrix was examined by SEM. The crystallization and melting behavior of the PBS matrix in the presence of dispersed GO nanosheets have been studied by DSC and polarized optical microscopy. Through the mechnical testing machine and DMA, PBS/GO nanocomposites with 3% GO have shown a 43% increase in tensile strength and a 45% improvement in storage modulus. This high performance of the nanocomposites is mainly attributed to the high strength of graphene oxide combined with the strong interfacial interactions in the uniformly dispersed PBS/GO nanocomposites.

  16. In situ reduction of as-prepared γ-Iron Oxide Nanoparticles

    DEFF Research Database (Denmark)

    Garbus, Pelle Gorm; Ahlburg, Jakob; Christensen, Mogens

    -ray diffraction measurement. The as-prepared maghemite nanoparticles were synthesized by the continuous decomposition of solutes in supercritical hydrothermal flow synthesis [3, 4]. The reagent used was ferric ammonium citrate (C6H8O7•xFe(III)•yNH3) that under hydrothermal flow synthesis decomposes into the γ......-iron oxide Fe2O3. The reduction of maghemite to body centered cubic (BCC) iron does not go through a detectable intermediate state.1.Jensen, K.M., et al., Mechanisms for iron oxide formation under hydrothermal conditions: an in situ total scattering study. ACS nano, 2014. 8(10): p. 10704-10714.2.Andersen, H...

  17. Solidification of HLLW into sintered ceramics

    International Nuclear Information System (INIS)

    O-Oka, K.; Ohta, T.; Masuda, S.; Tsunoda, N.

    1979-01-01

    Simulated HLLW from the PNC reprocessing plant at Tokai was solidified into sintered ceramics by normal sintering or hot-pressing with addition of some oxides. Among various ceramic products obtained so far, the most preferable was nepheline-type sintered solids formed with addition of SiO 2 and Al 2 O 3 to the simulated waste calcine. The solid shows advantageous properties in leach rate and mechanical strength, which suggest that the ceramic solids were prepared with additions of ZrO 2 or MnO 2 , and some of them showed good characteristics

  18. In-situ TEM visualization of vacancy injection and chemical partition during oxidation of Ni-Cr nanoparticles.

    Science.gov (United States)

    Wang, Chong-Min; Genc, Arda; Cheng, Huikai; Pullan, Lee; Baer, Donald R; Bruemmer, Stephen M

    2014-01-14

    Oxidation of alloy often involves chemical partition and injection of vacancies. Chemical partition is the consequence of selective oxidation, while injection of vacancies is associated with the differences of diffusivity of cations and anions. It is far from clear as how the injected vacancies behave during oxidation of metal. Using in-situ transmission electron microscopy, we captured unprecedented details on the collective behavior of injected vacancies during oxidation of metal, featuring an initial multi-site oxide nucleation, vacancy supersaturation, nucleation of a single cavity, sinking of vacancies into the cavity and accelerated oxidation of the particle. High sensitive energy dispersive x-ray spectroscopy mapping reveals that Cr is preferentially oxidized even at the initial oxidation, leading to a structure that Cr oxide is sandwiched near the inner wall of the hollow particle. The work provides a general guidance on tailoring of nanostructured materials involving multi-ion exchange such as core-shell structured composite nanoparticles.

  19. Method for in situ carbon deposition measurement for solid oxide fuel cells

    Science.gov (United States)

    Kuhn, J.; Kesler, O.

    2014-01-01

    Previous methods to measure carbon deposition in solid oxide fuel cell (SOFC) anodes do not permit simultaneous electrochemical measurements. Electrochemical measurements supplemented with carbon deposition quantities create the opportunity to further understand how carbon affects SOFC performance and electrochemical impedance spectra (EIS). In this work, a method for measuring carbon in situ, named here as the quantification of gasified carbon (QGC), was developed. TGA experiments showed that carbon with a 100 h residence time in the SOFC was >99.8% gasified. Comparison of carbon mass measurements between the TGA and QGC show good agreement. In situ measurements of carbon deposition in SOFCs at varying molar steam/carbon ratios were performed to further validate the QGC method, and suppression of carbon deposition with increasing steam concentration was observed, in agreement with previous studies. The technique can be used to investigate in situ carbon deposition and gasification behavior simultaneously with electrochemical measurements for a variety of fuels and operating conditions, such as determining conditions under which incipient carbon deposition is reversible.

  20. In situ spectroscopic monitoring of CO2 reduction at copper oxide electrode.

    Science.gov (United States)

    Wang, Liying; Gupta, Kalyani; Goodall, Josephine B M; Darr, Jawwad A; Holt, Katherine B

    2017-04-28

    Copper oxide modified electrodes were investigated as a function of applied electrode potential using in situ infrared spectroscopy and ex situ Raman and X-ray photoelectron spectroscopy. In deoxygenated KHCO 3 electrolyte bicarbonate and carbonate species were found to adsorb to the electrode during reduction and the CuO was reduced to Cu(i) or Cu(0) species. Carbonate was incorporated into the structure and the CuO starting material was not regenerated on cycling to positive potentials. In contrast, in CO 2 saturated KHCO 3 solution, surface adsorption of bicarbonate and carbonate was not observed and adsorption of a carbonato-species was observed with in situ infrared spectroscopy. This species is believed to be activated, bent CO 2 . On cycling to negative potentials, larger reduction currents were observed in the presence of CO 2 ; however, less of the charge could be attributed to the reduction of CuO. In the presence of CO 2 CuO underwent reduction to Cu 2 O and potentially Cu, with no incorporation of carbonate. Under these conditions the CuO starting material could be regenerated by cycling to positive potentials.

  1. In-situ polymerization of polyaniline on the surface of graphene oxide for high electrochemical capacitance

    International Nuclear Information System (INIS)

    Li, Xinlu; Zhong, Qineng; Zhang, Xinlin; Li, Tongtao; Huang, Jiamu

    2015-01-01

    Conducting polymer polyaniline (PANI) was in-situ polymerized on the surface of graphene oxide (GO) to form PANI encapsulating GO nanocomposites. The morphology and microstructure were examined by scanning electron microscopy, X-ray diffraction and N 2 absorption/desorption analysis. Electrochemical properties were tested by cyclic voltammetry, galvanostatic charge/discharge cycles and electrochemical impedance spectroscopy. Experimental results showed that ethanol assisted the dispersion of GO in water and facilitated the diffusion of polymer monomers on GO. GO as a support material can provide sufficient reaction sites for the deposition of aniline to form the film-like GO/PANI composites. Capacitive performance illustrated that the in-situ polymerization of PANI on GO was effective in improving the specific capacitance and cycling stability. - Highlights: • GO/PANI nanocomposites were achieved by in-situ polymerization. • PANI was uniformly coated on the surface of GO with addition of ethanol. • GO/PANI show high specific capacitance and cycling stability

  2. TEM in situ micropillar compression tests of ion irradiated oxide dispersion strengthened alloy

    Energy Technology Data Exchange (ETDEWEB)

    Yano, K.H., E-mail: kaylayano@u.boisestate.edu [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Swenson, M.J. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Wu, Y. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Center for Advanced Energy Studies, 995 University Blvd, Idaho Falls, ID, 83401 (United States); Wharry, J.P. [Boise State University, 1910 University Drive, Boise, ID, 83725 (United States); Purdue University, 400 Central Drive, West Lafayette, IN 47907 (United States)

    2017-01-15

    The growing role of charged particle irradiation in the evaluation of nuclear reactor candidate materials requires the development of novel methods to assess mechanical properties in near-surface irradiation damage layers just a few micrometers thick. In situ transmission electron microscopic (TEM) mechanical testing is one such promising method. In this work, microcompression pillars are fabricated from a Fe{sup 2+} ion irradiated bulk specimen of a model Fe-9%Cr oxide dispersion strengthened (ODS) alloy. Yield strengths measured directly from TEM in situ compression tests are within expected values, and are consistent with predictions based on the irradiated microstructure. Measured elastic modulus values, once adjusted for the amount of deformation and deflection in the base material, are also within the expected range. A pillar size effect is only observed in samples with minimum dimension ≤100 nm due to the low inter-obstacle spacing in the as received and irradiated material. TEM in situ micropillar compression tests hold great promise for quantitatively determining mechanical properties of shallow ion-irradiated layers.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  4. Monitoring the in-situ oxide growth on uranium by ultraviolet-visible reflectance spectroscopy

    Science.gov (United States)

    Schweke, Danielle; Maimon, Chen; Chernia, Zelig; Livneh, Tsachi

    2012-11-01

    We demonstrate the in-situ monitoring of oxide growth on U-0.1 wt. % Cr by means of UV-visible reflectance spectroscopy in the thickness range of ˜20-150 nm. Two different approaches are presented: In the "modeling approach," we employ a model for a metallic substrate covered by a dielectric layer, while taking into account the buildup of oxygen gradient and surface roughness. Then, we fit the simulated spectra to the experimental one. In the "extrema analysis," we derive an approximated analytical expression, which relates the oxide thickness to the position of the extrema in the reflectance spectra based on the condition for optical interference of the reflected light. Good agreement is found between the values extracted by the two procedures. Activation energy of ˜21 kcal/mole was obtained by monitoring the oxide growth in the temperature range of 22-90 °C. The upper bound for the thickness determination is argued to be mostly dictated by cracking and detachment processes in the formed oxide.

  5. Control of manganese dioxide particles resulting from in situ chemical oxidation using permanganate.

    Science.gov (United States)

    Crimi, Michelle; Ko, Saebom

    2009-02-01

    In situ chemical oxidation using permanganate is an approach to organic contaminant site remediation. Manganese dioxide particles are products of permanganate reactions. These particles have the potential to deposit in the subsurface and impact the flow-regime in/around permanganate injection, including the well screen, filter pack, and the surrounding subsurface formation. Control of these particles can allow for improved oxidant injection and transport and contact between the oxidant and contaminants of concern. The goals of this research were to determine if MnO(2) can be stabilized/controlled in an aqueous phase, and to determine the dependence of particle stabilization on groundwater characteristics. Bench-scale experiments were conducted to study the ability of four stabilization aids (sodium hexametaphosphate (HMP), Dowfax 8390, xanthan gum, and gum arabic) in maintaining particles suspended in solution under varied reaction conditions and time. Variations included particle and stabilization aid concentrations, ionic content, and pH. HMP demonstrated the most promising results, as compared to xanthan gum, gum arabic, and Dowfax 8390 based on results of spectrophotometric studies of particle behavior, particle filtration, and optical measurements of particle size and zeta potential. HMP inhibited particle settling, provided for greater particle stability, and resulted in particles of a smaller average size over the range of experimental conditions evaluated compared to results for systems that did not include HMP. Additionally, HMP did not react unfavorably with permanganate. These results indicate that the inclusion of HMP in a permanganate oxidation system improves conditions that may facilitate particle transport.

  6. In-situ sequential laser transfer and laser reduction of graphene oxide films

    Science.gov (United States)

    Papazoglou, S.; Petridis, C.; Kymakis, E.; Kennou, S.; Raptis, Y. S.; Chatzandroulis, S.; Zergioti, I.

    2018-04-01

    Achieving high quality transfer of graphene on selected substrates is a priority in device fabrication, especially where drop-on-demand applications are involved. In this work, we report an in-situ, fast, simple, and one step process that resulted in the reduction, transfer, and fabrication of reduced graphene oxide-based humidity sensors, using picosecond laser pulses. By tuning the laser illumination parameters, we managed to implement the sequential printing and reduction of graphene oxide flakes. The overall process lasted only a few seconds compared to a few hours that our group has previously published. DC current measurements, X-Ray Photoelectron Spectroscopy, X-Ray Diffraction, and Raman Spectroscopy were employed in order to assess the efficiency of our approach. To demonstrate the applicability and the potential of the technique, laser printed reduced graphene oxide humidity sensors with a limit of detection of 1700 ppm are presented. The results demonstrated in this work provide a selective, rapid, and low-cost approach for sequential transfer and photochemical reduction of graphene oxide micro-patterns onto various substrates for flexible electronics and sensor applications.

  7. Deformation behavior of sintered nanocrystalline silver layers

    International Nuclear Information System (INIS)

    Zabihzadeh, S.; Van Petegem, S.; Duarte, L.I.; Mokso, R.; Cervellino, A.; Van Swygenhoven, H.

    2015-01-01

    The microstructure of porous silver layers produced under different low temperature pressure-assisted sintering conditions is characterized and linked with the mechanical behavior studied in situ during X-ray diffraction. Peak profile analysis reveals important strain recovery and hardening mechanism during cyclic deformation. The competition between both mechanisms is discussed in terms of porosity and grain size

  8. Effect of TiC content on the microstructure and properties of Ti3SiC2-TiC composites in situ fabricated by spark plasma sintering

    International Nuclear Information System (INIS)

    Zhang Jianfeng; Wang Lianjun; Jiang Wan; Chen Lidong

    2008-01-01

    Spark plasma sintering technique was used to in situ fabricate high dense Ti 3 SiC 2 -TiC composites. The calculated TiC volume content from X-ray diffraction (XRD) is close to the theoretical one. It is found from fracture surface observation that TiC is about 1 μm, and Ti 3 SiC 2 is about 2-10 μm in grain size. The fracture modes consist of intergranular mainly for Ti 3 SiC 2 and transgranular fracture mainly for TiC. With the increasing of TiC volume content, Vickers hardness increases to the maximum value of 13 GPa for Ti 3 SiC 2 -40 vol.%TiC. Fracture toughness and flexural strength of the composites are also improved compared with those of monolithic Ti 3 SiC 2 except for Ti 3 SiC 2 -40 vol.%TiC composite. The main reasons for the sudden decrease of fracture toughness and flexural strength of Ti 3 SiC 2 -40 vol.%TiC composite can be attributed to the relatively lower density, some clusters of TiC in the composite and the transition of fracture mode from intergranular to transgranular. The thermal conductivities decreased with the addition of TiC. The minimum thermal conductivity is 22 W m deg. C -1 for Ti 3 SiC 2 -40 vol.%TiC composite

  9. In Situ Bioremediation of 1,4-Dioxane by Methane Oxidizing Bacteria in Coupled Anaerobic-Aerobic Zones

    Science.gov (United States)

    2016-02-11

    FINAL REPORT In Situ Bioremediation of 1,4-Dioxane by Methane Oxidizing Bacteria in Coupled Anaerobic-Aerobic Zones SERDP Project ER-2306...volatile organic compound (CVOCs), ethene and ethane in groundwater at Raritan Arsenal Area 18C after in situ bioremediation . 4 List of...aquifers, the bioremediation approach most commonly used for chlorinated solvents. The ability of methanotrophs to biodegrade 1,4-dioxane was

  10. In-situ reduced graphene oxide-polyvinyl alcohol composite coatings as protective layers on magnesium substrates

    Directory of Open Access Journals (Sweden)

    Xingkai Zhang

    2017-06-01

    Full Text Available A simple and feasible method was developed to fabricate in-situ reduced graphene oxide-polyvinyl alcohol composite (GO-PVA coatings as protective layers on magnesium substrates. Polyvinyl alcohol was used as an in-situ reductant to transform GO into reduced GO. Contiguous and uniform GO-PVA coatings were prepared on magnesium substrates by dip-coating method, and were further thermally treated at 120 °C under ambient condition to obtain in-situ reduced GO-PVA coatings. Owing to the reducing effect of PVA, thermal treatment at low temperature led to effective in-situ reduction of GO as confirmed by XRD, Raman, FTIR and XPS tests. The corrosion current density of magnesium substrates in 3.5 wt% NaCl solution could be lowered to its 1/25 when using in-situ reduced GO-PVA coatings as protective layers.

  11. Constraining the relationships between anaerobic oxidation of methane and sulfate reduction under in situ methane concentrations

    Science.gov (United States)

    Zhuang, G.; Wegener, G.; Joye, S. B.

    2017-12-01

    The anaerobic oxidation of methane (AOM) is an important microbial metabolism in the global carbon cycle. In marine methane seeps sediment, this process is mediated by syntrophic consortium that includes anaerobic methanotrophic archaea (ANME) and sulfate-reducing bacteria (SRB). Stoichiometrically in AOM methane oxidation should be coupled to sulfate reduction (SR) in a 1:1 ratio. However, weak coupling of AOM and SR in seep sediments was frequently observed from the ex situ rate measurements, and the metabolic dynamics of AOM and SR under in situ conditions remain poorly understood. Here we investigated the metabolic activity of AOM and SR with radiotracers by restoring in situ methane concentrations under pressure to constrain the in situ relationships between AOM and SR in the cold seep sediments of Gulf of Mexico as well as the sediment-free AOM enrichments cultivated from cold seep of Italian Island Elba or hydrothermal vent of Guaymas Basin5. Surprisingly, we found that AOM rates strongly exceeded those of SR when high pressures and methane concentrations were applied at seep sites of GC600 and GC767 in Gulf of Mexico. With the addition of molybdate, SR was inhibited but AOM was not affected, suggesting the potential coupling of AOM with other terminal processes. Amendments of nitrate, iron, manganese and AQDS to the SR-inhibited slurries did not stimulate or inhibit the AOM activity, indicating either those electron acceptors were not limiting for AOM in the sediments or AOM was coupled to other process (e.g., organic matter). In the ANME enrichments, higher AOM rates were also observed with the addition of high concentrations of methane (10mM and 50 mM). The tracer transfer of CO2 to methane, i.e., the back reaction of AOM, increased with increasing methane concentrations and accounted for 1%-5% of the AOM rates. AOM rates at 10 mM and 50 mM methane concentration were much higher than the SR rates, suggesting those two processes were not tightly coupled

  12. In situ X-ray Rietveld analysis of Ni-YSZ solid oxide fuel cell anodes during NiO reduction in H2

    International Nuclear Information System (INIS)

    Reyes Rojas, A; Esparza-Ponce, H E; Fuentes, L; Lopez-Ortiz, A; Keer, A; Reyes-Gasga, J

    2005-01-01

    A synthesis and characterization of solid oxide fuel cell (SOFC) anodes of nickel with 8%mol yttrium stabilized zirconia (Ni-YSZ) is presented. Attention was focused on the kinetics and phase composition associated with the transformation of NiO-YSZ to Ni-YSZ. The anodes were prepared with an alternative synthesis method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 deg. C and oxide reduction (NiO-YSZ → Ni-YSZ) at 800 deg. C for 8 h in a tubular reactor furnace using 10% H 2 /N 2 . The obtained material was compressed by unidirectional axial pressing into 1 cm-diameter discs with 15-66 wt% Ni and calcinated from room temperature to 800 deg. C. A heating rate of 1 deg. C min -1 showed the best results to avoid any anode cracking. Their structural and chemical characterization during the isothermal reduction were carried out by in situ time-resolved X-ray diffraction, refined with the Rietveld method (which allowed knowing the kinetic process of the reduction), scanning electron microscopy and X-ray energy dispersive spectroscopy. The results showed the formation of tetragonal YSZ 8%mol in the presence of nickel, a decrement in the unit cell volume of Ni and an increment of Ni in the Ni-YSZ anodes during the temperature reduction. The analysis indicated that the Johnson-Mehl-Avrami equation is unable to provide a good fit to the kinetics of the phase transformation. Instead, an alternative equation is presented

  13. Hydrous pyrolysis/oxidation process for in situ destruction of chlorinated hydrocarbon and fuel hydrocarbon contaminants in water and soil

    Science.gov (United States)

    Knauss, Kevin G.; Copenhaver, Sally C.; Aines, Roger D.

    2000-01-01

    In situ hydrous pyrolysis/oxidation process is useful for in situ degradation of hydrocarbon water and soil contaminants. Fuel hydrocarbons, chlorinated hydrocarbons, polycyclic aromatic hydrocarbons, petroleum distillates and other organic contaminants present in the soil and water are degraded by the process involving hydrous pyrolysis/oxidation into non-toxic products of the degradation. The process uses heat which is distributed through soils and water, optionally combined with oxygen and/or hydrocarbon degradation catalysts, and is particularly useful for remediation of solvent, fuel or other industrially contaminated sites.

  14. Optimal Design and Operation of In-Situ Chemical Oxidation Using Stochastic Cost Optimization Toolkit

    Science.gov (United States)

    Kim, U.; Parker, J.; Borden, R. C.

    2014-12-01

    In-situ chemical oxidation (ISCO) has been applied at many dense non-aqueous phase liquid (DNAPL) contaminated sites. A stirred reactor-type model was developed that considers DNAPL dissolution using a field-scale mass transfer function, instantaneous reaction of oxidant with aqueous and adsorbed contaminant and with readily oxidizable natural oxygen demand ("fast NOD"), and second-order kinetic reactions with "slow NOD." DNAPL dissolution enhancement as a function of oxidant concentration and inhibition due to manganese dioxide precipitation during permanganate injection are included in the model. The DNAPL source area is divided into multiple treatment zones with different areas, depths, and contaminant masses based on site characterization data. The performance model is coupled with a cost module that involves a set of unit costs representing specific fixed and operating costs. Monitoring of groundwater and/or soil concentrations in each treatment zone is employed to assess ISCO performance and make real-time decisions on oxidant reinjection or ISCO termination. Key ISCO design variables include the oxidant concentration to be injected, time to begin performance monitoring, groundwater and/or soil contaminant concentrations to trigger reinjection or terminate ISCO, number of monitoring wells or geoprobe locations per treatment zone, number of samples per sampling event and location, and monitoring frequency. Design variables for each treatment zone may be optimized to minimize expected cost over a set of Monte Carlo simulations that consider uncertainty in site parameters. The model is incorporated in the Stochastic Cost Optimization Toolkit (SCOToolkit) program, which couples the ISCO model with a dissolved plume transport model and with modules for other remediation strategies. An example problem is presented that illustrates design tradeoffs required to deal with characterization and monitoring uncertainty. Monitoring soil concentration changes during ISCO

  15. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    International Nuclear Information System (INIS)

    Burke, Luke; Mortimer, Chris J.; Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri; Hawkins, Karl; Maffeis, Thierry G.G.; Wright, Chris J.

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  16. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Burke, Luke; Mortimer, Chris J. [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Hawkins, Karl [Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Maffeis, Thierry G.G. [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Wright, Chris J., E-mail: c.wright@swansea.ac.uk [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  17. Study and fabrication of solid oxide fuel cells through tape casting and co-sintering; Etude et realisation par coulage en bande et co-frittage de cellules de pile a combustible a oxydes solides

    Energy Technology Data Exchange (ETDEWEB)

    Grosjean, A

    2004-11-15

    This work is dedicated to the devising of a low-cost fabrication process of solid oxide fuel cells (SOFC). Technical requirements impose the shaping method: stripe casting as well as the materials used: Yttria-stabilized zirconia (YSZ), nickel and lanthanum manganite doped with strontium (LSM). In order to comply with environmental requirements the developed process uses an aqueous barbotine solvent. We get electrodes and the electrolyte separately, the use of an absorbent drying process has enabled us to join 3 layers to form an elementary cell with great interfacial homogeneity. The resistance of the cell to sintering has been improved through the symmetrization of the deformations of the cell. In order to interpret the low electrical properties of the cell and its quick damaging, transmission microscopy studies have been performed. These studies have shown 2 facts. First, 2 isolating phases appear at the cathode (at the LSM/YSZ interface) because of a too high sintering temperature and secondly, a quick clustering of nickel grains appears during cell operation that leads to a local loss of the nickel grid percolation. This problem has been solved by increasing the size of nickel oxide grains from 0.5 {mu}m to 3 {mu}m) to stabilize the microstructure. The issue of the reactivity at the LSM/YSZ interfaces was tackled in 2 different ways, we have tried to lower the sintering temperature by using a zirconia nano-powder first and then by replacing zirconia in the electrolyte by gadolinium-doped ceria. The use of zirconia nano-powder has failed to decrease sintering temperature while preserving the electrolyte density and the use of ceria has triggered instabilities that have not yet been solved. Despite all these drawbacks, this process allows the fabrication of an excellent anode/electrolyte interface. (A.C.)

  18. Oxidative Dehydrogenation on Nanocarbon: Insights into the Reaction Mechanism and Kinetics via in Situ Experimental Methods.

    Science.gov (United States)

    Qi, Wei; Yan, Pengqiang; Su, Dang Sheng

    2018-03-20

    Sustainable and environmentally benign catalytic processes are vital for the future to supply the world population with clean energy and industrial products. The replacement of conventional metal or metal oxide catalysts with earth abundant and renewable nonmetallic materials has attracted considerable research interests in the field of catalysis and material science. The stable and efficient catalytic performance of nanocarbon materials was discovered at the end of last century, and these materials are considered as potential alternatives for conventional metal-based catalysts. With its rapid development in the past 20 years, the research field of carbon catalysis has been experiencing a smooth transition from the discovery of novel nanocarbon materials or related new reaction systems to the atomistic-level mechanistic understanding on the catalytic process and the subsequent rational design of the practical catalytic reaction systems. In this Account, we summarize the recent progress in the kinetic and mechanistic studies on nanocarbon catalyzed alkane oxidative dehydrogenation (ODH) reactions. The paper attempts to extract general concepts and basic regularities for carbon catalytic process directing us on the way for rational design of novel efficient metal-free catalysts. The nature of the active sites for ODH reactions has been revealed through microcalorimetric analysis, ambient pressure X-ray photoelectron spectroscopy (XPS) measurement, and in situ chemical titration strategies. The detailed kinetic analysis and in situ catalyst structure characterization suggests that carbon catalyzed ODH reactions involve the redox cycles of the ketonic carbonyl-hydroxyl pairs, and the key physicochemical parameters (activation energy, reaction order, and rate/equilibrium constants, etc.) of the carbon catalytic systems are proposed and compared with conventional transition metal oxide catalysts. The proposal of the intrinsic catalytic activity (TOF) provides the

  19. Reduction Dynamics of Doped Ceria, Nickel Oxide, and Cermet Composites Probed Using In Situ Raman Spectroscopy.

    Science.gov (United States)

    Maher, Robert C; Shearing, Paul R; Brightman, Edward; Brett, Dan J L; Brandon, Nigel P; Cohen, Lesley F

    2016-01-01

    The redox properties of gadolinium doped ceria (CGO) and nickel oxide (NiO) composite cermets underpin the operation of solid oxide electrochemical cells. Although these systems have been widely studied, a full comprehension of the reaction dynamics at the interface of these materials is lacking. Here, in situ Raman spectroscopic monitoring of the redox cycle is used to investigate the interplay between the dynamic and competing processes of hydrogen spillover and water dissociation on the doped ceria surface. In order to elucidate these mechanisms, the redox process in pure CGO and NiO is studied when exposed to wet and dry hydrogen and is compared to the cermet behavior. In dry hydrogen, CGO reduces relatively rapidly via a series of intermediate phases, while NiO reduces via a single-step process. In wet reducing atmospheres, however, the oxidation state of pure CGO is initially stabilized due to the dissociation of water by reduced Ce(III) and subsequent incorporation of oxygen into the structure. In the reduction process involving the composite cermet, the close proximity of the NiO improves the efficiency and speed of the composite reduction process. Although NiO is already incorporated into working cells, these observations suggest direct routes to further improve cell performance.

  20. In situ examination of Lactobacillus brevis after exposure to an oxidizing disinfectant

    Directory of Open Access Journals (Sweden)

    Yu eZhao

    2014-11-01

    Full Text Available Beer is a hostile environment for most microorganisms, but some lactic acid bacteria can grow in this environment. This is primarily because these organisms have developed the ability to grow in the presence of hops. It has been speculated that hop resistance is inversely correlated to resistance against oxidation, and this would have great impact on the use of various disinfectants in the brewing industry. In this study, we cultivated bacteria under aerobic and anaerobic conditions, and then investigated the in situ outgrowth of individual cells into microcolonies on MRS agar after exposure to the oxidizing agent peracetic acid (PAA. An automated microscope stage allowed us to analyse a much larger number of cells over extended periods of incubation. After PAA treatment, the lag time increased markedly, and extensive variation in morphology, µmax as well as stress resistance was observed between and within the tested L. brevis strains. The results suggest that aerobic cultivation increased the oxidative stress tolerance in L. brevis. The results also show that dead cells are randomly distributed in a microcolony and the majority of non-growing individual cells do not stain with a membrane impermanent dye (Propidium iodide, which indicates that PAA may not destroy the plasma membrane. In conclusion, the developed microscopic analysis of individual cells on MRS agar can provides faster results and more details of cell physiology compared to the traditional CFU method.

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  2. A Reactive Oxide Overlayer on Rh Nanoparticles during CO Oxidation and Its Size Dependence Studied by in Situ Ambient Pressure XPS

    International Nuclear Information System (INIS)

    Grass, Michael E.; Zhang, Yawen; Butcher, Derek R.; Park, Jeong Y.; Li, Yimin; Bluhm, Hendrik; Bratlie, Kaitlin M.; Zhang, Tianfu; Somorjai, Gabor A.

    2008-01-01

    CO oxidation is one of the most studied heterogeneous reactions, being scientifically and industrially important, particularly for removal of CO from exhaust streams and preferential oxidation for hydrogen purification in fuel cell applications. The precious metals Ru, Rh, Pd, Pt, and Au are most commonly used for this reaction because of their high activity and stability. Despite the wealth of experimental and theoretical data, it remains unclear what is the active surface for CO oxidation under catalytic conditions for these metals. In this communication, we utilize in situ synchrotron ambient pressure X-ray photoelectron spectroscopy (APXPS) to monitor the oxidation state at the surface of Rh nanoparticles during CO oxidation and demonstrate that the active catalyst is a surface oxide, the formation of which is dependent on particle size. The amount of oxide formed and the reaction rate both increase with decreasing particle size.

  3. In Situ Synthesis of Reduced Graphene Oxide and Gold Nanocomposites for Nanoelectronics and Biosensing

    Directory of Open Access Journals (Sweden)

    Chen Peng

    2011-01-01

    Full Text Available Abstract In this study, an in situ chemical synthesis approach has been developed to prepare graphene–Au nanocomposites from chemically reduced graphene oxide (rGO in aqueous media. UV–Vis absorption, atomic force microscopy, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy were used to demonstrate the successful attachment of Au nanoparticles to graphene sheets. Configured as field-effect transistors (FETs, the as-synthesized single-layered rGO-Au nanocomposites exhibit higher hole mobility and conductance when compared to the rGO sheets, promising its applications in nanoelectronics. Furthermore, we demonstrate that the rGO-Au FETs are able to label-freely detect DNA hybridization with high sensitivity, indicating its potentials in nanoelectronic biosensing.

  4. In situ observation of Ag-Cu-Ti liquid alloy/solid oxide interfaces

    Energy Technology Data Exchange (ETDEWEB)

    Durov, O.V. [Frantsevich Institute for Problems of Materials Science of NASU, 3 Krzhyzhanovsky Street, Kiev 142, 03680 (Ukraine)], E-mail: avdu@ukr.net; Krasovskyy, V.P. [Frantsevich Institute for Problems of Materials Science of NASU, 3 Krzhyzhanovsky Street, Kiev 142, 03680 (Ukraine)

    2008-11-15

    In situ investigation methods are a very interesting means for understanding high-temperature interface processes. A method of direct observation of the interactions between transparent materials (Al{sub 2}O{sub 3}, SiO{sub 2}, CaF{sub 2}) and metal melts was elaborated. For the Ag-36.65 at.%Cu-8.15 at.%Ti/sapphire system, the formation of a dark compound at the interface was observed to occur at high temperature. This result does not confirm the conclusion of a neutron spectroscopy study which indicated that titanium oxides form at the interface only during solidification of the alloy. Interactions of the same alloy with SiO{sub 2} and CaF{sub 2} were also considered.

  5. In situ X-ray probing reveals fingerprints of surface platinum oxide.

    Science.gov (United States)

    Friebel, Daniel; Miller, Daniel J; O'Grady, Christopher P; Anniyev, Toyli; Bargar, John; Bergmann, Uwe; Ogasawara, Hirohito; Wikfeldt, Kjartan Thor; Pettersson, Lars G M; Nilsson, Anders

    2011-01-07

    In situ X-ray absorption spectroscopy (XAS) at the Pt L(3) edge is a useful probe for Pt-O interactions at polymer electrolyte membrane fuel cell (PEMFC) cathodes. We show that XAS using the high energy resolution fluorescence detection (HERFD) mode, applied to a well-defined monolayer Pt/Rh(111) sample where the bulk penetrating hard X-rays probe only surface Pt atoms, provides a unique sensitivity to structure and chemical bonding at the Pt-electrolyte interface. Ab initio multiple-scattering calculations using the FEFF code and complementary extended X-ray absorption fine structure (EXAFS) results indicate that the commonly observed large increase of the white-line at high electrochemical potentials on PEMFC cathodes originates from platinum oxide formation, whereas previously proposed chemisorbed oxygen-containing species merely give rise to subtle spectral changes.

  6. Preparation, Characterization, and Properties of In Situ Formed Graphene Oxide/Phenol Formaldehyde Nanocomposites

    Directory of Open Access Journals (Sweden)

    Weihua Xu

    2013-01-01

    Full Text Available Graphene oxide (GO has shown great potential to be used as fillers to develop polymer nanocomposites for important applications due to their special 2D geometrical structure as well as their outstanding mechanical, thermal, and electrical properties. In this work, GO was incorporated into phenol formaldehyde (PF resin by in situ polymerization. The morphologies and structures of GO sheets were characterized by FTIR, XRD, and AFM methods. The structure and properties of the GO/PF nanocomposites were characterized using FTIR, XRD, DSC, and TGA methods. Effects of GO content, reactive conditions, and blending methods on the structure and properties of GO/PF nanocomposites were studied. It was found that due to the well dispersion of GO sheets in polymer matrix and the strong interfacial interaction between the GO sheets and PF matrix, the thermal stability and thermal mechanical properties of the GO/PF nanocomposites were greatly enhanced.

  7. Penetrating the oxide barrier in situ and separating freestanding porous anodic alumina films in one step.

    Science.gov (United States)

    Tian, Mingliang; Xu, Shengyong; Wang, Jinguo; Kumar, Nitesh; Wertz, Eric; Li, Qi; Campbell, Paul M; Chan, Moses H W; Mallouk, Thomas E

    2005-04-01

    A simple method for penetrating the barrier layer of an anodic aluminum oxide (AAO) film and for detaching the AAO film from residual Al foil was developed by reversing the bias voltage in situ after the anodization process is completed. With this technique, we have been able to obtain large pieces of free-standing AAO membranes with regular pore sizes of sub-10 nm. By combining Ar ion milling and wetting enhancement processes, Au nanowires were grown in the sub-10 nm pores of the AAO films. Further scaling down of the pore size and extension to the deposition of nanowires and nanotubes of materials other than Au should be possible by further optimizing this procedure.

  8. Green synthesis of dimension-controlled silver nanoparticle–graphene oxide with in situ ultrasonication

    International Nuclear Information System (INIS)

    Hui, K.S.; Hui, K.N.; Dinh, D.A.; Tsang, C.H.; Cho, Y.R.; Zhou, Wei; Hong, Xiaoting; Chun, Ho-Hwan

    2014-01-01

    Graphical abstract: -- Abstract: A green chemical approach to control the dimensions of Ag nanoparticle-decorated graphene oxide (AgNP–GO) composites was proposed by in situ ultrasonication of a mixture of AgNO 3 and GO solution with the assistance of vitamin C acting as an environmentally friendly reducing agent at room temperature. The AgNP–GO composites were characterized by X-ray diffraction, transmission electron microscopy, energy-dispersive spectroscopy, Fourier transform infrared spectroscopy, Raman spectra and ultraviolet–visible absorption spectra. The results demonstrated that Ag nanoparticles with an average diameter of ∼15 nm were uniformly dispersed on the surface of GO nanosheets by in situ ultrasonication of 1 min with vitamin C. Increasing the ultrasonication times resulted in Ag nanoparticles with tunable dimensions ranging from 15 to 55 nm being formed on the surface of GO nanosheets. The amount of silver nitrate and the ultrasonication time play a key role in the control of the dimension of Ag nanoparticles on GO, and a formation mechanism of the as-prepared AgNP–GO composites is proposed. This study provides a guide to controlling the dimensions of AgNP–GO composites, which may hold promise as advanced materials for various analytical applications such as catalysis, sensors and microchips

  9. Growth and decay of a two-dimensional oxide quasicrystal: High-temperature in situ microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Foerster, Stefan [Physik-Institut, Universitaet Zuerich (Switzerland); Institute of Physics, Martin-Luther-Universitaet Halle-Wittenberg, Halle (Germany); Flege, Jan Ingo; Falta, Jens [Institute of Solid State Physics, University of Bremen (Germany); MAPEX Center for Materials and Processes, University of Bremen (Germany); Zollner, Eva Maria; Schumann, Florian Otto; Hammer, Rene; Bayat, Alireza; Schindler, Karl-Michael [Institute of Physics, Martin-Luther-Universitaet Halle-Wittenberg, Halle (Germany); Widdra, Wolf [Institute of Physics, Martin-Luther-Universitaet Halle-Wittenberg, Halle (Germany); Max-Planck-Institut fuer Mikrostrukturphysik, Halle (Germany)

    2017-01-15

    The recently discovered two-dimensional oxide quasicrystal (OQC) derived from BaTiO{sub 3} on Pt(111) is the first material in which a spontaneous formation of an aperiodic structure at the interface to a periodic support has been observed. Herein, we report in situ low-energy electron microscopy (LEEM) studies on the fundamental processes involved in the OQC growth. The OQC formation proceeds in two steps via of an amorphous two-dimensional wetting layer. At 1170 K the long-range aperiodic order of the OQC develops. Annealing in O{sub 2} induces the reverse process, the conversion of the OQC into BaTiO{sub 3} islands and bare Pt(111), which has been monitored by in situ LEEM. A quantitative analysis of the temporal decay of the OQC shows that oxygen adsorption on bare Pt patches is the rate limiting step of this dewetting process. (copyright 2016 by WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Plasma Jet Printing and in Situ Reduction of Highly Acidic Graphene Oxide.

    Science.gov (United States)

    Dey, Avishek; Krishnamurthy, Satheesh; Bowen, James; Nordlund, Dennis; Meyyappan, M; Gandhiraman, Ram P

    2018-05-23

    Miniaturization of electronic devices and the advancement of Internet of Things pose exciting challenges to develop technologies for patterned deposition of functional nanomaterials. Printed and flexible electronic devices and energy storage devices can be embedded onto clothing or other flexible surfaces. Graphene oxide (GO) has gained much attention in printed electronics due its solution processability, robustness, and high electrical conductivity in the reduced state. Here, we introduce an approach to print GO films from highly acidic suspensions with in situ reduction using an atmospheric pressure plasma jet. Low-temperature plasma of a He and H 2 mixture was used successfully to reduce a highly acidic GO suspension (pH < 2) in situ during deposition. This technique overcomes the multiple intermediate steps required to increase the conductivity of deposited GO. X-ray spectroscopic studies confirmed that the reaction intermediates and the concentration of oxygen functionalities bonded to GO have been reduced significantly by this approach without any additional steps. Moreover, the reduced GO films showed enhanced conductivity. Hence, this technique has a strong potential for printing conducting patterns of GO for a range of large-scale applications.

  11. IMPORTANCE OF IN SITU MONITORS IN THE PREPARATION OF LAYERED OXIDE HETEROSTRUCTURES BY REACTIVE MBE.

    Energy Technology Data Exchange (ETDEWEB)

    Schlom, Darrell G.; Haeni, J. H.; Theis, C. D. (Christopher); Tian, W.; Pan, X. Q.; Brown, G. W. (Geoffrey W.); Hawley, M. E. (Marilyn E.)

    2001-01-01

    Using a variety of in situ monitors and when possible adsorption-controlled growth conditions, layered oxide heterostructures including new compounds and metastable superlattices have been grown by reactive molecular beam epitaxy (MBE). The heteroepitaxial layers grown include Bi{sub 4}Ti{sub 3}O{sub 12}-SrTiO{sub 3} and Bi{sub 4}Ti{sub 3}O{sub 12}-PbTiO{sub 3} Aurivillius phases, Sr{sub n+1}Ti{sub n}O{sub 3n+1} Ruddlesden-Popper phases, and metastable PbTiO{sub 3}/SrTiO{sub 3} and BaTiO{sub 3}/SrTiO{sub 3} superlattices. Accurate composition control is key to the controlled growth of such structures, and to this end combinations of reflection high-energy electron diffraction (RHEED), atomic absorption spectroscopy (AA), a quartz crystal microbalance (QCM), and adsorption-controlled growth conditions were employed during growth. The structural perfection of the films has been investigated using in situ RHEED, four-circle x-ray diffraction, atomic force microscopy (AFM), and high-resolution transmission electron microscopy (TEM).

  12. In situ emulsion cationic polymerization of isoprene onto the surface of graphite oxide sheets

    Energy Technology Data Exchange (ETDEWEB)

    Pazat, Alice [Ingénierie des Matériaux Polymères, IMP, CNRS UMR 5223, Université Claude Bernard Lyon 1 and INSA de Lyon, 15 boulevard Latarjet, 69122 Villeurbanne cedex (France); Laboratoire de Recherches et de Contrôle du Caoutchouc et des Plastiques, LRCCP, 60 rue Auber, 94408 Vitry-sur-Seine cedex (France); Beyou, Emmanuel, E-mail: beyou@univ-lyon1.fr [Ingénierie des Matériaux Polymères, IMP, CNRS UMR 5223, Université Claude Bernard Lyon 1 and INSA de Lyon, 15 boulevard Latarjet, 69122 Villeurbanne cedex (France); Barrès, Claire [Ingénierie des Matériaux Polymères, IMP, CNRS UMR 5223, Université Claude Bernard Lyon 1 and INSA de Lyon, 15 boulevard Latarjet, 69122 Villeurbanne cedex (France); Bruno, Florence; Janin, Claude [Laboratoire de Recherches et de Contrôle du Caoutchouc et des Plastiques, LRCCP, 60 rue Auber, 94408 Vitry-sur-Seine cedex (France)

    2017-02-28

    Highlights: • Graphite oxide sheets were functionalized by polyisoprene in a two steps procedure. • The polyisoprene chains were grafted onto functionalized GO sheets by the grafting through technique. • A polyisoprene weight content of 50% was calculated from TGA measurements. • A decrease of the air permeability coefficient of 27% for the vulcanized PI composites has been reached. - Abstract: Grafting of polymers onto graphite oxide sheets (GO) has been widely studied in recent years due to the numerous applications of GO-based composites. Herein, polyisoprene (PI) chains were anchored on the surface of GO by in situ cationic polymerization using a “grafting through” approach with allyltrimethoxysilane-modified GO (GO-ATMS). First, the functionalization of GO sheets through the hydrolysis-condensation of allyltrimethoxysilane (ATMS) molecules was qualitatively evidenced by infra-red spectroscopy and X-ray photoelectron spectrometry and a weight content of 4% grafted ATMS was calculated from thermogravimetric analysis. Then, isoprene was in situ polymerized through a one-pot cationic mechanism by using a highly water-dispersible Lewis acid surfactant combined catalyst. For comparison, it was shown that the cationic polymerization of isoprene in presence of un-functionalized GO sheets led to a polyisoprene weight content on the solid filler divided by 3 compared to GO-ATMS. Finally, the compounding of the modified GO/PI composites was performed at a processing temperature of 80 °C with 2 phr and 15 phr loadings and it was shown a decrease of the air permeability coefficient of 27% for the vulcanizates with 15 phr loading.

  13. In situ emulsion cationic polymerization of isoprene onto the surface of graphite oxide sheets

    International Nuclear Information System (INIS)

    Pazat, Alice; Beyou, Emmanuel; Barrès, Claire; Bruno, Florence; Janin, Claude

    2017-01-01

    Highlights: • Graphite oxide sheets were functionalized by polyisoprene in a two steps procedure. • The polyisoprene chains were grafted onto functionalized GO sheets by the grafting through technique. • A polyisoprene weight content of 50% was calculated from TGA measurements. • A decrease of the air permeability coefficient of 27% for the vulcanized PI composites has been reached. - Abstract: Grafting of polymers onto graphite oxide sheets (GO) has been widely studied in recent years due to the numerous applications of GO-based composites. Herein, polyisoprene (PI) chains were anchored on the surface of GO by in situ cationic polymerization using a “grafting through” approach with allyltrimethoxysilane-modified GO (GO-ATMS). First, the functionalization of GO sheets through the hydrolysis-condensation of allyltrimethoxysilane (ATMS) molecules was qualitatively evidenced by infra-red spectroscopy and X-ray photoelectron spectrometry and a weight content of 4% grafted ATMS was calculated from thermogravimetric analysis. Then, isoprene was in situ polymerized through a one-pot cationic mechanism by using a highly water-dispersible Lewis acid surfactant combined catalyst. For comparison, it was shown that the cationic polymerization of isoprene in presence of un-functionalized GO sheets led to a polyisoprene weight content on the solid filler divided by 3 compared to GO-ATMS. Finally, the compounding of the modified GO/PI composites was performed at a processing temperature of 80 °C with 2 phr and 15 phr loadings and it was shown a decrease of the air permeability coefficient of 27% for the vulcanizates with 15 phr loading.

  14. Effects of in situ plasma treatment on optical and electrical properties of index-matched transparent conducting oxide layer

    International Nuclear Information System (INIS)

    Lim, Yong Hwan; Yoo, Hana; Choi, Bum Ho; Kim, Young Baek; Lee, Jong Ho; Shin, Dong Chan

    2010-01-01

    We investigated the effects of in situ plasma-treatment on optical and electrical properties of index-matched indium tin oxide (IMITO) thin film. To render the IMITO-coated surface hydrophilic and study the optical and electrical characteristics, we performed in situ oxygen plasma post-treatment without breaking vacuum. The 94.6% transmittance in the visible wavelength range (400-700 nm) increased on average to 96.4% and the maximum transmittance reached 98% over a broad wavelength range. The surface roughness and sheet resistance improved from 0.9 nm and 200 Ω/sq to 0.0905 nm and 100 Ω/sq, respectively, by in situ plasma post-treatment. We confirmed by contact angle measurement that the hydrophobic IMITO surface was altered to hydrophilic. The improved optical and electrical characteristics of in situ plasma-treated IMITO makes it adequate for high-resolution liquid crystal on silicon displays.

  15. In situ oxidation state profiling of nickel hexacyanoferrate derivatized electrodes using line-imaging Raman spectroscopy and multivariate calibration

    International Nuclear Information System (INIS)

    Haight, S.M.; Schwartz, D.T.

    1999-01-01

    Metal hexacyanoferrate compounds show promise as electrochemically switchable ion exchange materials for use in the cleanup of radioactive wastes such as those found in storage basins and underground tanks at the Department of Energy's Hanford Nuclear Reservation. Reported is the use of line-imaging Raman spectroscopy for the in situ determination of oxidation state profiles in nickel hexacyanoferrate derivatized electrodes under potential control in an electrochemical cell. Line-imaging Raman spectroscopy is used to collect 256 contiguous Raman spectra every ∼5 microm from thin films (ca. 80 nm) formed by electrochemical derivatization of nickel electrodes. The cyanide stretching region of the Raman spectrum of the film is shown to be sensitive to iron oxidation state and is modeled by both univariate and multivariate correlations. Although both correlations fit the calibration set well, the multivariate (principle component regression or PCR) model's predictions of oxidation state are less sensitive to noise in the spectrum, yielding a much smoother oxidation state profile than the univariate model. Oxidation state profiles with spatial resolution of approximately 5 microm are shown for a nickel hexacyanoferrate derivatized electrode in reduced, intermediate, and oxidized states. In situ oxidation state profiles indicate that the 647.1 nm laser illumination photo-oxidizes the derivatized electrodes. This observation is confirmed using photoelectrochemical methods

  16. Formation of high oxide ion conductive phases in the sintered oxides of the system Bi2O3-Ln2O3 (Ln = La-Yb)

    International Nuclear Information System (INIS)

    Iwahara, H.; Esaka, T.; Sato, T.; Takahashi, T.

    1981-01-01

    The electrical conduction in various phases of the system Bi 2 O 3 -Ln 2 O 3 (Ln = La, Nd, Sm, Dy, Er, or Yb) was investigated by measuring ac conductivity and the emf of the oxygen gas concentration cell. High-oxide-ion conduction was observed in the rhombohedral and face-centered cubic (fcc) phase in these systems. The fcc phase could be stabilized over a wide range of temperature by adding a certain amount of Ln 2 O 3 . In these cases, the larger the atomic number of Ln, the lower the content of Ln 2 O 3 required to form the fcc solid solution, except in the case of Yb 2 O 3 . The oxide ion conductivity of this phase decreased with increasing content of Ln 2 O 3 . Maximum conductivity was obtained at the lower limit of the fcc solid solution formation range in each system, which was more than one order of magnitude higher than those of conventional stabilized zirconias. Lattice parameters of the fcc phase were calculated from the x-ray diffraction patterns. The relationship between the oxide ion conductivity and the lattice parameter was also discussed

  17. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    Science.gov (United States)

    Wang, Jinlong; Yunus, Rizwangul; Li, Jinge; Li, Peilin; Zhang, Pengyi; Kim, Jeonghyun

    2015-12-01

    Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnOx) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnOx/PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnOx layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO4 and then surface-deposition of MnOx particles from the bulk phase. The MnOx particles assembled with nanosheets were uniformly coated on the PET fibers. MnOx/PET showed good activity for HCHO decomposition at room temperature which followed the Mars-van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m3, space velocity ∼17,000 h-1 and relative humidity∼50%. This research provides a facile method to deposit active MnOx onto polymers with low air resistance, and composite MnOx/PET material is promising for indoor air purification.

  18. In-situ synthesis and performance of titanium oxide/poly(methyl methacrylate) nanocomposites.

    Science.gov (United States)

    Bandugula, Uttam C; Clayton, L M; Harmon, J P; Kumar, Ashok

    2005-05-01

    Polymer nanocomposites have elicited extensive research efforts due to their potential to exhibit spectacular properties. They have immense potential and are befitting materials to serve as an ideal and futuristic alternative for varied applications. Poly(methyl methacrylate) (PMMA) and titanium oxide (TiO2) nanocomposites used in this study were fabricated by an in-situ free radical polymerization process. Three point bend tests were conducted with a modified universal microtribometer to evaluate fracture toughness. The results indicated that the stress intensity values increase as the concentration of titanium oxide increases up to 1 vol% and subsequently decrease at higher concentrations. Scanning electron microscopy (SEM) images of fracture surfaces afforded clues as to the possible deformation mechanism. Ultraviolet-visible spectroscopy (UV-vis) evaluated the degree of transparency of the nanocomposites. It was observed that samples became opaque as the concentration was increased beyond 0.01% volume fraction. X-ray diffraction characterized the TiO2 crystalline phase and Scherrer's equation was used to calculate the crystallite size. Among the concentrations considered the 3% volume fraction sample had the largest crystallite size. Finally, microhardness measurements further characterized the mechanical properties of the composites.

  19. In situ X-ray studies of film cathodes for solid oxide fuel cells

    International Nuclear Information System (INIS)

    Fuoss, Paul; Chang, Kee-Chul; You, Hoydoo

    2013-01-01

    Highlights: •Synchrotron X-rays are used to study in operando the structural and chemical changes of LSM and LSCF film cathodes during half-cell operations. •A-site and B-site cations actively segregate or desegregate on the changes of temperature, pO 2 , and electrochemical potential. •Chemical lattice expansions show that oxygen-cathode interface is the primary source of rate-limiting processes. •The surface and subsurface of the LSM and LSCF films have different oxidation-states due to vacancy concentration changes. •Liquid-phase infiltration and coarsening processes of cathode materials into porous YSZ electrolyte backbone were monitored by USAXS. -- Abstract: Synchrotron-based X-ray techniques have been used to study in situ the structural and chemical changes of film cathodes during half-cell operations. The X-ray techniques used include X-ray reflectivity (XR), total-reflection X-ray fluorescence (TXRF), high-resolution diffraction (HRD), ultra-small angle X-ray scattering (USAXS). The epitaxial thin film model cathodes for XR, TXRF, and HRD measurements are made by pulse laser deposition and porous film cathodes for USAX measurements are made by screen printing technique. The experimental results reviewed here include A-site and B-site segregations, lattice expansion, oxidation-state changes during cell operations and liquid-phase infiltration and coarsening of cathode to electrolyte backbone

  20. In-situ XPS analysis of oxidized and reduced plasma deposited ruthenium-based thin catalytic films

    Science.gov (United States)

    Balcerzak, Jacek; Redzynia, Wiktor; Tyczkowski, Jacek

    2017-12-01

    A novel in-situ study of the surface molecular structure of catalytically active ruthenium-based films subjected to the oxidation (in oxygen) and reduction (in hydrogen) was performed in a Cat-Cell reactor combined with a XPS spectrometer. The films were produced by the plasma deposition method (PEMOCVD). It was found that the films contained ruthenium at different oxidation states: metallic (Ru0), RuO2 (Ru+4), and other RuOx (Ru+x), of which content could be changed by the oxidation or reduction, depending on the process temperature. These results allow to predict the behavior of the Ru-based catalysts in different redox environments.

  1. Reduction of mixed Mn-Zr oxides: in situ XPS and XRD studies.

    Science.gov (United States)

    Bulavchenko, O A; Vinokurov, Z S; Afonasenko, T N; Tsyrul'nikov, P G; Tsybulya, S V; Saraev, A A; Kaichev, V V

    2015-09-21

    A series of mixed Mn-Zr oxides with different molar ratios Mn/Zr (0.1-9) have been prepared by coprecipitation of manganese and zirconium nitrates and characterized by X-ray diffraction (XRD) and BET methods. It has been found that at concentrations of Mn below 30 at%, the samples are single-phase solid solutions (MnxZr1-xO2-δ) based on a ZrO2 structure. X-ray photoelectron spectroscopy (XPS) measurements showed that manganese in these solutions exists mainly in the Mn(4+) state on the surface. An increase in Mn content mostly leads to an increase in the number of Mn cations in the structure of solid solutions; however, a part of the manganese cations form Mn2O3 and Mn3O4 in the crystalline and amorphous states. The reduction of these oxides with hydrogen was studied by a temperature-programmed reduction technique, in situ XRD, and near ambient pressure XPS in the temperature range from 100 to 650 °C. It was shown that the reduction of the solid solutions MnxZr1-xO2-δ proceeds via two stages. During the first stage, at temperatures between 100 and 500 °C, the Mn cations incorporated into the solid solutions MnxZr1-xO2-δ undergo partial reduction. During the second stage, at temperatures between 500 and 700 °C, Mn cations segregate on the surface of the solid solution. In the samples with more than 30 at% Mn, the reduction of manganese oxides was observed: Mn2O3 → Mn3O4 → MnO.

  2. In situ characterization of uranium and americium oxide solid solution formation for CRMP process: first combination of in situ XRD and XANES measurements.

    Science.gov (United States)

    Caisso, Marie; Picart, Sébastien; Belin, Renaud C; Lebreton, Florent; Martin, Philippe M; Dardenne, Kathy; Rothe, Jörg; Neuville, Daniel R; Delahaye, Thibaud; Ayral, André

    2015-04-14

    Transmutation of americium in heterogeneous mode through the use of U1-xAmxO2±δ ceramic pellets, also known as Americium Bearing Blankets (AmBB), has become a major research axis. Nevertheless, in order to consider future large-scale deployment, the processes involved in AmBB fabrication have to minimize fine particle dissemination, due to the presence of americium, which considerably increases the risk of contamination. New synthesis routes avoiding the use of pulverulent precursors are thus currently under development, such as the Calcined Resin Microsphere Pelletization (CRMP) process. It is based on the use of weak-acid resin (WAR) microspheres as precursors, loaded with actinide cations. After two specific calcinations under controlled atmospheres, resin microspheres are converted into oxide microspheres composed of a monophasic U1-xAmxO2±δ phase. Understanding the different mechanisms during thermal conversion, that lead to the release of organic matter and the formation of a solid solution, appear essential. By combining in situ techniques such as XRD and XAS, it has become possible to identify the key temperatures for oxide formation, and the corresponding oxidation states taken by uranium and americium during mineralization. This paper thus presents the first results on the mineralization of (U,Am) loaded resin microspheres into a solid solution, through in situ XAS analysis correlated with HT-XRD.

  3. Combined in situ zymography, immunofluorescence, and staining of iron oxide particles in paraffin-embedded, zinc-fixed tissue sections.

    Science.gov (United States)

    Haeckel, Akvile; Schoenzart, Lena; Appler, Franziska; Schnorr, Joerg; Taupitz, Matthias; Hamm, Bernd; Schellenberger, Eyk

    2012-01-01

    Superparamagnetic iron oxide particles are used as potent contrast agents in magnetic resonance imaging. In histology, these particles are frequently visualized by Prussian blue iron staining of aldehyde-fixed, paraffin-embedded tissues. Recently, zinc salt-based fixative was shown to preserve enzyme activity in paraffin-embedded tissues. In this study, we demonstrate that zinc fixation allows combining in situ zymography with fluorescence immunohistochemistry (IHC) and iron staining for advanced biologic investigation of iron oxide particle accumulation. Very small iron oxide particles, developed for magnetic resonance angiography, were applied intravenously to BALB/c nude mice. After 3 hours, spleens were explanted and subjected to zinc fixation and paraffin embedding. Cut tissue sections were further processed to in situ zymography, IHC, and Prussian blue staining procedures. The combination of in situ zymography as well as IHC with subsequent Prussian blue iron staining on zinc-fixed paraffin-embedded tissues resulted in excellent histologic images of enzyme activity, protease distribution, and iron oxide particle accumulation. The combination of all three stains on a single section allowed direct comparison with only moderate degradation of fluorescein isothiocyanate-labeled substrate. This protocol is useful for investigating the biologic environment of accumulating iron oxide particles, with excellent preservation of morphology.

  4. Effects of sintering atmosphere and initial particle size on sintering of gadolinia-doped ceria

    International Nuclear Information System (INIS)

    Batista, Rafael Morgado

    2014-01-01

    The effects of the sintering atmosphere and initial particle size on the sintering of ceria containing 10 mol% gadolinia (GdO 1.5 ) were systematically investigated. The main physical parameter was the specific surface area of the initial powders. Nanometric powders with three different specific surface areas were utilized, 210 m 2 /g, 36,2 m 2 /g e 7,4 m 2 /g. The influence on the densification, and micro structural evolution were evaluated. The starting sintering temperature was verified to decrease with increasing on the specific surface area of raw powders. The densification was accelerated for the materials with smaller particle size. Sintering paths for crystallite growth were obtained. Master sintering curves for gadolinium-doped ceria were constructed for all initial powders. A computational program was developed for this purpose. The results for apparent activation energy showed noticeable dependence with specific surface area. In this work, the apparent activation energy for densification increased with the initial particle size of powders. The evolution of the particle size distributions on non isothermal sintering was investigated by WPPM method. It was verified that the grain growth controlling mechanism on gadolinia doped ceria is the pore drag for initial stage and beginning of intermediate stage. The effects of the sintering atmosphere on the stoichiometry deviation of ceria, densification, microstructure evolution, and electrical conductivity were analyzed. Inert, oxidizing, and reducing atmospheres were utilized on this work. Deviations on ceria stoichiometry were verified on the bulk materials. The deviation verified was dependent of the specific surface area and sintering atmosphere. Higher reduction potential atmospheres increase Ce 3+ bulk concentration after sintering. Accelerated grain growth and lower electrical conductivities were verified when reduction reactions are significantly present on sintering. (author)

  5. In-situ XRD and EDS method study on the oxidation behaviour of Ni-Cu sulphide ore.

    Science.gov (United States)

    Li, Guangshi; Cheng, Hongwei; Xiong, Xiaolu; Lu, Xionggang; Xu, Cong; Lu, Changyuan; Zou, Xingli; Xu, Qian

    2017-06-12

    The oxidation mechanism of sulfides is the key issue during the sulphide-metallurgy process. In this study, the phase transformation and element migration were clearly demonstrated by in-situ laboratory-based X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS), respectively. The reaction sequence and a four-step oxidation mechanism were proposed and identified. The elemental distribution demonstrated that at a low temperature, the Fe atoms diffused outward and the Ni/Cu atoms migrated toward the inner core, whereas the opposite diffusion processes were observed at a higher temperature. Importantly, the unique visual presentation of the oxidation behaviour provided by the combination of in-situ XRD and EDS might be useful for optimising the process parameters to improve the Ni/Cu extraction efficiency during Ni-Cu sulphide metallurgy.

  6. Microwave sintering of nano size powder β-TCP bioceramics

    Directory of Open Access Journals (Sweden)

    Mirhadi B.

    2014-01-01

    Full Text Available A nano sized beta tricalcium phosphate (β-TCP powder was conventional sintered (CS and microwave sintered (MW, in order to obtain dense β-TCP ceramics. In this work the effect of microwave sintering conditions on the microstructure, phase composition and mechanical properties of materials based on tricalcium phosphate (TCP was investigated by SEM (scanning electron microscopyand XRD(X-ray diffraction and then compared with conventional sintered samples. Nano-size β-TCP powders with average grain size of 80 nm were prepared by the wet chemical precipitation method with calcium nitrate and diammonium hydrogen phosphate as calcium and phosphorus precursors, respectively. The precipitation process employed was also found to be suitable for the production of submicrometre β-TCP powder in situ. The β-TCP samples microwave (MW sintered for 15 min at 1100°C, with average grain size of 3μm, showed better densification, higher density and certainly higher hardness than samples conventionally sintered for 2 h at the same temperature. By comparing sintered and MW sintered β-TCP samples, it was concluded that MW sintered β-TCP samples have superior mechanical properties.

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

    International Nuclear Information System (INIS)

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

    2010-01-01

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

  8. Sintering of nonstoichiometric UO2

    International Nuclear Information System (INIS)

    Susnik, D.; Holc, J.

    1983-01-01

    Activated sintering of UO 2 pellets at 1100 deg C is described. In CO 2 atmosphere is UO 2 is nonstoichiometric and pellets from active UO 2 powders sinter at 900 deg C to high density. At 1100 deg C the final sintered density is practically achieved at heating on sintering temperature. After reduction and cooling in H 2 atmosphere which is followed sintering in CO 2 the structure is identical to the structured UO 2 pellets sintered at high temperature in H 2 . Density of activated sintered UO 2 pellets is stable, even after additional sintering at 1800 deg C. (author)

  9. Processing and microstructure characterisation of oxide dispersion strengthened Fe–14Cr–0.4Ti–0.25Y2O3 ferritic steels fabricated by spark plasma sintering

    International Nuclear Information System (INIS)

    Zhang, Hongtao; Huang, Yina; Ning, Huanpo; Williams, Ceri A.; London, Andrew J.; Dawson, Karl; Hong, Zuliang; Gorley, Michael J.; Grovenor, Chris R.M.; Tatlock, Gordon J.; Roberts, Steve G.; Reece, Michael J.; Yan, Haixue; Grant, Patrick S.

    2015-01-01

    Highlights: • Nanostructured ODS steels were successfully produced by SPS. • Presence of Y 2 Ti 2 O 7 nanoclusters was confirmed by synchrotron XRD and microscopy. • The chemistry of nanoclusters tested by ATP indicated they are Y–Ti–O oxides. - Abstract: Ferritic steels strengthened with Ti–Y–O nanoclusters are leading candidates for fission and fusion reactor components. A Fe–14Cr–0.4Ti + 0.25Y 2 O 3 (14YT) alloy was fabricated by mechanical alloying and subsequently consolidated by spark plasma sintering (SPS). The densification of the 14YT alloys significantly improved with an increase in the sintering temperature. Scanning electron microscopy and electron backscatter diffraction revealed that 14YT SPS-sintered at 1150 °C under 50 MPa for 5 min had a high density (99.6%), a random grain orientation and a bimodal grain size distribution (<500 nm and 1–20 μm). Synchrotron X-ray diffraction patterns showed bcc ferrite, Y 2 Ti 2 O 7 , FeO, and chromium carbides, while transmission electron microscopy and atom probe tomography showed uniformly dispersed Y 2 Ti 2 O 7 nanoclusters of <5 nm diameter and number density of 1.04 × 10 23 m −3 . Due to the very much shorter consolidation times and lower pressures used in SPS compared with the more usual hot isostatic pressing routes, SPS is shown to be a cost-effective technique for oxide dispersion strengthened (ODS) alloy manufacturing with microstructural features consistent with the best-performing ODS alloys

  10. From Oxygen Generation to Metals Production: In Situ Resource Utilization by Molten Oxide Electrolysis

    Science.gov (United States)

    Khetpal, Deepak; Ducret, Andrew C.; Sadoway, Donald R.

    2003-01-01

    For the exploration of other bodies in the solar system, electrochemical processing is arguably the most versatile technology for conversion of local resources into usable commodities: by electrolysis one can, in principle, produce (1) breathable oxygen, (2) silicon for the fabrication of solar cells, (3) various reactive metals for use as electrodes in advanced storage batteries, and (4) structural metals such as steel and aluminum. Even so, to date there has been no sustained effort to develop such processes, in part due to the inadequacy of the database. The objective here is to identify chemistries capable of sustaining molten oxide electrolysis in the cited applications and to examine the behavior of laboratory-scale cells designed to generate oxygen and to produce metal. The basic research includes the study of the underlying high-temperature physical chemistry of oxide melts representative of lunar regolith and of Martian soil. To move beyond empirical approaches to process development, the thermodynamic and transport properties of oxide melts are being studied to help set the limits of composition and temperature for the processing trials conducted in laboratory-scale electrolysis cells. The goal of this investigation is to deliver a working prototype cell that can use lunar regolith and Martian soil to produce breathable oxygen along with metal by-product. Additionally, the process can be generalized to permit adaptation to accommodate different feedstock chemistries, such as those that will be encountered on other bodies in the solar system. The expected results of this research include: (1) the identification of appropriate electrolyte chemistries; (2) the selection of candidate anode and cathode materials compatible with electrolytes named above; and (3) performance data from a laboratory-scale cell producing oxygen and metal. On the strength of these results it should be possible to assess the technical viability of molten oxide electrolysis for in

  11. Guideline tests on the corrosion of sintered uranium oxide by lead and sodium about 450 deg. C; Essais d'orientation sur la corrosion de l'oxyde d'uranium fritte par le plomb et le sodium aux environs de 450 deg. C

    Energy Technology Data Exchange (ETDEWEB)

    Portnoff, A.; Pointud, R.

    1958-05-15

    Within the frame of the investigation of behaviour of a fuel element (such as UO{sub 2}) under irradiation, the authors report the study of the physical-chemical action of the coolant at different temperatures on the body to be irradiated. Thus, sintered uranium oxide has been submitted to corrosion by lead and by sodium during 250 hours at temperatures between 400 and 500 C. The physical characteristics of the UO{sub 2} powder and of different sintered UO{sub 2} pellets produced from this powder under different sintering processes are indicated, as well as the results of a spectrographic analysis of the sintered UO{sub 2}. Corrosion devices, treatments and obtained results are reported for corrosion by lead and by sodium. In the latter case, extraction processes are discussed (using butyl alcohol, or melting in vaseline oil)

  12. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    International Nuclear Information System (INIS)

    Wang, Jinlong; Yunus, Rizwangul; Li, Jinge; Li, Peilin; Zhang, Pengyi; Kim, Jeonghyun

    2015-01-01

    Graphical abstract: - Highlights: • The MnO x particles assembled with nanosheets were uniformly coated on PET fibers. • The growth process of MnO x layer on PET is clearly clarified. • MnO x /PET showed good activity for HCHO decomposition at room temperature. • MnO x /PET material is promising for indoor air purification due to its light, flexible and low air-resistant properties. - Abstract: Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnO x ) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnO x /PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnO x layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO 4 and then surface-deposition of MnO x particles from the bulk phase. The MnO x particles assembled with nanosheets were uniformly coated on the PET fibers. MnO x /PET showed good activity for HCHO decomposition at room temperature which followed the Mars–van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m 3 , space velocity ∼17,000 h −1 and relative humidity∼50%. This research provides a facile method to deposit active MnO x onto polymers with low air resistance, and composite MnO x /PET material is promising for indoor air purification.

  13. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jinlong [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China); Yunus, Rizwangul [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Xinjiang Zhongtai Chemical Company, Xinjiang 831511 (China); Li, Jinge; Li, Peilin [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Zhang, Pengyi, E-mail: zpy@tsinghua.edu.cn [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China); Kim, Jeonghyun [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China)

    2015-12-01

    Graphical abstract: - Highlights: • The MnO{sub x} particles assembled with nanosheets were uniformly coated on PET fibers. • The growth process of MnO{sub x} layer on PET is clearly clarified. • MnO{sub x}/PET showed good activity for HCHO decomposition at room temperature. • MnO{sub x}/PET material is promising for indoor air purification due to its light, flexible and low air-resistant properties. - Abstract: Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnO{sub x}) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnO{sub x}/PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnO{sub x} layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO{sub 4} and then surface-deposition of MnO{sub x} particles from the bulk phase. The MnO{sub x} particles assembled with nanosheets were uniformly coated on the PET fibers. MnO{sub x}/PET showed good activity for HCHO decomposition at room temperature which followed the Mars–van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m{sup 3}, space velocity ∼17,000 h{sup −1} and relative humidity∼50%. This research provides a facile method to deposit active MnO{sub x} onto polymers with low air resistance, and composite MnO{sub x}/PET material is promising for indoor air purification.

  14. In Situ Chemical Oxidation Through Lance Permeation at the Portsmouth Gaseous Diffusion Plant (PORTS)

    International Nuclear Information System (INIS)

    Martin, M.Z.

    2003-01-01

    In situ chemical oxidation through lance permeation (ISCO-LP) is an emerging remediation technology in which chemical oxidants (such as potassium or sodium permanganate) are delivered to the subsurface using vertical lance-like injectors. It is applicable to sites with oxidizable contaminants such as chlorinated solvents and fuel hydrocarbons. Because vertical lance injections can be deployed at relatively close spacing, ISCO-LP potentially can be used to clean-up contamination in low-permeability media. This document provides information that can help potential users determine whether ISCO-LP would apply to a particular environmental management problem. It contains a general description of the technology (Section 2), performance data from a field demonstration (Section 3), an assessment of technology applicability (Section 4), a summary of cost elements (Section 5), and a list of regulatory, environmental safety and health issues (Section 6). It is patterned after the Innovative Technology Summary Reports (ITSR) published by the Department of Energy's (DOE) Office of Science and Technology under the Subsurface Contaminants Focus Area (SCFA). As in the previously published ITSRs, the technology described in this report was developed through funding from SCFA. Most of the information contained in this report was obtained from a field demonstration of ISCO-LP conducted in July-August 2000 at DOE's Portsmouth Gaseous Diffusion Plant (PORTS). The field test was not completed due to an accident that caused a field worker serious injuries. Although performance assessment data are very limited, the field test highlighted important health and safety issues that must be considered by site managers and technology vendors interested in implementing ISCO-LP

  15. Physical deoxygenation of graphene oxide paper surface and facile in situ synthesis of graphene based ZnO films

    International Nuclear Information System (INIS)

    Ding, Jijun; Wang, Minqiang; Zhang, Xiangyu; Ran, Chenxin; Shao, Jinyou; Ding, Yucheng

    2014-01-01

    In-situ sputtering ZnO films on graphene oxide (GO) paper are used to fabricate graphene based ZnO films. Crystal structure and surface chemical states are investigated. Results indicated that GO paper can be effectively deoxygenated by in-situ sputtering ZnO on them without adding any reducing agent. Based on the principle of radio frequency magnetron sputtering, we propose that during magnetron sputtering process, plasma streams contain large numbers of electrons. These electrons not only collide with argon atoms to produce secondary electrons but also they are accelerated to bombard the substrates (GO paper) resulting in effective deoxygenation of oxygen-containing functional groups. In-situ sputtering ZnO films on GO paper provide an approach to design graphene-semiconductor nanocomposites

  16. In situ chemical oxidative polymerization preparation of poly(3,4-ethylenedioxythiophene)/graphene nanocomposites with enhanced thermoelectric performance.

    Science.gov (United States)

    Xu, Kongli; Chen, Guangming; Qiu, Dong

    2015-05-01

    Three different in situ chemical oxidative polymerization routes, that is, (A) spin-coating and subsequent liquid layer polymerization, (B) spin-coating followed by vapor phase polymerization, and (C) in situ polymerization and then post-treatment by immersion in ethylene glycol (EG), have been developed to achieve poly(3,4-ethylenedioxythiophene)/reduced graphene oxide (PEDOT/rGO) nanocomposites. As demonstrated by scanning electron microscopic and energy-dispersive X-ray spectroscopic techniques, PEDOT has been successfully coated on the surface of the rGO nanosheets by each of the three preparation routes. Importantly, all of the nanocomposites display a greatly enhanced thermoelectric performance (power factors) relative to those of the corresponding neat PEDOT. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Effect of coating density on oxidation resistance and Cr vaporization from solid oxide fuel cell interconnects

    Science.gov (United States)

    Talic, Belma; Falk-Windisch, Hannes; Venkatachalam, Vinothini; Hendriksen, Peter Vang; Wiik, Kjell; Lein, Hilde Lea

    2017-06-01

    Manganese cobalt spinel oxides are promising materials for protective coatings for solid oxide fuel cell (SOFC) interconnects. To achieve high density such coatings are often sintered in a two-step procedure, involving heat treatment first in reducing and then in oxidizing atmospheres. Sintering the coating inside the SOFC stack during heating would reduce production costs, but may result in a lower coating density. The importance of coating density is here assessed by characterization of the oxidation kinetics and Cr evaporation of Crofer 22 APU with MnCo1.7Fe0.3O4 spinel coatings of different density. The coating density is shown to have minor influence on the long-term oxidation behavior in air at 800 °C, evaluated over 5000 h. Sintering the spinel coating in air at 900 °C, equivalent to an in-situ heat treatment, leads to an 88% reduction of the Cr evaporation rate of Crofer 22 APU in air-3% H2O at 800 °C. The air sintered spinel coating is initially highly porous, however, densifies with time in interaction with the alloy. A two-step reduction and re-oxidation heat treatment results in a denser coating, which reduces Cr evaporation by 97%.

  18. In Situ Treatment Train for Remediation of Perfluoroalkyl Contaminated Groundwater: In Situ Chemical Oxidation of Sorbed Contaminants (ISCO SC)

    Science.gov (United States)

    2017-07-18

    viable. Enzymes are employed in natural and engineered systems to overcome reaction energy barriers and thus may be a promising solution. For... Chemical and Engineering Data, 52(4), 1165–1170. http://doi.org/10.1021/je060285g Johnson, R. L., Tratnyek, P. G., & Johnson, R. O. B. (2008...persulfates by carbon nanotubes: Oxidation of organic compounds by nonradical mechanism. Chemical Engineering Journal, 266, 28–33. http://doi.org/10.1016

  19. A study of the kinetics and mechanisms of electrocrystallization of indium oxide on an in situ prepared metallic indium electrode

    International Nuclear Information System (INIS)

    Omanovic, S.; Metikos-Hukovic, M.

    2004-01-01

    The mechanisms and kinetics of nucleation and growth of indium oxide film on an in situ prepared metallic indium electrode was studied in a borate buffer solution of pH 10.0 using cyclic voltammetry and chroanoamperometry techniques. It was shown that the initial stage of nucleation of the oxide film includes a three-dimensional progressive nucleation process, combined with a diffusion-controlled growth of the stable indium oxide crystals. The thermodynamic data obtained indicated a strong tendency of indium to form an indium oxide film on its surface in an aqueous solution. It was found that the rate-determining step in the nucleation and growth process is the surface diffusion of electroactive species. The nucleation rate constant, and the number of nucleation active sites were calculated independently. It was shown that between 2 and 15% of sites on the indium surface act as active nucleation centers, and that each active site represents a critical nucleus

  20. Preparation and properties of in situ amino-functionalized graphene oxide/polyimide composite films

    Science.gov (United States)

    Lu, Yunhua; Hao, Jican; Xiao, Guoyong; Chen, Lin; Wang, Tonghua; Hu, Zhizhi

    2017-11-01

    The pure light-colored and transparent polyimide (PI) film was prepared from aromatic dianhydride 4,4‧-(hexafluoroisopropylidene)diphthalic anhydride (6FDA) and diamine 1,4-bis(4-amino-2-trifluoromethylphenoxy)benzene (6FAPB) in the solvent of DMAc via two-step method. Graphene oxide (GO) was in situ grafted with 6FAPB and directly used as a functional inorganic nanofiller to further synthesize poly(amic acid) (PAA)/GO solution. Then, PI/GO composite films with different loadings of GO were prepared by the thermal imidization. The mechanical, thermal, optical, electrical, surface properties, and electrochemical behavior were characterized. The FTIR and XPS results indicate that amino groups can be successfully grafted on the surface of GO. The tensile strength and Young's modulus of the PI-1.0%GO composite film were increased to 118.4 MPa and 2.91 GPa, respectively, which was an approximate improvement of 30.8% and 39.9% compared with pure PI film. These PI/GO composites showed around 256 °C for the glass transition temperature, and around 535 °C for the 5% thermal decomposition temperature, respectively. However, the optical transmittance was significantly decreased from 81.5% (pure PI) to 0.8% (PI-1.0%GO). Besides, the electrical conductivity increased from 1.6 × 10-13 S/m (pure PI) to 2.5 × 10-9 S/m (PI-1.0%GO). Furthermore, when the incorporation of GO was 1.0 wt%, an obvious reduction from 1.08% (pure PI) to 0.65% in the water uptake was observed for the PI/GO composite films, and the water surface contact angle raised from 72.5° (pure PI) to 83.5°. The electrochemical behavior showed that the ability of oxygen atom on the imide ring to gain and loss electron was increased due to incorporation of GO. These results indicated that the strong interfacial interaction between GO and PAA as well as uniform dispersion of GO in PI matrix were benefit to improve the mechanical, thermal, electrical properties and so on. The in situ amino-functionalized approach

  1. Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

    Science.gov (United States)

    Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

    2013-02-01

    The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH)3) to bixbyite-type indium oxide (c-In2O3). The electron beam is focused onto a single cube-shaped In(OH)3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In2O3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at 10.1016/j.jssc.2012.09.022. After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH)3 is transformed to a diffuse strongly textured ring-like pattern of c-In2O3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In2O3 domains with the size of about 5-10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In2O3), calculated from the shrinkage of the parent c-In(OH)3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In2O3 crystallization within the framework of Avrami-Erofeev formalism. The Avrami exponent of ˜3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive decomposition of c-In(OH)3 to c

  2. Science of sintering

    International Nuclear Information System (INIS)

    Kuczynski, G.

    1977-01-01

    Although the methods of integration of materials by sintering, have been used since the early history of humanity, the actual understanding of the process involved came only in the last three decades. As in the most human endeavors, the art preceded theory. The comprehension of the elementary processes occuring during sintering comes from the studies of model system. Although the elementary processes occuring during sintering are today quite well understood, the problem of shrinkage of a powder compact which was at the origin of Sintering Science is still far from solved. This is due to the complexity of the internal geometry of the compacts. The recent attempts to apply statistics to this problem, seem to offer some promise

  3. Uranium dioxide. Sintering test

    International Nuclear Information System (INIS)

    Anon.

    Description of a sintering method and of the equipment devoted to uranium dioxide powder caracterization and comparison between different samples. Determination of the curve giving specific volume versus pressure and micrographic examination of a pellet at medium pressure [fr

  4. Kinetics of UO2 sintering

    International Nuclear Information System (INIS)

    Ristic, M.M.

    1962-01-01

    Detailed conclusions related to the UO 2 sintering can be drawn from investigating the kinetics of the sintering process. This report gives an thorough analysis of the the data concerned with sintering available in the literature taking into account the Jander and Arrhenius laws. This analysis completes the study of influence of the O/U ratio and the atmosphere on the sintering. Results presented are fundamentals of future theoretical and experimental work related to characterisation of the UO 2 sintering process

  5. Indium hydroxide to oxide decomposition observed in one nanocrystal during in situ transmission electron microscopy studies

    International Nuclear Information System (INIS)

    Miehe, Gerhard; Lauterbach, Stefan; Kleebe, Hans-Joachim; Gurlo, Aleksander

    2013-01-01

    The high-resolution transmission electron microscopy (HR-TEM) is used to study, in situ, spatially resolved decomposition in individual nanocrystals of metal hydroxides and oxyhydroxides. This case study reports on the decomposition of indium hydroxide (c-In(OH) 3 ) to bixbyite-type indium oxide (c-In 2 O 3 ). The electron beam is focused onto a single cube-shaped In(OH) 3 crystal of {100} morphology with ca. 35 nm edge length and a sequence of HR-TEM images was recorded during electron beam irradiation. The frame-by-frame analysis of video sequences allows for the in situ, time-resolved observation of the shape and orientation of the transformed crystals, which in turn enables the evaluation of the kinetics of c-In 2 O 3 crystallization. Supplementary material (video of the transformation) related to this article can be found online at (10.1016/j.jssc.2012.09.022). After irradiation the shape of the parent cube-shaped crystal is preserved, however, its linear dimension (edge) is reduced by the factor 1.20. The corresponding spotted selected area electron diffraction (SAED) pattern representing zone [001] of c-In(OH) 3 is transformed to a diffuse strongly textured ring-like pattern of c-In 2 O 3 that indicates the transformed cube is no longer a single crystal but is disintegrated into individual c-In 2 O 3 domains with the size of about 5–10 nm. The induction time of approximately 15 s is estimated from the time-resolved Fourier transforms. The volume fraction of the transformed phase (c-In 2 O 3 ), calculated from the shrinkage of the parent c-In(OH) 3 crystal in the recorded HR-TEM images, is used as a measure of the kinetics of c-In 2 O 3 crystallization within the framework of Avrami–Erofeev formalism. The Avrami exponent of ∼3 is characteristic for a reaction mechanism with fast nucleation at the beginning of the reaction and subsequent three-dimensional growth of nuclei with a constant growth rate. The structural transformation path in reconstructive

  6. Investigation of the Sintering Process Using Non-Contact Electromagnetic Acoustic Transducers

    International Nuclear Information System (INIS)

    James C. Foley; David K. Rehbein; Daniel J. Barnard

    2001-01-01

    In-situ characterizations of green state part density and sintering state have long been desired in the powder metal community. Recent advances in non-contact electromagnetic acoustic transducer (EMAT) technology have enabled in-situ monitoring of acoustic amplitude and velocity as sintering proceeds. Samples were made from elemental powders of Al (99.99%), Al (99.7%), Ag, (99.99%), Cu (99.99%) and Fe (99.9%). The powders were pressed in a uniaxial die and examined with acoustic waves for changes in velocity and amplitude during sintering for the samples containing Al, Ag, and Cu. The changes in acoustic properties were correlated with sample microstructures and mechanical properties. Evolution of a series of reverberating echoes during sintering is shown to provide information on the state of sintering, and changes in sintering kinetics as well as having the potential for detection of interior flaws

  7. Short Communication on "In-situ TEM ion irradiation investigations on U3Si2 at LWR temperatures"

    Science.gov (United States)

    Miao, Yinbin; Harp, Jason; Mo, Kun; Bhattacharya, Sumit; Baldo, Peter; Yacout, Abdellatif M.

    2017-02-01

    The radiation-induced amorphization of U3Si2 was investigated by in-situ transmission electron microscopy using 1 MeV Kr ion irradiation. Both arc-melted and sintered U3Si2 specimens were irradiated at room temperature to confirm the similarity in their responses to radiation. The sintered specimens were then irradiated at 350 °C and 550 °C up to 7.2 × 1015 ions/cm2 to examine their amorphization behavior under light water reactor (LWR) conditions. U3Si2 remains crystalline under irradiation at LWR temperatures. Oxidation of the material was observed at high irradiation doses.

  8. In situ fabrication of blue ceramic coatings on wrought Al Alloy 2024 by plasma electrolytic oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Wang Zhijiang; Nie Xueyuan; Hu, Henry; Hussein, Riyad O. [Department of Mechanical, Automotive and Materials Engineering, University of Windsor, Windsor, Ontario N9B 3P4 (Canada)

    2012-03-15

    In situ formation of ceramic coatings on 2024 Al alloy with a blue color was successfully achieved using a plasma electrolytic oxidation process working at atmospheric pressure. This novel blue ceramic coating overcomes the shortcomings of surface treatments resulting from conventional dyeing processes by depositing organic dyes into the porous structure of anodic film, which has poor resistance to abrasion and rapid fading when exposed to sunlight. X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy were employed to characterize the microstructure of the blue ceramic coating. The fabricated ceramic coating was composed of CoAl{sub 2}O{sub 4}, {alpha}-Al{sub 2}O{sub 3}, and {gamma}-Al{sub 2}O{sub 3.} By controlling the working parameters, the distribution of the CoAl{sub 2}O{sub 4} phase on the surface can be adjusted, and plays a key role in the appearance of the coating. Electrochemical testing, thermal cycling method, and pin-on-disk sliding wear testing were employed to evaluate corrosion, thermal cycling, and wear resistance of the ceramic coatings. The results indicate that the blue ceramic coating has a similar polarization resistance to that of conventional anodic film and can significantly enhance the corrosion resistance of aluminum alloy. There are no destructive horizontal cracks observed within the blue ceramic coating when subjected to 120 times of thermal cycling, which heats the samples up to 573 K and followed by submersion in water at room temperature for 10 min. Compared with the aluminum substrate as well as a conventional anodic film coated aluminum sample, the wear resistance of the blue ceramic coating coated sample was significantly increased while the coefficient of friction was decreased from 0.34 to 0.14.

  9. In situ fabrication of blue ceramic coatings on wrought Al Alloy 2024 by plasma electrolytic oxidation

    International Nuclear Information System (INIS)

    Wang Zhijiang; Nie Xueyuan; Hu, Henry; Hussein, Riyad O.

    2012-01-01

    In situ formation of ceramic coatings on 2024 Al alloy with a blue color was successfully achieved using a plasma electrolytic oxidation process working at atmospheric pressure. This novel blue ceramic coating overcomes the shortcomings of surface treatments resulting from conventional dyeing processes by depositing organic dyes into the porous structure of anodic film, which has poor resistance to abrasion and rapid fading when exposed to sunlight. X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy were employed to characterize the microstructure of the blue ceramic coating. The fabricated ceramic coating was composed of CoAl 2 O 4 , α-Al 2 O 3 , and γ-Al 2 O 3. By controlling the working parameters, the distribution of the CoAl 2 O 4 phase on the surface can be adjusted, and plays a key role in the appearance of the coating. Electrochemical testing, thermal cycling method, and pin-on-disk sliding wear testing were employed to evaluate corrosion, thermal cycling, and wear resistance of the ceramic coatings. The results indicate that the blue ceramic coating has a similar polarization resistance to that of conventional anodic film and can significantly enhance the corrosion resistance of aluminum alloy. There are no destructive horizontal cracks observed within the blue ceramic coating when subjected to 120 times of thermal cycling, which heats the samples up to 573 K and followed by submersion in water at room temperature for 10 min. Compared with the aluminum substrate as well as a conventional anodic film coated aluminum sample, the wear resistance of the blue ceramic coating coated sample was significantly increased while the coefficient of friction was decreased from 0.34 to 0.14.

  10. In-situ GISAXS study on the oxidation behavior of liquid Ga on Ni(Cu)/Si substrates

    Energy Technology Data Exchange (ETDEWEB)

    Cheng, Weidong [College of Materials Science and Engineering, Qiqihar University, Qiqihar 161006 (China); Liu, Mingling [Department of Mechanical and Electrical Engineering, Qinhuangdao Institute of Technology, Qinhuangdao 066100 (China); Wu, Zhaojun [Department of Practice Teaching and Equipment Management, Qiqihar University, Qiqihar 161006 (China); Xing, Xueqing; Mo, Guang; Wu, Zhonghua [Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049 (China); Liu, Hong, E-mail: lhong68@sina.com.cn [School of Biomedical Engineering, Capital Medical University, Beijing 100069 (China)

    2015-11-01

    Liquid Ga could be used as a flexible heat-transfer medium or contact medium in the synchrotron-radiation-based instruments. The chemical stability of liquid Ga on other metal surface determines the serviceability of liquid Ga. In this paper, the oxidation evolutions of liquid Ga on Ni and Cu substrates have been investigated by in-situ grazing incidence small angle X-ray scattering (GISAXS) as a function of substrate temperature. The liquid Ga on Ni and Cu substrates shows different oxidation behaviors. A successive and slower oxidation from oxide clusters to oxide layer takes place with temperature increasing from 25 to 190 °C on the surface of the Ga/Ni/Si specimen, but a quick oxidation occurs on the entire surface of the Ga/Cu/Si specimen at the initial 25 °C. The subsequent heating increases the surface roughness of both liquid Ga, but increases simultaneously the surface curvature of the Ga/Cu/Si specimen. The understanding of the substrate-dependent oxidation behavior of liquid Ga is beneficial to its application as a heat-transfer medium.

  11. Predicting sintering deformation of ceramic film constrained by rigid substrate using anisotropic constitutive law

    International Nuclear Information System (INIS)

    Li Fan; Pan Jingzhe; Guillon, Olivier; Cocks, Alan

    2010-01-01

    Sintering of ceramic films on a solid substrate is an important technology for fabricating a range of products, including solid oxide fuel cells, micro-electronic PZT films and protective coatings. There is clear evidence that the constrained sintering process is anisotropic in nature. This paper presents a study of the constrained sintering deformation using an anisotropic constitutive law. The state of the material is described using the sintering strains rather than the relative density. In the limiting case of free sintering, the constitutive law reduces to a conventional isotropic constitutive law. The anisotropic constitutive law is used to calculate sintering deformation of a constrained film bonded to a rigid substrate and the compressive stress required in a sinter-forging experiment to achieve zero lateral shrinkage. The results are compared with experimental data in the literature. It is shown that the anisotropic constitutive law can capture the behaviour of the materials observed in the sintering experiments.

  12. Characterization of oxidation resistance of stainless steels at high temperature by metallographic examinations and in-situ electrical resistance measurements; Charakterisierung der Oxidationsbestaendigkeit in nichtrostenden Staehlen bei hoher Temperatur durch Metallographische Untersuchungen und In-Situ-Messungen des elektrischen Widerstands

    Energy Technology Data Exchange (ETDEWEB)

    Bruncko, Mihael; Rudolf, Rebeka; Anzel, Ivan [Maribor Univ. (Slovenia). Faculty of Mechanical Engineering; Mehrabi, Kambiz [Pankl Drivetrain Systems GmbH und Co. KG, Kapfenberg (Austria); Kneissl, Albert C. [Leoben Univ. (Austria). Dept. of Physical Metallurgy and Materials Testing

    2013-07-01

    Practically all metals and alloys survive high-temperature exposure by growing oxide scales and/or by precipitation of the oxide particles in the matrix. Formed products can grow in shape of external oxide layers on surfaces, or as discrete oxide particles precipitated in a metal matrix. The first case represents external oxidation, and the other case is called internal oxidation. These processes are very important, because they determine the properties and applicability of metallic materials. Generally, they are undesired, because they cause deterioration of the mechanical properties and decomposition of metallic material. On the other side, the controlled process of external oxidation could be used for formation of protective coatings and the internal oxidation for dispersion strengthening of materials. In this paper we present monitoring of high-temperature oxidation of X12Cr13 stainless steel by in-situ electrical resistance measurements at different annealing temperatures in the air atmosphere. We determined the kinetics of oxide scale formation and its morphology with additional metallographic examination made by optical and scanning electron microscopy. The results of this research work show that in-situ monitoring and characterization of high-temperature oxidation present a strong tool that will contribute to a better fundamental understanding of the phenomena that occur during high-temperature oxidation of metallic materials. (orig.)

  13. In Situ Analysis of the Li-O2 Battery with Thermally Reduced Graphene Oxide Cathode: Influence of Water Addition

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Christensen, Mathias Kjærgård; Younesi, Reza

    2016-01-01

    The Li-O2 battery technology holds the promise to deliver a battery with significantly increased specific energy compared to today's Li-ion batteries. As a cathode support material, reduced graphene oxide has received increasing attention in the Li-O2 battery community due to the possibility...... of increased discharge capacity, increased battery cyclability, and decreased, charging, overpotential. In this. article we investigate the effect of water on a thermally, redircedigraphene, oxide cathode in a Li-O2 battery. Differential electrochemical mass spectrciscnieveals a, decreased electron count......-of-the cathode and not only on addition of water to the electrolyte as demonstrated by the solution-based mechanism In situ synchrotron X-ray diffraction experiment using a new design of a capillary-based Li-O2 cell with a thermally reduced graphene oxide cathode shows formation of LiOH along with Li2O2....

  14. Pressure sintering and creep deformation: a joint modeling approach

    International Nuclear Information System (INIS)

    Notis, M.R.

    1979-10-01

    Work related to microchemical and microstructural aspects of the joint modeling of pressure sintering and creep in ceramic oxides is reported. Quantitative techniques for the microchemical analysis of ceramic oxides and for the examination of impurity segregation effects in polycrystalline ceramic materials were developed. This has included fundamental absorption corrections for the oxygen anion species as a function of foil thickness. The evolution in microstructure during the transition from intermediate stage to final stage densification during hot pressing of cobalt oxide and preliminary studies with doped oxides were studied. This work shows promise in using time-integrated microstructural effects to elucidate the role of impurities in the sintering of ceramic materials

  15. In situ photoelectrochemistry and Raman spectroscopic characterization on the surface oxide film of nickel electrode in 30 wt.% KOH solution

    International Nuclear Information System (INIS)

    Nan Junmin; Yang Yong; Lin Zugeng

    2006-01-01

    The oxide films of nickel electrode formed in 30 wt.% KOH solution under potentiodynamic conditions were characterized by means of electrochemical, in situ PhotoElectrochemistry Measurement (PEM) and Confocal Microprobe Raman spectroscopic techniques. The results showed that a composite oxide film was produced on nickel electrode, in which aroused cathodic or anodic photocurrent depending upon polarization potentials. The cathodic photocurrent at -0.8 V was raised from the amorphous film containing nickel hydroxide and nickel monoxide, and mainly attributed to the formation of NiO through the separation of the cavity and electron when laser light irradiates nickel electrode. With the potential increasing to more positive values, Ni 3 O 4 and high-valence nickel oxides with the structure of NiO 2 were formed successively. The composite film formed in positive potential aroused anodic photocurrent from 0.33 V. The anodic photocurrent was attributed the formation of oxygen through the cavity reaction with hydroxyl on solution interface. In addition, it is demonstrated that the reduction resultants of high-valence nickel oxides were amorphous, and the oxide film could not be reduced completely. A stable oxide film could be gradually formed on the surface of nickel electrode with the cycling and aging in 30 wt.% KOH solution

  16. Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

    Energy Technology Data Exchange (ETDEWEB)

    Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H, E-mail: dasilva.ac@uol.com.br [Instituto de Pesquisas Enegeticas e Nucleares (IPEN/CNEN-SP), DP (Brazil); Braga, F.J.C. [Consulmat Materiais de Referencia, Solucoes e Servicos, Sao Carlos, SP (Brazil); Setz, L.F.G. [Universidade Federal do ABC (UFABC), Santo Andre, SP (Brazil)

    2014-07-01

    Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

  17. Dispersed hydroxyapatite and modified bioglass 45S5 composites: sintering behavior of glass matrix ranging from 20 to 30 wt% in calcium oxide investigation

    International Nuclear Information System (INIS)

    Silva, A.C.; Parra-Silva, J.; Santos, S.C.; Mello-Castanho, S.R.H; Braga, F.J.C.; Setz, L.F.G.

    2014-01-01

    Biomaterial technology plays an important role in cell-based tissue proliferation environment creation. The hydroxyapatite (HA) bioceramics are reference materials to employment as a bone substitute, however, their slow rate of degradation and its low rate of bioactivity (Ib) are presented as limiting factors for application as bone graft. In contrast, the bioglass (BG) is a resorbable and osteoinductive material and can act as fluxing in HA/BG composites. The present work objective the development of HA/BG (40/70wt%) composites, Three compositions of the 45S5 bioglass derived ranging from 20-30wt% in CaO were used in order to study the sintering behavior of these materials with hydroxyapatite 30wt% dispersed. The composites were uniaxially pressed in the form of cylinders and sinterized at (1100°C/1h). The characterization was made employing scanning electron microscopy, Infra-Red Spectrometry, X-ray diffraction and hydrolytic resistance test. The results indicate the potential use of the materials developed for applications like bone graft.(author)

  18. Morphological analysis and modelling of sintering and of sintered materials

    International Nuclear Information System (INIS)

    Jernot, Jean-Paul

    1982-01-01

    This research thesis addresses the study of solid phase sintering of metallic powders, and aims at describing as precisely as possible the different involved matter transport mechanisms, first by using a thermodynamic approach to sintering. Sintering diagrams are also used to determine prevailing mechanisms. The microstructure of sintered materials has been studied by using image quantitative analysis, thus by using a morphological approach to sintering. Morphological parameters allow, on the one hand, the evolution of powders during sintering to be followed, and, on the other hand, sintered products to be correctly characterised. Moreover, the author reports the study of the evolution of some physical properties of sintered materials with respect to their microstructure parameters. This leads to the development of a modelling of the behaviour of these materials [fr

  19. The influence of green microstructure and sintering parameters on precipitation process during copper-nickel-zinc ferrites sintering

    International Nuclear Information System (INIS)

    Barba, A.; Clausell, C.; Jarque, J. C.; Monzo, M.

    2014-01-01

    Microstructural changes that occur during heat treatment of copper-nickel-zinc ferrites have been studied. The process of precipitation of the two types of crystals that occur during the sintering process has been analyzed. It is found that this process depends on dry relative density of the press specimens and on the following sintering parameters: sintering temperature, sintering time and cooling rate of the thermal cycle. Crystal precipitates characterization have been done by scanning electron microscopy (SEM), energy-dispersive X-ray (EDX) analysis, X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS). These techniques have allowed to determine the nature of these crystals, which in this case correspond to zinc and copper oxides. It has been used two chemical reactions to explain the bulk precipitation and subsequent re-dissolution of these crystal precipitates during sintering. (Author)

  20. Study of the oxidation risks during the sintering of uranium dioxide, and characterization of the excess oxygen; Etude du risque d'oxydation lors du frittage du bioxyde d'uranium et caracterisation de l'oxygene excedentaire

    Energy Technology Data Exchange (ETDEWEB)

    Conte, M; Brandela, M

    1966-05-01

    During sintering in reducing atmospheres, UO{sub 2} pellets can be oxidized by gaseous impurities. The effects of temperature cycles, the partial pressure of O{sub 2} and the flow rate of the gas over the pellets were investigated. In these atmospheres, the O{sub 2} partial pressure during sintering is low at high temperatures, as a consequence of the dissociation rate of the combined water, but below 1000 deg C, it can be high enough to result in a noticeable oxidation of the surface of the pellets during cooling. The crystalline phases which can occur have been identified and two methods of detection have been proposed: a micrographic examination after chemical etching and radiocrystallography. (authors) [French] Lors du frittage industriel du bioxyde d'uranium en atmosphere reductrice (hydrogene ou ammoniac dissocie) la presence d'impuretes oxydantes dans l'atmosphere peut provoquer l'oxydation des pastilles d'UO{sub 2}; les auteurs ont etudie les phenomenes en faisant varier le cycle de temperature, la pression partielle d'oxygene introduit dans l'hydrogene, la vitesse de passage du gaz sur les pastilles. Dans les atmospheres considerees la pression partielle d'oxygene au-dessus de l'UO{sub 2} en cours de frittage est faible a temperature elevee car elle resulte de la dissociation de l'eau formee, mais a t < 1000 degrees C elle, peut etre assez importante pour provoquer une oxydation notable de la surface des pastilles lors du refroidissement. Les phases cristallines susceptibles d'etre formees ont ete reperees et deux methodes de detection proposees: la micrographie apres attaque chimique specifique et la radiocristallographie. (auteurs)

  1. Sintering of composite

    International Nuclear Information System (INIS)

    Bordia, R.K.; Scherer, G.W.

    1988-01-01

    Several constitutive laws have been used in the literature to predict the response of sintering bodies under external and internal stress fields. These analyses are based on the assumptions of linear and isotropic behavior. The authors provide a critical examination of these equations and show that some of the available constitutive laws predict a negative Poisson's ratio. These laws have been used to analyze sintering of ceramic matrix composites with rigid inclusions and predict large values of the internal stresses and significant retardation of the densification of composites. Since a negative value of Poisson's ratio has never been observed in sinter - forging experiments, the authors conclude that either the stresses are small (as predicted by the constitutive laws with positive Poisson's ratio) or the basic assumption of linearity and isotropy used in all the analyses is incorrect. Finally, the authors discuss some phenomena that could be important in understanding the densification of ceramic matrix composites

  2. Design of Magnetic Gelatine/Silica Nanocomposites by Nanoemulsification: Encapsulation versus in Situ Growth of Iron Oxide Colloids

    Directory of Open Access Journals (Sweden)

    Joachim Allouche

    2014-07-01

    Full Text Available The design of magnetic nanoparticles by incorporation of iron oxide colloids within gelatine/silica hybrid nanoparticles has been performed for the first time through a nanoemulsion route using the encapsulation of pre-formed magnetite nanocrystals and the in situ precipitation of ferrous/ferric ions. The first method leads to bi-continuous hybrid nanocomposites containing a limited amount of well-dispersed magnetite colloids. In contrast, the second approach allows the formation of gelatine-silica core-shell nanostructures incorporating larger amounts of agglomerated iron oxide colloids. Both magnetic nanocomposites exhibit similar superparamagnetic behaviors. Whereas nanocomposites obtained via an in situ approach show a strong tendency to aggregate in solution, the encapsulation route allows further surface modification of the magnetic nanocomposites, leading to quaternary gold/iron oxide/silica/gelatine nanoparticles. Hence, such a first-time rational combination of nano-emulsion, nanocrystallization and sol-gel chemistry allows the elaboration of multi-component functional nanomaterials. This constitutes a step forward in the design of more complex bio-nanoplatforms.

  3. Manufacture of nano graphite oxides derived from aqueous glucose solutions and in-situ synthesis of magnetite–graphite oxide composites

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Xiang, E-mail: liuxiang@ahut.edu.cn; Zhao, Tiantian; Liu, Pengpeng; Cui, Ping, E-mail: cokecp@sohu.com; Hu, Peng

    2015-03-01

    A “bottom up” approach of manufacturing graphite oxides (GOs) derived from aqueous glucose solutions by virtue of an environmentally-friendly process and the way of in-situ synthesizing magnetite–GOs composites are described in this work in detail. The dehydrations among glucose molecules under hydrothermal condition result in the initial carbon quantum dots and ultimate GOs. The structural information of the GOs is obtained by the infrared, ultraviolet–visible and X-ray photoelectron spectra. The magnetite–GOs composites were obtained by a one-pot method under the same hydrothermal conditions as the one of preparing GOs. The composites perform high activities in catalytic degradation of Rhodamine B in the presence of hydrogen peroxides without extra heating or pH adjusting. Both the GOs and the magnetite–GOs composites are also assured by measurements of transmission electron microscope and X-ray powder diffraction. - Highlights: • Graphite oxides are made from aqueous glucose solutions by hydrothermal reaction. • A way of in-situ synthesizing composites of magnetite–graphite oxides is depicted. • The composites perform high activities in catalytic degradation of Rhodamine B.

  4. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    International Nuclear Information System (INIS)

    Chen, Nali; Ren, Yapeng; Kong, Peipei; Tan, Lin; Feng, Huixia; Luo, Yongchun

    2017-01-01

    Highlights: • A new method to prepare reduced graphene oxide/polyaniline composite is developed. • Aniline serves as a reduction for graphene oxide under weak alkali condition. • Different characterizations confirm that GO can be effectively reduced by aniline. • A high specific capacitance of 524.4 F·g"−"1 is obtained at 0.5 A·g"−"1. - Abstract: Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  5. In situ one-pot preparation of reduced graphene oxide/polyaniline composite for high-performance electrochemical capacitors

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Nali [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Ren, Yapeng; Kong, Peipei; Tan, Lin [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Feng, Huixia, E-mail: fenghx@lut.cn [College of Petrochemical Technology, Lanzhou University of Technology, Lanzhou 730050, Gansu (China); Luo, Yongchun, E-mail: luoyc@lut.cn [State Key Laboratory of Advanced Processing and Recycling of Nonferrous Metals, Lanzhou University of Technology, Lanzhou 730050, Gansu (China)

    2017-01-15

    Highlights: • A new method to prepare reduced graphene oxide/polyaniline composite is developed. • Aniline serves as a reduction for graphene oxide under weak alkali condition. • Different characterizations confirm that GO can be effectively reduced by aniline. • A high specific capacitance of 524.4 F·g{sup −1} is obtained at 0.5 A·g{sup −1}. - Abstract: Reduced graphene oxide/polyaniline (rGO/PANI) composites are prepared through an effective in situ one-pot synthesis route that includes the reduction of graphene oxide (GO) by aniline under weak alkali condition via hydrothermal method and then followed by in situ polymerization of aniline. X-ray diffraction, Fourier transform infrared spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, X-ray photoelectron spectroscopy, scanning electron microscope and transmission electron microscope are employed to reveal that GO is successfully reduced by aniline under weak alkali condition and PANI can be deposited on the surfaces of reduced graphene oxide (rGO) sheets. The effect of rGO is optimized by tuning the mass ratios of aniline to GO to improve the electrochemical performance of rGO/PANI composites. The maximum specific capacitance of rGO/PANI composites achieves 524.4 F/g with a mass ratio of aniline to GO 10:1 at a current density of 0.5 A/g, in comparison to the specific capacitance of 397 F/g at the same current density of pure PANI. Particularly, the specific capacity retention rate is 81.1% after 2000 cycles at 100 mv/s scan rate, which is an improvement over that of pure PANI (55.5%).

  6. Enhanced permanganate in situ chemical oxidation through MnO2 particle stabilization: evaluation in 1-D transport systems.

    Science.gov (United States)

    Crimi, Michelle; Quickel, Mark; Ko, Saebom

    2009-02-27

    In situ chemical oxidation using permanganate is an increasingly employed approach to organic contaminant remediation at hazardous waste sites. Manganese dioxide (MnO2) particles form as a by-product of the reaction of permanganate with contaminants and naturally-reduced subsurface materials. These particles are of interest because they have the potential to deposit in the subsurface and impact the flow regime in/around permanganate injection, including the well screen, filter pack, and the surrounding subsurface formation. Control of these particles can allow for improved oxidant injection and transport, and contact between the oxidant and contaminants of concern. Sodium hexametaphosphate (HMP) has previously been identified as a promising aid to stabilize MnO2 in solution when included in the oxidizing solution, increasing the potential to inhibit particle deposition and impact subsurface flow. The goal of the experimental studies described herein was to investigate the ability of HMP to prevent particle deposition in transport studies using four different types of porous media. Permanganate was delivered to a contaminant source zone (trichloroethylene) located within four different media types with variations in sand, clay, organic carbon, and iron oxides (as goethite) content. Deposition of MnO2 within the columns was quantified with distance from the source zone. Experiments were repeated in replicate columns with the inclusion of HMP directly with the oxidant delivery solution, and MnO2 deposition was again quantified. While total MnO2 deposition within the 60 cm columns did not change significantly with the addition of HMP, deposition within the contaminant source zone decreased by 25-85%, depending on the specific media type. The greatest differences in deposition were observed in the goethite-containing and clay-containing columns. Columns containing these two media types experienced completely plugged flow in the oxidant-only delivery systems; however

  7. Mechanistic studies of chemical looping desulfurization of Mn-based oxides using in situ X-ray absorption spectroscopy

    International Nuclear Information System (INIS)

    König, C.F.J.; Nachtegaal, M.; Seemann, M.; Clemens, F.; Garderen, N. van; Biollaz, S.M.A.; Schildhauer, T.J.

    2014-01-01

    Highlights: • Mn sorbents remove H 2 S from hot syngas in chemical looping desulfurization process. • State of Mn followed by in situ X-ray absorption spectroscopy and mass spectrometry. • Two-step mechanism explains the formation of SO 2 under reducing conditions. - Abstract: Cleaning of producer gas from biomass gasification is required for further processing, e.g. to avoid catalyst poisoning in subsequent conversion steps. High-temperature gas cleaning, of which sulfur removal is an important part, is a promising way to improve the overall efficiency of biomass conversion. In a high temperature “chemical looping desulfurization” process, a sorbent material, here manganese oxide, is cycled between producer gas from the gasifier to remove sulfur species, and an oxidizing atmosphere, in which the sulfur species are released as SO 2 . Alternatively, the use of such material as reactive bed material could be integrated into an allothermal dual fluidized bed gasifier. In a laboratory reactor, we subjected manganese-based materials to a periodically changing gas atmosphere, simulating a “chemical looping desulfurization” reactor. The “fuel reactor” gas contained H 2 , CO, CH 4 and H 2 S, similar as in the producer gas, and the “oxidizing reactor” contained diluted O 2 . Mass spectrometry showed that most of the H 2 S is taken up by the sample in the “fuel reactor” part, while also some unwanted SO 2 is generated in the “fuel reactor” part. Most of the sulfur is released in the oxidizing reactor. Simultaneous in situ X-ray absorption spectroscopy (XAS) of the Mn materials during different stages of the chemical looping desulfurization process showed that the initial Mn 3 O 4 is transformed in the presence of H 2 S to MnS via a MnO intermediate in the fuel reactor. Oxygen from the reduction of Mn 3 O 4 oxidizes some H 2 S to the undesired SO 2 in the fuel reactor. Upon exposure to O 2 , MnS is again oxidized to Mn 3 O 4 via MnO, releasing SO

  8. Non-pressurized sintered silicon carbide with titanium carbide reinforcement

    International Nuclear Information System (INIS)

    Adler, J.

    1992-01-01

    A non-pressurized compression of SiC-TiC composite materials can be achieved via liquid phase sintering by the application of oxidic additives. Materials with TiC proportions up to 40% by volume of TiC and densities of 97 to 98% TD were produced at sintering temperatures around 1875 C. With SiC sintered in the liquid phase an increase of toughness at fracture of 80% compared with conventionally non-pressurized sintered SiC was achieved with B/C additive. No further increase could be achieved by the addition of TiC particles. However, the oxidation resistance at 1200 C was worsened. (orig.) [de

  9. Modeling sintering of multilayers under influence of gravity

    DEFF Research Database (Denmark)

    Frandsen, Henrik Lund; Olevsky, Eugene; Tadesse Molla, Tesfaye

    2013-01-01

    , which describes the combined effect of sintering and gravity of thin multilayers, is derived and later compared with experimental results. It allows for consideration of both uniaxial and biaxial stress states. The model is based on the Skorohod-Olevsky viscous sintering framework, the classical...... laminate theory and the elastic-viscoelastic correspondence principle. The modeling approach is then applied to illustrate the effect of gravity during sintering of thin layers of cerium gadolinium oxide (CGO), and it is found to be significant. © 2012 The American Ceramic Society....

  10. Low temperature spark plasma sintering of YIG powders

    International Nuclear Information System (INIS)

    Fernandez-Garcia, L.; Suarez, M.; Menendez, J.L.

    2010-01-01

    A transition from a low to a high spin state in the magnetization saturation between 1000 and 1100 o C calcination temperature is observed in YIG powders prepared by oxides mixture. Spark plasma sintering of these powders between 900 and 950 o C leads to dense samples with minimal formation of YFeO 3 , opening the way to co-sintering of YIG with metals or metallic alloys. The optical properties depend on the sintering stage: low (high) density samples show poor (bulk) optical absorption.

  11. Laser cladding in-situ carbide particle reinforced Fe-based composite coatings with rare earth oxide addition

    Institute of Scientific and Technical Information of China (English)

    吴朝锋; 马明星; 刘文今; 钟敏霖; 张红军; 张伟明

    2009-01-01

    Particulate reinforced metal matrix composite(PR-MMC) has excellent properties such as good wear resistance,corrosion resistance and high temperature properties.Laser cladding is usually used to form PR-MMC on metal surface with various volume fractions of ceramic particles.Recent literatures showed that laser melting of powder mixture containing carbon and carbide-forming elements,was favorable for the formation of in-situ synthesized carbide particles.In this paper,rare earth oxide(RE2O3) was added into t...

  12. Probing Structural Changes in Poly(3-hexylthiophene) (P3HT) During Electrochemical Oxidation with In Situ X-ray Scattering

    Science.gov (United States)

    Thelen, Jacob L.; Patel, Shrayesh N.; Javier, Anna E.; Balsara, Nitash P.

    2014-03-01

    Mixtures of poly(3-hexylthiophene)-b-poly(ethylene oxide) (P3HT-b-PEO) block copolymer and lithium bis(trifluromethanesulfonyl) imide (LiTFSI) salt can microphase separate into electron (P3HT) and ion (PEO/LiTFSI) conducting domains. P3HT is a semicrystalline polymer with intrinsically semiconducting electronic properties. Electrochemical oxidation (doping) of the P3HT block provides the P3HT-b-PEO/LiTFSI mixtures with electronic conductivity suitable for lithium battery operation. Due to the presence of the solid-state electrolyte (PEO/LiTFSI) in intimate contact with the microphase separated P3HT domains, electrochemical oxidation of P3HT can be performed entirely in the solid state; therefore, P3HT-b-PEO/LiTFSI provides a unique opportunity to study the structural changes in P3HT induced by oxidation. We use in situ x-ray scattering techniques to probe structural changes in P3HT during electrochemical oxidation and correlate these changes with previously observed enhancements in electron mobility. Supported by the Joint Center for Energy Storage Research (JCESR).

  13. Ultrasound irradiation based in-situ synthesis of star-like Tragacanth gum/zinc oxide nanoparticles on cotton fabric.

    Science.gov (United States)

    Ghayempour, Soraya; Montazer, Majid

    2017-01-01

    Application of natural biopolymers for green and safe synthesis of zinc oxide nanoparticles on the textiles is a novel and interesting approach. The present study offers the use of natural biopolymer, Tragacanth gum, as the reducing, stabilizing and binding agent for in-situ synthesis of zinc oxide nanoparticles on the cotton fabric. Ultrasonic irradiation leads to clean and easy synthesis of zinc oxide nanoparticles in short-time at low-temperature. FESEM/EDX, XRD, FT-IR spectroscopy, DSC, photocatalytic activities and antimicrobial assay are used to characterize Tragacanth gum/zinc oxide nanoparticles coated cotton fabric. The analysis confirmed synthesis of star-like zinc oxide nanoparticles with hexagonal wurtzite structure on the cotton fabric with the average particle size of 62nm. The finished cotton fabric showed a good photocatalytic activity on degradation of methylene blue and 100% antimicrobial properties with inhibition zone of 3.3±0.1, 3.1±0.1 and 3.0±0.1mm against Staphylococcus aureus, Escherichia coli and Candida albicans. Copyright © 2016 Elsevier B.V. All rights reserved.

  14. Part 1: The effect of lattice defects on the sintering of lithium fluoride; Part 2: The morphology of calcium oxide from calcium carbonate decomposition

    International Nuclear Information System (INIS)

    Fenwick, D.M.

    1990-09-01

    Our motivation for studying the effect of lattice defects on sintering kinetics came from a theory by Searcy concerning surface melting of solids. Surface melting has been shown to occur in ice, argon, and lead at temperatures below the melting point. While surface melting of this sort is an equilibrium phenomenon, Searcy has predicted that surface melting may also occur in a non-equilibrium situation -- when a solid is being rapidly heated and has a below-equilibrium concentration of vacancies for the temperature reached. To test the surface melting theory we have compared the density changes of two different types of powder compacts of lithium fluoride after subjecting both to the same fast-firing heat treatment. One type of compact consisted of powder originating from a crystal which he had quenched from a high temperature, and the other consisted of powder from a crystal which we had annealed at a lower temperature. When calcite is decomposed in vacuum, CaO is sometimes found in two distinguishable layers. Both layers are comprised of fairly uniformly sized, cylindrical rods on the order of 10 nm in diameter with the normal NaCl-type crystal structure. The outer layer consists of ∼1 μm diameter bundles of rods separated by ∼1 μm wide cracks. The second layer, adjacent to any undecomposed calcite -- the ''intermediate layer'' -- probably consists of rods which are relatively evenly spaced. Because sintering is negligible when calcite decomposition occurs below 700 degree C in a vacuum of 10 -3 torr or less, the outer layer is probably formed by a diffusionless, cooperative re-packing of CaO rods first formed with the uniform spacing characteristic of the intermediate layer. 35 refs., 25 figs., 6 tabs

  15. Preparation of Nd–Fe–B sintered magnets from HDDR-processed powder

    Energy Technology Data Exchange (ETDEWEB)

    Takagi, Kenta, E-mail: k-takagi@aist.go.jp [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Akada, Misaho [Magnetic Materials R& D Center, Research Associations of Magnetic Materials for High-Efficiency Motors (MagHEM), Nagoya 463-8560 (Japan); Soda, Rikio; Ozaki, Kimihiro [Green Innovative Magnetic Materials Research Center, National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan)

    2015-11-01

    The electric-current sintering technique was used to fully densify hydrogenation–disproportionation–desorption–recombination (HDDR)-processed Nd–Fe–B powder at temperatures below the grain growth temperature in order to produce high-coercive bulk magnets. However, the sintered magnets exhibited anomalous coercivity reduction that depended on sintered density. Reheating examination of the sintered magnets revealed that the reduced coercivity was increased in proportion to the heating temperature, resulting in complete recovery of coercivity. As a result, the combination of electric-current sintering and post-annealing produced sintered magnets with a coercivity of 15 kOe. Scanning and transmission electron microscopy revealed no evidence that associated the anomalous coercivity reduction and recovery with grain boundary morphology. On the other hand, various HDDR powders with different particle sizes were sintered, and finer powders yielded lower coercivity after sintering, implying that the anomalous coercivity reduction was associated with particle surface oxides of the raw powder. - Highlights: • We conduct a sintering of HDDR-processed Nd–Fe–B powder without coercivity reduction. • Rapid current sintering allows densification of this powder without grain growth. • However, the sintered magnets show an anomalous coercivity reduction phenomenon. • It is found that post-annealing completely recovers the reduced coercivity. • The anomalous coercivity reduction would be due to surface oxide of the raw powder.

  16. In-situ atomic layer deposition growth of Hf-oxide

    International Nuclear Information System (INIS)

    Karavaev, Konstantin

    2010-01-01

    We have grown HfO 2 on Si(001) by atomic layer deposition (ALD) using HfCl 4 , TEMAHf, TDMAHf and H 2 O as precursors. The early stages of the ALD were investigated with high-resolution photoelectron spectroscopy and X-ray absorption spectroscopy. We observed the changes occurring in the Si 2p, O 1s, Hf 4f, Hf 4d, and Cl 2p (for HfCl 4 experiment) core level lines after each ALD cycle up to the complete formation of two layers of HfO 2 . The investigation was carried out in situ giving the possibility to determine the properties of the grown film after every ALD cycle or even after a half cycle. This work focused on the advantages in-situ approach in comparison with ex-situ experiments. The study provides to follow the evolution of the important properties of HfO 2 : contamination level, density and stoichiometry, and influence of the experimental parameters to the interface layer formation during ALD. Our investigation shows that in-situ XPS approach for ALD gives much more information than ex-situ experiments. (orig.)

  17. In-situ atomic layer deposition growth of Hf-oxide

    Energy Technology Data Exchange (ETDEWEB)

    Karavaev, Konstantin

    2010-06-17

    We have grown HfO{sub 2} on Si(001) by atomic layer deposition (ALD) using HfCl{sub 4}, TEMAHf, TDMAHf and H{sub 2}O as precursors. The early stages of the ALD were investigated with high-resolution photoelectron spectroscopy and X-ray absorption spectroscopy. We observed the changes occurring in the Si 2p, O 1s, Hf 4f, Hf 4d, and Cl 2p (for HfCl{sub 4} experiment) core level lines after each ALD cycle up to the complete formation of two layers of HfO{sub 2}. The investigation was carried out in situ giving the possibility to determine the properties of the grown film after every ALD cycle or even after a half cycle. This work focused on the advantages in-situ approach in comparison with ex-situ experiments. The study provides to follow the evolution of the important properties of HfO{sub 2}: contamination level, density and stoichiometry, and influence of the experimental parameters to the interface layer formation during ALD. Our investigation shows that in-situ XPS approach for ALD gives much more information than ex-situ experiments. (orig.)

  18. Sinterability and conductivity of barium doped aluminium lanthanum oxyapatite La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5} electrolyte of solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Cao Xiaoguo [Faculty of Materials and Energy, Guangdong University of Technology, Guangzhou 510006, Guangdong (China); Jiang Sanping, E-mail: s.jiang@curtin.edu.au [Fuels and Energy Technology Institute and Department of Chemical Engineering, Curtin University, Perth, WA 6102 (Australia)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer Ba doping enhances the sintering and densification properties of aluminium lanthanum apatite. Black-Right-Pointing-Pointer Ba doping improves the oxide conductivity of aluminium lanthanum apatite. Black-Right-Pointing-Pointer The enhancement of Ba doping is mainly due to the significantly reduced grain boundary resistance of the aluminium lanthanum apatite. - Abstract: Apatite ceramics are interesting alternative solid oxide fuel cells (SOFCs) electrolytes because of their open structure for the transportation of oxide ions and their good chemical stability. This study reports the influence of barium doping on the microstructure, sinterability and oxide conductivity properties of the aluminium lanthanum oxyapatite La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5}. SEM results show that lanthanum substitution with barium improves the sinterability of apatite ceramics. The barium doping also enhances the conductivity of the aluminium lanthanum silicates. The oxygen ion conductivity of La{sub 9.5}Ba{sub 0.5}Si{sub 5.5}Al{sub 0.5}O{sub 26.5} sintered at 1600 Degree-Sign C is 2.21 Multiplication-Sign 10{sup -2} S cm{sup -1} at 800 Degree-Sign C, higher than 9.81 Multiplication-Sign 10{sup -3} S cm{sup -1} of La{sub 10}Si{sub 5}AlO{sub 26.5} sample prepared under the same conditions. The results in the present study demonstrate that doping Ba on the La site for aluminium lanthanum oxyapatite reduces the sintering temperature and improves the ion conductivity. The enhancement of Ba dopant is mainly on the improvement of the densification and thus substantially reduced grain boundary resistance of aluminium lanthanum oxyapatite particularly at low temperatures.

  19. Ferroferric oxide/polystyrene (Fe3O4/PS superparamagnetic nanocomposite via facile in situ bulk radical polymerization

    Directory of Open Access Journals (Sweden)

    2010-03-01

    Full Text Available Organo-modified ferroferric oxide superparamagnetic nanoparticles, synthesized by the coprecipitation of superparamagnetic nanoparticles in presence of oleic acid (OA, were incorporated in polystyrene (PS by the facile in situ bulk radical polymerization by using 2,2-azobisisobutyronitrile (AIBN as initiator. The transmission electron microscopy (TEM analysis of the resultant uniform ferroferric oxide/polystyrene superparamagnetic nanocomposite (Fe3O4/PS showed that the superparamagnetic nanoparticles had been dispersed homogeneously in the polymer matrix due to the surface grafted polystyrene, confirmed by Fourier transform infrared (FT-IR spectroscopy and thermogravimetric analysis (TGA. The superparamagnetic property of the Fe3O4/PS nanocomposite was testified by the vibrating sample magnetometer (VSM analysis. The strategy developed is expected to be applied for the large-scale industrial manufacturing of the superparamagnetic polymer nanocomposite.

  20. Treatment of dye wastewater with permanganate oxidation and in situ formed manganese dioxides adsorption: cation blue as model pollutant.

    Science.gov (United States)

    Liu, Ruiping; Liu, Huijuan; Zhao, Xu; Qu, Jiuhui; Zhang, Ran

    2010-04-15

    This study investigated the process of potassium permanganate (KMnO(4)) oxidation and in situ formed hydrous manganese dioxides (deltaMnO(2)) (i.e., KMnO(4) oxidation and deltaMnO(2) adsorption) for the treatment of dye wastewater. The effectiveness of decolorization, removing dissolved organic carbon (DOC), and increasing biodegradable oxygen demand (BOD) were compared among these processes of KMnO(4) oxidation, deltaMnO(2) adsorption, and KMnO(4) oxidation and deltaMnO(2) adsorption. DeltaMnO(2) adsorption contributed to the maximum DOC removal of 65.0%, but exhibited limited capabilities of decolorizing and increasing biodegradability. KMnO(4) oxidation alone at pH 0.5 showed satisfactory decrease of UV-vis absorption peaks, and the maximum BOD(5)/DOC value of 1.67 was achieved. Unfortunately, the DOC removal was as low as 27.4%. Additionally, the great amount of acid for pH adjustment and the much too low pH levels limited its application in practice. KMnO(4) oxidation and deltaMnO(2) adsorption at pH 2.0 was the best strategy prior to biological process, in balancing the objectives of decolorization, DOC removal, and BOD increase. The optimum ratio of KMnO(4) dosage to X-GRL concentration (R(KMnO(4)/X-GRL)) was determined to be 2.5, at which KMnO(4) oxidation and deltaMnO(2) adsorption contributed to the maximal DOC removal of 53.4%. Additionally, the optimum pH for X-GRL treatment was observed to be near 3.0. 2009 Elsevier B.V. All rights reserved.

  1. The dimensional accuracy of the sintered billets

    Directory of Open Access Journals (Sweden)

    Чингиз Ариф оглы Алиев

    2016-01-01

    Full Text Available The article presents the results of assessing the impact of the behaviour stability of the components included in the compositions and process parameters of their production, on the dimensional accuracy of workpieces. It was found that by increasing the amount of oxide in the composition is greater compaction of the sintered billet in the process of heat treatment. This also increases the density of all components of the composition

  2. Polluted soils with heavy metals. Stabilization by magnesium oxide. Ex-situ and in-situ testings; Suelos contaminados con metales pesados. Estabilizacion con oxido de magnesio. Ensayos ex situ-in situ

    Energy Technology Data Exchange (ETDEWEB)

    Cenoz, S.; Hernandez, J.; Gangutia, N.

    2004-07-01

    This work describes the use of Low-Grade MgO as a stabiliser agent for polluted soil reclaim. Low-Grade MgO may be an economically feasible alternative in the stabilisation of heavy metals from heavily contaminated soils. The effectiveness of Low-Grade MgO has been studied in three ex-situ stabilisation of heavily polluted soils contaminated by the flue-dust of pyrite roasting. LG-MgO provides an alkali reservoir guaranteeing long-term stabilisation without varying the pH conditions. The success of the ex-situ stabilisation was corroborated with the analysis of heavy metals in the leachates collected from the landfill o ver a long period of time. The study also includes the results obtained in an in-situ pilot scale stabilisation of contaminated soil. (Author) 17 refs.

  3. Layer by Layer Ex-Situ Deposited Cobalt-Manganese Oxide as Composite Electrode Material for Electrochemical Capacitor.

    Science.gov (United States)

    Rusi; Chan, P Y; Majid, S R

    2015-01-01

    The composite metal oxide electrode films were fabricated using ex situ electrodeposition method with further heating treatment at 300°C. The obtained composite metal oxide film had a spherical structure with mass loading from 0.13 to 0.21 mg cm(-2). The structure and elements of the composite was investigated using X-ray diffraction (XRD) and energy dispersive X-ray (EDX). The electrochemical performance of different composite metal oxides was studied by cyclic voltammetry (CV) and galvanostatic charge-discharge (CD). As an active electrode material for a supercapacitor, the Co-Mn composite electrode exhibits a specific capacitance of 285 Fg(-1) at current density of 1.85 Ag(-1) in 0.5 M Na2SO4 electrolyte. The best composite electrode, Co-Mn electrode was then further studied in various electrolytes (i.e., 0.5 M KOH and 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolytes). The pseudocapacitive nature of the material of Co-Mn lead to a high specific capacitance of 2.2 x 10(3) Fg(-1) and an energy density of 309 Whkg(-1) in a 0.5 M KOH/0.04 M K3Fe(CN) 6 electrolyte at a current density of 10 Ag(-1). The specific capacitance retention obtained 67% of its initial value after 750 cycles. The results indicate that the ex situ deposited composite metal oxide nanoparticles have promising potential in future practical applications.

  4. In-situ studies of microbial CH4 oxidation efficiency in Arctic wetland soils. Applications of stable carbon isotopes

    International Nuclear Information System (INIS)

    Preuss, Inken-Marie

    2013-01-01

    Arctic wetland soils are significant sources of the climate-relevant trace gas methane (CH 4 ). The observed accelerated warming of the Arctic is expected to cause deeper permafrost thawing followed by increased carbon mineralization and CH 4 formation in water-saturated permafrost-affected tundra soils thus creating a positive feedback to climate change. Aerobic CH 4 oxidation is regarded as the key process reducing CH 4 emissions from wetlands, but quantification of turnover rates has remained difficult so far. This study improved the in-situ quantification of microbial CH 4 oxidation efficiency in arctic wetland soils in Russia's Lena River Delta based on stable isotope signatures of CH 4 . In addition to the common practice of determining the stable isotope fractionation during oxidation, additionally the fractionation effect of diffusion, an important gas transport mechanism in tundra soils, was investigated for both saturated and unsaturated conditions. The isotopic fractionation factors α ox and α diff were used to calculate the CH 4 oxidation efficiency from the CH 4 stable isotope signatures of wet polygonal tundra soils of different hydrology. Further, the method was used to study the short-term effects of temperature increase with a climate manipulation experiment. For the first time, the stable isotope fractionation of CH 4 diffusion through water-saturated soils was determined with α diff = 1.001 ± 0.0002 (n = 3). CH 4 stable isotope fractionation during diffusion through air-filled pores of the investigated polygonal tundra soils was α diff = 1.013 ± 0.003 (n = 18). For the studied sites the fractionation factor for diffusion under saturated conditions α diff = 1.001 seems to be of utmost importance for the quantification of the CH 4 oxidation efficiency, since most of the CH 4 is oxidized in the saturated part at the aerobic-anaerobic interface. Furthermore, it was found that α ox differs widely between sites and horizons (mean α ox = 1

  5. Carbon nanotube surface modification with polyelectrolyte brushes endowed with quantum dots and metal oxide nanoparticles through in situ synthesis

    International Nuclear Information System (INIS)

    Llarena, Irantzu; Romero, Gabriela; Moya, Sergio E; Ziolo, Ronald F

    2010-01-01

    Carbon nanotubes (CNTs) have been successfully coated with a covalently bonded polymer brush of negatively charged poly(3-sulfopropylamino methacrylate) (PSPM) by in situ polymerization employing atomic transfer radical polymerization (ATRP) from initiating silanes attached to the CNTs before the polymerization. The CNT-bonded brush forms a polymer layer or shell-like structure around the CNTs and provides colloidal stabilization for the CNTs in aqueous media. In situ syntheses of nanocrystalline CdS and magnetic iron oxide in the polymer brushes lead to the formation of hybrid nanocomposites consisting of nanoparticle-containing PSPM-coated CNTs that remain readily dispersible and stable in aqueous media. The hybrid nanostructures are synthesized by ion exchange with the cations of the sulfonate groups of the PSPM followed by precipitation and were followed by stepwise zeta potential measurements and TEM. Such structures could have applications in the design of more complex structures and devices. The general synthetic scheme can be extended to include other nanoparticles as brush cargo to broaden the utility or functionality of the CNTs. TEM data shows nanocrystalline CdS in the range of 5-8 nm embedded in the PSPM brush and nanocrystalline iron oxide with a size between 2 and 4 nm, with the former consistent with UV-vis spectroscopy and fluorescence measurements.

  6. Sintered nuclear fuel compact and method for its production

    International Nuclear Information System (INIS)

    Peehs, M.; Dorr, W.

    1988-01-01

    This patent describes a method of producing a sintered nuclear fuel compact with which reactivity losses in a nuclear reactor having long fuel element cycles are avoided, which comprises, forming a compact of a mixture of powders containing at least one nuclear fuel oxide selected from the group consisting of UO/sub 2/, PuO/sub 2/, ThO/sub 2/, mixed oxide (U, Pu)O/sub 2/ and mixed oxide (U, Th)O/sub 2/, at least one neutron poison selected from the group consisting of UB/sub x/, where x=2; 4 and/or 12 and B/sub 4/C, and sintering the compact of the mixture of powders so that the neutron piston is embedded in a sintered matrix of the nuclear fuel oxide at a treatment temperature in a range from 1000 0 C to 1400 0 C in an oxidizing sintering atmosphere, and then heat treating the sintered compact in a reducing gas atmosphere

  7. Disruption of an Alumina Layer During Sintering of Aluminium in Nitrogen

    Directory of Open Access Journals (Sweden)

    Pieczonka T.

    2017-06-01

    Full Text Available Aluminium oxide layer on aluminium particles cannot be avoided. However, to make the metal-metal contacts possible, this sintering barrier has to be overcome in some way, necessarily to form sintering necks and their development. It is postulated that the disruption of alumina layer under sintering conditions may originate physically and chemically. Additionally, to sinter successfully non alloyed aluminium powder in nitrogen, the operation of both types mechanism is required. It is to be noted that metallic aluminium surface has to be available to initiate reactions between aluminium and the sintering atmosphere, i.e. mechanical disruption of alumina film precedes the chemical reactions, and only then chemically induced mechanisms may develop. Dilatometry, gravimetric and differential thermal analyses, and microstructure investigations were used to study the sintering response of aluminium at 620°C in nitrogen, which is the only sintering atmosphere producing shrinkage.

  8. XPS characterisation of in situ treated lanthanum oxide and hydroxide using tailored charge referencing and peak fitting procedures

    International Nuclear Information System (INIS)

    Sunding, M.F.; Hadidi, K.; Diplas, S.; Lovvik, O.M.; Norby, T.E.; Gunnaes, A.E.

    2011-01-01

    Highlights: → Gold particles deposited in vacuum as energy reference for insulating samples in XPS. → Separation of La 3d and MNN peaks in XP spectra acquired with Al Kα radiation. → We describe the spectral differences between lanthanum oxide and lanthanum hydroxide. → A doublet in O 1s of La 2 O 3 is ascribed to two distinct oxygen sites in the crystal. - Abstract: A technique is described for deposition of gold nanoparticles under vacuum, enabling consistent energy referencing of X-ray photoelectron spectra obtained from lanthanum hydroxide La(OH) 3 and in situ treated lanthanum oxide La 2 O 3 powders. A method is also presented for the separation of the overlapping lanthanum 3d and MNN peaks in X-ray photoelectron spectra acquired with Al Kα radiation. The lower satellite intensity in La(OH) 3 compared to La 2 O 3 is related to the higher ionicity of the La-O bond in the former compared to the latter compound. The presence of an additional peak in the valence band spectrum of the hydroxide compared to the oxide is attributed to the O-H bond as indicated by density functional theory based calculations. A doublet in the O 1s peak of lanthanum oxide is associated to the presence of two distinct oxygen sites in the crystal structure of this compound.

  9. XPS characterisation of in situ treated lanthanum oxide and hydroxide using tailored charge referencing and peak fitting procedures

    Energy Technology Data Exchange (ETDEWEB)

    Sunding, M.F., E-mail: m.f.sunding@fys.uio.no [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); Hadidi, K. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); Diplas, S. [Department of Chemistry and Centre for Material Science and Nanotechnology (SMN), University of Oslo, P.O. Box 1033 Blindern, NO-0315 Oslo (Norway); SINTEF Materials and Chemistry, P.O. Box 124 Blindern, NO-0314 Oslo (Norway); Lovvik, O.M. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway); SINTEF Materials and Chemistry, P.O. Box 124 Blindern, NO-0314 Oslo (Norway); Norby, T.E. [Department of Chemistry and Centre for Material Science and Nanotechnology (SMN), University of Oslo, P.O. Box 1033 Blindern, NO-0315 Oslo (Norway); Gunnaes, A.E. [Department of Physics, University of Oslo, P.O. Box 1048 Blindern, NO-0316 Oslo (Norway)

    2011-07-15

    Highlights: {yields} Gold particles deposited in vacuum as energy reference for insulating samples in XPS. {yields} Separation of La 3d and MNN peaks in XP spectra acquired with Al K{alpha} radiation. {yields} We describe the spectral differences between lanthanum oxide and lanthanum hydroxide. {yields} A doublet in O 1s of La{sub 2}O{sub 3} is ascribed to two distinct oxygen sites in the crystal. - Abstract: A technique is described for deposition of gold nanoparticles under vacuum, enabling consistent energy referencing of X-ray photoelectron spectra obtained from lanthanum hydroxide La(OH){sub 3} and in situ treated lanthanum oxide La{sub 2}O{sub 3} powders. A method is also presented for the separation of the overlapping lanthanum 3d and MNN peaks in X-ray photoelectron spectra acquired with Al K{alpha} radiation. The lower satellite intensity in La(OH){sub 3} compared to La{sub 2}O{sub 3} is related to the higher ionicity of the La-O bond in the former compared to the latter compound. The presence of an additional peak in the valence band spectrum of the hydroxide compared to the oxide is attributed to the O-H bond as indicated by density functional theory based calculations. A doublet in the O 1s peak of lanthanum oxide is associated to the presence of two distinct oxygen sites in the crystal structure of this compound.

  10. Impact of Air Oxidation on Dissolved Organic Matter from Boom Clay: Comparison Between Natural and Artificial Oxidation Series and In Situ Piezometers Water From Hades Galleries

    International Nuclear Information System (INIS)

    Blanchart, Pascale; Faure, Pierre; Michels, Raymond; Bruggeman, Christophe; De Craen, Mieke; Parant, Stephane

    2012-01-01

    molecular weight of DOM; - The appearance of a specific fluorescence fingerprint. DOM isolated from piezometers was characterized by the same multi-technical approach (DOC measurement, 3D-fluorescence, SEC-HPLC, PyGC-MS). The molecular as well as spectroscopic fingerprints previously determined on natural and artificial oxidized samples were compared to those of the in situ DOM. Specific fingerprints of DOM isolated from oxidized Boom clay were not consistent with the DOM signatures observed in piezometers. On the contrary, these DOM characteristics are close to water isolated from unaltered Boom clay Thus, the composition of the DOM currently present in the piezometer waters can not be related to the leaching of oxidized host rock but is probably inherited directly from the well preserved host rock. (authors)

  11. Second-Order Biomimicry: In Situ Oxidative Self-Processing Converts Copper(I)/Diamine Precursor into a Highly Active Aerobic Oxidation Catalyst.

    Science.gov (United States)

    McCann, Scott D; Lumb, Jean-Philip; Arndtsen, Bruce A; Stahl, Shannon S

    2017-04-26

    A homogeneous Cu-based catalyst system consisting of [Cu(MeCN) 4 ]PF 6 , N , N '-di- tert -butylethylenediamine (DBED), and p -( N , N -dimethylamino)pyridine (DMAP) mediates efficient aerobic oxidation of alcohols. Mechanistic study of this reaction shows that the catalyst undergoes an in situ oxidative self-processing step, resulting in conversion of DBED into a nitroxyl that serves as an efficient cocatalyst for aerobic alcohol oxidation. Insights into this behavior are gained from kinetic studies, which reveal an induction period at the beginning of the reaction that correlates with the oxidative self-processing step, EPR spectroscopic analysis of the catalytic reaction mixture, which shows the buildup of the organic nitroxyl species during steady state turnover, and independent synthesis of oxygenated DBED derivatives, which are shown to serve as effective cocatalysts and eliminate the induction period in the reaction. The overall mechanism bears considerable resemblance to enzymatic reactivity. Most notable is the "oxygenase"-type self-processing step that mirrors generation of catalytic cofactors in enzymes via post-translational modification of amino acid side chains. This higher-order function within a synthetic catalyst system presents new opportunities for the discovery and development of biomimetic catalysts.

  12. The physical chemistry and materials science behind sinter-resistant catalysts.

    Science.gov (United States)

    Dai, Yunqian; Lu, Ping; Cao, Zhenming; Campbell, Charles T; Xia, Younan

    2018-06-18

    Catalyst sintering, a main cause of the loss of catalytic activity and/or selectivity at high reaction temperatures, is a major concern and grand challenge in the general area of heterogeneous catalysis. Although all heterogeneous catalysts are inevitably subjected to sintering during their operation, the immediate and drastic consequences can be mitigated by carefully engineering the catalytic particles and their interactions with the supports. In this tutorial review, we highlight recent progress in understanding the physical chemistry and materials science involved in sintering, including the discussion of advanced techniques, such as in situ microscopy and spectroscopy, for investigating the sintering process and its rate. We also discuss strategies for the design and rational fabrication of sinter-resistant catalysts. Finally, we showcase recent success in improving the thermal stability and thus sinter resistance of supported catalytic systems.

  13. Computer Modeling of Direct Metal Laser Sintering

    Science.gov (United States)

    Cross, Matthew

    2014-01-01

    A computational approach to modeling direct metal laser sintering (DMLS) additive manufacturing process is presented. The primary application of the model is for determining the temperature history of parts fabricated using DMLS to evaluate residual stresses found in finished pieces and to assess manufacturing process strategies to reduce part slumping. The model utilizes MSC SINDA as a heat transfer solver with imbedded FORTRAN computer code to direct laser motion, apply laser heating as a boundary condition, and simulate the addition of metal powder layers during part fabrication. Model results are compared to available data collected during in situ DMLS part manufacture.

  14. In situ growth of well-ordered NiFe-MOF-74 on Ni foam by Fe2+ induction as an efficient and stable electrocatalyst for water oxidation.

    Science.gov (United States)

    Xing, Jiale; Guo, Kailu; Zou, Zehua; Cai, Minmin; Du, Jing; Xu, Cailing

    2018-06-06

    Well-ordered NiFe-MOF-74 is in situ grown on Ni foam by the induction of Fe2+ and directly used as an OER electrocatalyst. Benefited from the intrinsic open porous structure of MOF-74, the in situ formed MOF arrays and the synergistic effect of Ni and Fe, outstanding water oxidation activity is obtained in alkaline electrolytes with an overpotential of 223 mV at 10 mA cm-2.

  15. Bonding evolution with sintering temperature in low alloyed steels with chromium

    Directory of Open Access Journals (Sweden)

    Fuentes-Pacheco L.

    2009-01-01

    Full Text Available At present, high performance PM steels for automotive applications follow a processing route that comprises die compaction of water-atomized powder, followed by sintering and secondary treatments, and finishing operations. This study examines Cr-alloyed sintered steels with two level of alloying. In chromium-alloyed steels, the surface oxide on the powder is of critical importance for developing the bonding between the particles during sintering. Reduction of this oxide depends mainly on three factors: temperature, dew point of the atmosphere, and carbothermic reduction provided by the added graphite. The transformation of the initial surface oxide evolves sequence as temperature increases during sintering, depending on the oxide composition. Carbothermic reduction is supposed to be the controlling mechanism, even when sintering in hydrogen-containing atmospheres. The effect of carbothermic reduction can be monitored by investigating the behavior of the specimens under tensile testing, and studying the resultant fracture surfaces.

  16. Fabrication of a large area cathode-supported thin electrolyte film for solid oxide fuel cells via tape casting and co-sintering techniques

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Chunhua; Liu, Renzhu; Wang, Shaorong; Wen, Tinglian [Shanghai Institute of Ceramics, Chinese Academy of Sciences (SICCAS), 1295 Dingxi Road, Shanghai 200050 (China)

    2009-04-15

    A large area cathode-supported electrolyte film, comprising porous (La{sub 0.8}Sr{sub 0.2}){sub 0.95}MnO{sub 3} (LSM95) cathode substrate, LSM95/Zr{sub 0.89}Sc{sub 0.1}Ce{sub 0.01}O{sub 2-x} (SSZ) cathode active layer, and SSZ electrolyte, has been successfully fabricated by tape casting and co-sintering techniques. The interface reaction between cathode and electrolyte was inhibited by using A-site deficient LSM. A dense enough SSZ thin film with a thickness of {proportional_to}26 {mu}m was obtained at 1250 C. By using Pt as anode, the obtained single cell reached the maximum power density of 0.54 W cm{sup -2} at 800 C in O{sub 2}/humidified H{sub 2}, with open circuit voltage (OCV) value of 1.08 V. (author)

  17. Sintering Studies of Ga-Doped CeO2 (Ga-Doped PuO2 Surrogate) for Mixed Oxide Nuclear Fuel

    International Nuclear Information System (INIS)

    Haertling, C.; Huling, J.; Park, Y.S.

    1999-01-01

    Sintering studies of CeO 2 and CeO 2 + 2 wt. % Ga 2 O 3 were completed. Firing temperatures studied were 1250-1650 C with 2 to 4 hour firing soak times in air. Powders fabricated by three methods (as-received, attrition-mill and nitrite-derived) were studied. Attrition-milled CeO 2 improved densities as compared with as-received CeO 2 . Attrition-milled CeO 2 with 2 wt.% Ga 2 O 3 showed decreased densities with increasing temperatures. As-received CeO 2 with 2 wt.% Ga 2 O 3 showed a opposite trend, increasing in density with increased firing temperature. Two pellet preparation methods were studied, a one-step-press method and a two-step-press method. The two-step-press method showed greater densities at lower firing temperatures and times as compared with the one-step-press method, however for CeO 2 + 2 wt.% Ga 2 O 3 , the two methods gave equivalent results at 1650 C, 6 hr. firing conditions

  18. Characteristics Of The Porous Body Sintered By Nano-Sized Fe-Cr-Al Alloy Powder

    Directory of Open Access Journals (Sweden)

    Lee Su-In

    2015-06-01

    Full Text Available Porous metal with uniform honeycomb structure was successfully produced by sintering using Fe-Cr-Al nano powder, which was prepared by the pulsed wire evaporation (PWE in ethanol. Its process consisted of the several steps; 1 coating on the surface of polyurethane sponge with the liquid droplets generated from the ethanol-based slurry where the Fe-Cr-Al nano powders were uniformly dispersed, 2 heat treatment of debinding to remove the polyurethane sponge and 3 sintering of the porous green body formed by Fe-Cr-Al nano powders. The strut thickness of porous Fe-Cr-Al was increased by the increase of spraying times in ESP step. Also, The shrinkages and the oxidation resistance of the sintered porous body was increased with increase of sintering temperature. The optimal sintering temperature was shown to 1450°C in views to maximize the oxidation resistance and sinterability.

  19. IN SITU INFRARED STUDY OF CATALYTIC DECOMPOSITION OF NITRIC OXIDE (NO); FINAL

    International Nuclear Information System (INIS)

    Unknown

    1999-01-01

    The growing concerns for the environment and increasingly stringent standards for NO emission have presented a major challenge to control NO emissions from electric utility plants and automobiles. Catalytic decomposition of NO is the most attractive approach for the control of NO emission for its simplicity. Successful development of an effective catalyst for NO decomposition will greatly decrease the equipment and operation cost of NO control. Due to lack of understanding of the mechanism of NO decomposition, efforts on the search of an effective catalyst have been unsuccessful. Scientific development of an effective catalyst requires fundamental understanding of the nature of active site, the rate-limiting step, and an approach to prolong the life of the catalyst. The authors have investigated the feasibility of two novel approaches for improving catalyst activity and resistance to sintering. The first approach is the use of silanation to stabilize metal crystallites and supports for Cu-ZSM-5 and promoted Pt catalysts; the second is utilization of oxygen spillover and desorption to enhance NO decomposition activity. The silanation approach failed to stabilize Cu-ZSM-5 activity under hydrothermal condition. Silanation blocked the oxygen migration and inhibited oxygen desorption. Oxygen spillover was found to be an effective approach for promoting NO decomposition activity on Pt-based catalysts. Detailed mechanistic study revealed the oxygen inhibition in NO decomposition and reduction as the most critical issue in developing an effective catalytic approach for controlling NO emission

  20. Solid oxide electrode kinetics in light of in situ surface studies

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg

    2014-01-01

    The combination of in situ and in particular in operando characterization methods such as electrochemical impedance spectroscopy (EIS) on both technical and model electrode are well known ways to gain some practical insight in electrode reaction kinetics. Yet, is has become clear that in spite...... of the strengths it is not sufficient to reveal much details of the electrode mechanisms mainly because it provide average values only. Therefore it has to be combined with surface science methods in order to reveal the interface structure and composition. Ex situ methods have been very useful over the latest....... Furthermore, it seems that detailed mathematical modeling using new tools like COMSOL is necessary for the synthesis of the large amount of data for a well-characterized electrode into one physical meaningful picture. A brief review of literature an own data will be presented with a practical example of SOFC...

  1. Laser Surface Treatment of Sintered Alumina

    Science.gov (United States)

    Hagemann, R.; Noelke, C.; Kaierle, S.; Wesling, V.

    Sintered alumina ceramics are used as refractory materials for industrial aluminum furnaces. In this environment the ceramic surface is in permanent contact with molten aluminum resulting in deposition of oxidic material on its surface. Consequently, a lower volume capacity as well as thermal efficiency of the furnaces follows. To reduce oxidic adherence of the ceramic material, two laser-based surface treatment processes were investigated: a powder- based single-step laser cladding and a laser surface remelting. Main objective is to achieve an improved surface quality of the ceramic material considering the industrial requirements as a high process speed.

  2. In situ FTIRS study of ethanol electro-oxidation on anode catalysts in direct ethanol fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Q.; Sun, G.; Jiang, L.; Zhu, M.; Yan, S.; Wang, G.; Xin, Q. [Chinese Academy of Sciences, Dalian (China). Dalian Inst. of Chemical Physics; Chen, Q.; Li, J.; Jiang, Y.; Sun, S. [Xiamen Univ., Xiamen (China). State Key Lab. for Physical Chemistry of Solid Surfaces

    2006-07-01

    The low activation of ethanol oxidation at lower temperatures is an obstacle to the development of cost-effective direct ethanol fuel cells (DEFCs). This study used a modified polyol method to prepare carbon-supported platinum (Pt) based catalysts. Carbon supported Pt-based catalysts were fabricated by a modified polyol method and characterized through transmission electron spectroscopy (TEM) and X-ray diffraction (XRD). Results of the study showed that the particles in the Pt/C and PtRu/C and PtSn/C catalysts were distributed on the carbon support uniformly. Diffraction peaks of the Pt shifted positively in the PtRu/C catalysts and negatively in the PtSn/C catalysts. In situ Fourier Transform Infra-red spectroscopy (FTIR) was used to investigate the adsorption and oxidation process of ethanol on the catalysts. Results showed that the electrocatalytic activity of ethanol oxidation on the materials was enhanced. Linear bonded carbon monoxide (CO) was the most strongly absorbed species, and the main products produced by the catalysts were carbon dioxide (CO{sub 2}), acetaldehyde, and acetic acid. Results showed that the PtRu/C catalyst broke the C-C bond more easily than the Pt/C and PtSn/C compounds. However, the results of a linear sweep voltammogram analysis showed that ethanol oxidation of the PtSn/C was enhanced. Bands observed on the compound indicated the formation of acetic acid and acetaldehyde. It was concluded that the enhancement of PtSn/C for ethanol oxidation was due to the formation of acetic acid and acetaldehyde at lower potentials. 4 refs., 1 fig.

  3. 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.

  4. Sintering and electrical properties of strontium-doped lanthanum manganite

    Energy Technology Data Exchange (ETDEWEB)

    Tarrago, Diego Pereira; Sousa, Vania Caldas de [Universidade Federal do Rio Grande do Sul (LABIOMAT/PPGEM/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia de Minas, Metalurgica e de Materiais. Lab. de Biomateriais], Email: dptarrago@gmail.com; Moreno Buriel, Berta; Chinarro Martini, Eva; Jurado Egea, Jose Ramon [Consejo Superior de Investigaciones Cientificas (ICV/CSIC), Madrid (Spain). Inst. de Ceramica y Vidrio; Malfatti, Celia de Fraga [Universidade Federal do Rio Grande do Sul (LAPEC/PPGEM/UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia de Minas, Metalurgica e de Materiais. Lab. de Pesquisa em Corrosao

    2010-07-01

    Lanthanum strontium manganites (LSM) are potential materials for cathode applications in solid oxide fuel cells (SOFC) due to their good catalytic activity, chemical stability and compatibility with electrolyte materials in high temperatures. The sinterability of single phase La{sub 1-x}Sr{sub x}Mn{sub O3} (x=0.18) perovskite powders and the electrical properties of the resulting samples are analyzed in this study. Using a heating microscope, the powders were pressed and sintered at different pressures and temperatures, resulting in an open porosity of 33.36% when compacted at 125 MPa and sintered at 1200 degree C. Top and cross-section s canning electron microscopy (SEM) micrographs revealed interconnected pores in the sintered body and, hence, a suitable microstructure for the application. The activation energy for conductance was 0.04 eV and the tested LSM bulk started to exhibit adequate electrical properties at about 500 degree C. (author)

  5. Influence of size and volume fraction of SiC particulates on properties of ex situ reinforced Al-4.5Cu-3Mg metal matrix composite prepared by direct metal laser sintering process

    Energy Technology Data Exchange (ETDEWEB)

    Ghosh, Subrata Kumar [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Midnapore (West), Kharagpur 721302, West Bengal (India); Saha, Partha, E-mail: psaha@mech.iitkgp.ernet.in [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Midnapore (West), Kharagpur 721302, West Bengal (India); Kishore, Shyam [Department of Mechanical Engineering, Indian Institute of Technology Kharagpur, Midnapore (West), Kharagpur 721302, West Bengal (India)

    2010-07-15

    Direct metal laser sintering (DMLS) process has a great potential to prepare metal matrix composites (MMCs) in fabrication of arbitrary shaped jobs through rapid manufacturing. In the present work, silicon carbide particulates reinforced aluminium based metal matrix composite was developed by direct metal laser sintering process. Influences of SiC particulate (SiCp) on density, porosity and microhardness of the composite were investigated. It shows that SiCp having 300 mesh size provides higher density and lower porosity because of lower clustering effect. Higher microhardness was achieved at 1200 mesh of reinforcement because of lower grain size. Microhardness increases with increase of volume fraction of SiCp and higher value was achieved at high reinforcement content of 30 vol.%. Microstructure was studied through scanning electron microscopy (SEM) and X-ray elemental mapping. Interfacial microstructure was also investigated and cracks were found in number of cases due to difference between co-efficient of thermal expansion of matrix alloy and SiCp.

  6. Influence of size and volume fraction of SiC particulates on properties of ex situ reinforced Al-4.5Cu-3Mg metal matrix composite prepared by direct metal laser sintering process

    International Nuclear Information System (INIS)

    Ghosh, Subrata Kumar; Saha, Partha; Kishore, Shyam

    2010-01-01

    Direct metal laser sintering (DMLS) process has a great potential to prepare metal matrix composites (MMCs) in fabrication of arbitrary shaped jobs through rapid manufacturing. In the present work, silicon carbide particulates reinforced aluminium based metal matrix composite was developed by direct metal laser sintering process. Influences of SiC particulate (SiCp) on density, porosity and microhardness of the composite were investigated. It shows that SiCp having 300 mesh size provides higher density and lower porosity because of lower clustering effect. Higher microhardness was achieved at 1200 mesh of reinforcement because of lower grain size. Microhardness increases with increase of volume fraction of SiCp and higher value was achieved at high reinforcement content of 30 vol.%. Microstructure was studied through scanning electron microscopy (SEM) and X-ray elemental mapping. Interfacial microstructure was also investigated and cracks were found in number of cases due to difference between co-efficient of thermal expansion of matrix alloy and SiCp.

  7. A full-scale demonstration of in situ chemical oxidation through recirculation at the X-701B site

    International Nuclear Information System (INIS)

    West, O.R.; Cline, S.R.; Holden, W.L.; Gardner, F.G.; Schlosser, B.M.; Thate, J.E.; Pickering, D.A.; Houk, T.C.

    1997-12-01

    In 1996, researchers at Oak Ridge National Laboratory (ORNL) proposed an oxidant delivery technique involving injection and recirculation of the oxidant solution into a contaminated aquifer through multiple horizontal and vertical wells. This technique would be applicable to saturated, hydraulically conductive formations. In the spring of 1997, the Department of Energy (DOE) at the Portsmouth Gaseous Diffusion Plant (PORTS) agreed to collaborate with the DOE's Subsurface Contaminants Focus Area to conduct a field-scale treatability study using in situ chemical oxidation through recirculation (ISCOR). PORTS agreed to support the demonstration at the X-701B site where the technology can potentially be used to remediate TCE-contaminated groundwater and sediments. The ISCOR field demonstration took advantage of existing infrastructure and extensive site characterization data generated from previous field demonstrations at X-701B. The field test was implemented using a pair of previously installed horizontal wells that transect an area of DNAPL contamination. Groundwater was extracted from one horizontal well, pumped to an existing pump and treat facility, dosed with KMnO 4 , and re-injected into a parallel horizontal well approximately 90 ft away. The field demonstration lasted approximately one month. Treatment effectiveness was determined by comparing contaminant levels in pre-treatment, during, and post-treatment groundwater samples and pre- and post-treatment soil samples

  8. Two-step flash light sintering of copper nanoparticle ink to remove substrate warping

    Energy Technology Data Exchange (ETDEWEB)

    Ryu, Chung-Hyeon; Joo, Sung-Jun [Department of Mechanical Convergence Engineering, Hanyang University, Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Kim, Hak-Sung, E-mail: kima@hanyang.ac.kr [Department of Mechanical Convergence Engineering, Hanyang University, Haengdang-dong, Seongdong-gu, Seoul 133-791 (Korea, Republic of); Institute of Nano Science and Technology, Hanyang University, Seoul, 133-791 (Korea, Republic of)

    2016-10-30

    Highlights: • We performed the two-step flash light sintering for copper nanoparticle ink to remove substrate warping. • 12 J/cm{sup 2} of preheating and 7 J/cm{sup 2} of main sintering energies were determined as optimum conditions to sinter the copper nanoparticle ink. • The resistivity of two-step sintered copper nanoparticle ink was 3.81 μΩ cm with 5B adhesion level, 2.3 times greater than that of bulk copper. • The two-step sintered case showed a high conductivity without any substrate warping. - Abstract: A two-step flash light sintering process was devised to reduce the warping of polymer substrates during the sintering of copper nanoparticle ink. To determine the optimum sintering conditions of the copper nanoparticle ink, the flash light irradiation conditions (pulse power, pulse number, on-time, and off-time) were varied and optimized. In order to monitor the flash light sintering process, in situ resistance and temperature monitoring of copper nanoink were conducted during the flash light sintering process. Also, a transient heat transfer analysis was performed by using the finite-element program ABAQUS to predict the temperature changes of copper nanoink and polymer substrate. The microstructures of the sintered copper nanoink films were analyzed by scanning electron microscopy. Additionally, an X-ray diffraction and Fourier transform infrared spectroscopy were used to characterize the crystal phase change of the sintered copper nanoparticles. The resulting two-step flash light sintered copper nanoink films exhibited a low resistivity (3.81 μΩ cm, 2.3 times of that of bulk copper) and 5B level of adhesion strength without warping of the polymer substrate.

  9. In-situ electrochemical doping of nanoporous anodic aluminum oxide with indigo carmine organic dye

    International Nuclear Information System (INIS)

    Stępniowski, Wojciech J.; Norek, Małgorzata; Budner, Bogusław; Michalska-Domańska, Marta; Nowak-Stępniowska, Agata; Bombalska, Aneta; Kaliszewski, Miron; Mostek, Anna; Thorat, Sanjay; Salerno, Marco; Giersig, Michael; Bojar, Zbigniew

    2016-01-01

    Nanoporous anodic aluminum oxide was formed in sulfuric acid with addition of indigo carmine. During anodizing, the organic dye was incorporated into the porous oxide walls. X-ray photoelectron spectroscopy revealed the presence of nitrogen and sulfur in the anodic aluminum oxide. Two types of incorporated sulfur were found: belonging to the sulfate anions SO_4"2"− of the electrolyte and belonging to the C-SO_3"− side groups of the indigo carmine. Raman spectroscopy confirmed the incorporation and showed that the inorganic–organic hybrid material inherited optical properties from the indigo carmine. Typical modes from pyrrolidone rings, unique for indigo carmine in the investigated system (650 and 1585 cm"−"1), were found to be the strongest for the greatest anodizing voltages used. Despite the indigo carmine incorporation, the morphology of the oxide is still nanoporous and its geometry is still tuned by the voltage applied during aluminum anodization. This work presents an inexpensive and facile approach to doping an inorganic oxide material with organic compounds. - Highlights: • Nanoporous anodic alumina was formed in electrolyte with indigo carmine. • XPS confirmed the presence of N and S in anodic alumina. • Raman spectroscopy revealed indigo carmine bands in anodic alumina. • The higher the voltage, the more indigo carmine was incorporated.

  10. In-situ electrochemical doping of nanoporous anodic aluminum oxide with indigo carmine organic dye

    Energy Technology Data Exchange (ETDEWEB)

    Stępniowski, Wojciech J., E-mail: wojciech.stepniowski@wat.edu.pl [Department of Advanced Materials and Technology, Faculty of Advanced Technology and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Norek, Małgorzata [Department of Advanced Materials and Technology, Faculty of Advanced Technology and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Budner, Bogusław [Institute of Optoelectronics, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Michalska-Domańska, Marta [Department of Advanced Materials and Technology, Faculty of Advanced Technology and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Institute of Optoelectronics, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Nowak-Stępniowska, Agata; Bombalska, Aneta; Kaliszewski, Miron [Institute of Optoelectronics, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Mostek, Anna [Department of Advanced Materials and Technology, Faculty of Advanced Technology and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland); Thorat, Sanjay; Salerno, Marco [Department of Nanophysics, Istituto Italiano di Tecnologia, via Morego 30, Genova I-16163 (Italy); Giersig, Michael [Institut für Experimentalphysik, Freie Universität Berlin, Arnimallee 14, 14195 Berlin (Germany); Bojar, Zbigniew [Department of Advanced Materials and Technology, Faculty of Advanced Technology and Chemistry, Military University of Technology, 2 Kaliskiego Str., 00-908 Warszawa (Poland)

    2016-01-01

    Nanoporous anodic aluminum oxide was formed in sulfuric acid with addition of indigo carmine. During anodizing, the organic dye was incorporated into the porous oxide walls. X-ray photoelectron spectroscopy revealed the presence of nitrogen and sulfur in the anodic aluminum oxide. Two types of incorporated sulfur were found: belonging to the sulfate anions SO{sub 4}{sup 2−} of the electrolyte and belonging to the C-SO{sub 3}{sup −} side groups of the indigo carmine. Raman spectroscopy confirmed the incorporation and showed that the inorganic–organic hybrid material inherited optical properties from the indigo carmine. Typical modes from pyrrolidone rings, unique for indigo carmine in the investigated system (650 and 1585 cm{sup −1}), were found to be the strongest for the greatest anodizing voltages used. Despite the indigo carmine incorporation, the morphology of the oxide is still nanoporous and its geometry is still tuned by the voltage applied during aluminum anodization. This work presents an inexpensive and facile approach to doping an inorganic oxide material with organic compounds. - Highlights: • Nanoporous anodic alumina was formed in electrolyte with indigo carmine. • XPS confirmed the presence of N and S in anodic alumina. • Raman spectroscopy revealed indigo carmine bands in anodic alumina. • The higher the voltage, the more indigo carmine was incorporated.

  11. Graphene oxide directed in-situ deposition of electroactive silver nanoparticles and its electrochemical sensing application for DNA analysis

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Ningning [College of Chemistry and Environment, Fujian Province Key Laboratory of Modern Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou, 363000 (China); Gao, Feng, E-mail: fgao1981@mnnu.edu.cn [College of Chemistry and Environment, Fujian Province Key Laboratory of Modern Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou, 363000 (China); Department of Chemistry, Graduate School of Science and Engineering, Shimane University, 1060 Nishikawatsu, Matsue, Shimane, 690-8504 (Japan); He, Suyu; Zhu, Qionghua; Huang, Jiafu [College of Chemistry and Environment, Fujian Province Key Laboratory of Modern Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou, 363000 (China); Tanaka, Hidekazu [Department of Chemistry, Graduate School of Science and Engineering, Shimane University, 1060 Nishikawatsu, Matsue, Shimane, 690-8504 (Japan); Wang, Qingxiang, E-mail: axiang236@126.com [College of Chemistry and Environment, Fujian Province Key Laboratory of Modern Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou, 363000 (China)

    2017-01-25

    The development of high-performance biosensing platform is heavily dependent on the recognition property of the sensing layer and the output intensity of the signal probe. Herein, we present a simple and highly sensitive biosensing interface for DNA detection on the basis of graphene oxide nanosheets (GONs) directed in-situ deposition of silver nanoparticles (AgNPs). The fabrication process and electrochemical properties of the biosensing interface were probed by electrochemical techniques and scanning electron microscopy. The results indicate that GONs can specifically adsorb at the single-stranded DNA probe surface, and induces the deposition of highly electroactive AgNPs. Upon hybridization with complementary oligonucleotides to generate the duplex DNA on the electrode surface, the GONs with the deposited AgNPs will be liberated from the sensing interface due to the inferior affinity of GONs and duplex DNA, resulting in the reduction of the electrochemical signal. Such a strategy combines the superior recognition of GONs toward single-stranded DNA and double-stranded DNA, and the strong electrochemical response of in-situ deposited AgNPs. Under optimal conditions, the biosensor can detect target DNA over a wide range from 10 fM to 10 nM with a detection limit of 7.6 fM. Also, the developed biosensor shows outstanding discriminating ability toward oligonucleotides with different mismatching degrees. - Highlights: • An novel DNA biosensor was constructed based on GONs with deposited AgNPs. • GONs catalyze the in-situ deposition of AgNPs on the sensing interface. • Unique π-stacking of GONs with probe DNA contributes high selectivity of the biosensor. • High electroactivity of AgNPs leads to low detection limit (7.6 fM) for target DNA.

  12. as heterogeneous enantioselective epoxidation catalyst using in situ generated dimethyldioxirane as oxidant

    Directory of Open Access Journals (Sweden)

    Jairo Cubillos

    2007-01-01

    Full Text Available En este trabajo se investigó la actividad catalítica del catalizador de Jacobsen inmovilizado en Al-MCMC-41 y en NH2-Si-MCM-41 en la epoxidación enantioselectiva de tres olefinas proquirales, utilizando dimetildioxirano generado in situ como agente oxidante. Con este agente oxidante, el catalizador no sufrió cambios significativos en su estructura química. El catalizador se reutilizó exitosamente, cuando se inmovilizó por enlace químico covalente a través del ligando de salen.

  13. Tailoring the Electrochemical Properties of Carbon Nanotube Modified Indium Tin Oxide via in Situ Grafting of Aryl Diazonium.

    Science.gov (United States)

    Hicks, Jacqueline M; Wong, Zhi Yi; Scurr, David J; Silman, Nigel; Jackson, Simon K; Mendes, Paula M; Aylott, Jonathan W; Rawson, Frankie J

    2017-05-23

    Our ability to tailor the electronic properties of surfaces by nanomodification is paramount for various applications, including development of sensing, fuel cell, and solar technologies. Moreover, in order to improve the rational design of conducting surfaces, an improved understanding of structure/function relationships of nanomodifications and effect they have on the underlying electronic properties is required. Herein, we report on the tuning and optimization of the electrochemical properties of indium tin oxide (ITO) functionalized with single-walled carbon nanotubes (SWCNTs). This was achieved by controlling in situ grafting of aryl amine diazonium films on the nanoscale which were used to covalently tether SWCNTs. The structure/function relationship of these nanomodifications on the electronic properties of ITO was elucidated via time-of-flight secondary ion mass spectrometry and electrochemical and physical characterization techniques which has led to new mechanistic insights into the in situ grafting of diazonium. We discovered that the connecting bond is a nitro group which is covalently linked to a carbon on the aryl amine. The increased understanding of the surface chemistry gained through these studies enabled us to fabricate surfaces with optimized electron transfer kinetics. The knowledge gained from these studies allows for the rational design and tuning of the electronic properties of ITO-based conducting surfaces important for development of various electronic applications.

  14. Impact of process temperature on GaSb metal-oxide-semiconductor interface properties fabricated by ex-situ process

    Energy Technology Data Exchange (ETDEWEB)

    Yokoyama, Masafumi, E-mail: yokoyama@mosfet.t.u-tokyo.ac.jp; Takenaka, Mitsuru; Takagi, Shinichi [Department of Electrical Engineering and Information Systems, The University of Tokyo, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); JST-CREST, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); Asakura, Yuji [Department of Electrical Engineering and Information Systems, The University of Tokyo, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); Yokoyama, Haruki [NTT Photonics Laboratories, NTT Corporation, Atsugi 243-0198 (Japan)

    2014-06-30

    We have studied the impact of process temperature on interface properties of GaSb metal-oxide-semiconductor (MOS) structures fabricated by an ex-situ atomic-layer-deposition (ALD) process. We have found that the ALD temperature strongly affects the Al{sub 2}O{sub 3}/GaSb MOS interface properties. The Al{sub 2}O{sub 3}/GaSb MOS interfaces fabricated at the low ALD temperature of 150 °C have the minimum interface-trap density (D{sub it}) of ∼4.5 × 10{sup 13 }cm{sup −2} eV{sup −1}. We have also found that the post-metalization annealing at temperature higher than 200 °C degrades the Al{sub 2}O{sub 3}/GaSb MOS interface properties. The low-temperature process is preferable in fabricating GaSb MOS interfaces in the ex-situ ALD process to avoid the high-temperature-induced degradations.

  15. Low-temperature thermal reduction of graphene oxide: In situ correlative structural, thermal desorption, and electrical transport measurements

    Science.gov (United States)

    Lipatov, Alexey; Guinel, Maxime J.-F.; Muratov, Dmitry S.; Vanyushin, Vladislav O.; Wilson, Peter M.; Kolmakov, Andrei; Sinitskii, Alexander

    2018-01-01

    Elucidation of the structural transformations in graphene oxide (GO) upon reduction remains an active and important area of research. We report the results of in situ heating experiments, during which electrical, mass spectrometry, X-ray photoelectron spectroscopy (XPS), Raman spectroscopy, and transmission electron microscopy (TEM) measurements were carried out correlatively. The simultaneous electrical and temperature programmed desorption measurements allowed us to correlate the onset of the increase in the electrical conductivity of GO by five orders of magnitude at about 150 °C with the maxima of the rates of desorption of H2O, CO, and CO2. Interestingly, this large conductivity change happens at an intermediate level of the reduction of GO, which likely corresponds to the point when the graphitic domains become large enough to enable percolative electronic transport. We demonstrate that the gas desorption is intimately related to (i) the changes in the chemical structure of GO detected by XPS and Raman spectroscopy and (ii) the formation of nanoscopic holes in GO sheets revealed by TEM. These in situ observations provide a better understanding of the mechanism of the GO thermal reduction.

  16. DNAPL remediation with in situ chemical oxidation using potassium permanganate - Part I. Mineralogy of Mn oxide and its dissolution in organic acids

    Science.gov (United States)

    Li, X. David; Schwartz, Franklin W.

    2004-01-01

    Previous studies on in situ chemical oxidation of trichloroethylene (TCE) with potassium permanganate indicated that the solid reaction product, Mn oxide, could reduce the permeability of the porous medium and impact the success of dense non-aqueous phase liquid (DNAPL) removal. In order to address the issue of permeability reduction caused by precipitation, this study investigated the mineralogy of Mn oxides and the possibilities of removing the solid precipitates by dissolution. The solid reaction product from the oxidation of TCE by permanganate is semi-amorphous potassium-rich birnessite, which has a layered mineral structure with an interlayer spacing of 7.3 Å. The chemical formula is K 0.854Mn 1.786O 4·1.55H 2O. It has a relatively small specific surface area at 23.6±0.82 m 2/g. Its point of zero charge (pzc) was measured as 3.7±0.4. This birnessite is a relatively active species and could participate in various reactions with existing organic and inorganic matter. The dissolution kinetics of Mn oxide was evaluated in batch experiments using solutions of citric acid, oxalic acid, and ethylenediaminetetraacetic acid (EDTA). Initial dissolution rates were determined to be 0.126 mM/m 2/h for citric acid, 1.35 mM/m 2/h for oxalic acid, and 5.176 mM/m 2/h for EDTA. These rates compare with 0.0025 mM/m 2/h for nitric acid at pH=2. Organic acids dissolve Mn oxide quickly. Reaction rates increase with acid concentration, as tested with citric acid. The dissolution mechanism likely involves proton and ligand-promoted dissolution and reductive dissolution. Citric and oxalic acid can induce ligand-promoted dissolution, while EDTA can induce ligand-promoted and reductive dissolutions. At low pH, proton-promoted dissolution seems to occur with all the acids tested, but this process is not dominant. Reductive dissolution appears to be the most effective process in dissolving the solid, followed by ligand-promoted dissolution. These experiments indicate the significant

  17. Optimization of three FISH procedures for in situ detection of anaerobic ammonium oxidizing bacteria in biological wastewater treatment.

    Science.gov (United States)

    Pavlekovic, Marko; Schmid, Markus C; Schmider-Poignee, Nadja; Spring, Stefan; Pilhofer, Martin; Gaul, Tobias; Fiandaca, Mark; Löffler, Frank E; Jetten, Mike; Schleifer, K-H; Lee, Natuschka M

    2009-08-01

    Fluorescence in situ hybridization (FISH) using fluorochrome-labeled DNA oligonucleotide probes has been successfully applied for in situ detection of anaerobic ammonium oxidizing (anammox) bacteria. However, application of the standard FISH protocols to visualize anammox bacteria in biofilms from a laboratory-scale wastewater reactor produced only weak signals. Increased signal intensity was achieved either by modifying the standard FISH protocol, using peptide nucleic acid probes (PNA FISH), or applying horse radish peroxidase- (HRP-) labeled probes and subsequent catalyzed reporter deposition (CARD-FISH). A comparative analysis using anammox biofilm samples and suspended anammox biomass from different laboratory wastewater bioreactors revealed that the modified standard FISH protocol and the PNA FISH probes produced equally strong fluorescence signals on suspended biomass, but only weak signals were obtained with the biofilm samples. The probe signal intensities in the biofilm samples could be enhanced by enzymatic pre-treatment of fixed cells, and by increasing the hybridization time of the PNA FISH protocol. CARD-FISH always produced up to four-fold stronger fluorescent signals but unspecific fluorescence signals, likely caused by endogenous peroxidases as reported in several previous studies, compromised the results. Interference of the development of fluorescence intensity with endogenous peroxidases was also observed in cells of aerobic ammonium oxidizers like Nitrosomonas europea, and sulfate-reducers like Desulfobacter postgatei. Interestingly, no interference was observed with other peroxidase-positive microorganisms, suggesting that CARD-FISH is not only compromised by the mere presence of peroxidases. Pre-treatment of cells to inactivate peroxidase with HCl or autoclavation/pasteurization failed to inactive peroxidases, but H(2)O(2) significantly reduced endogenous peroxidase activity. However, for optimal inactivation, different H(2)O(2

  18. Role of oxidizing agent in the chemistry of in-situ uranium leaching

    International Nuclear Information System (INIS)

    Carlson, R.H.; Norris, R.D.; Schellinger, R.

    1982-01-01

    Synthetic two-component mixtures (uraninite and iron sulfide) as well as native uranium ores obtained from Texas and Wyoming have been examined. Physical/chemical ore properties are correlated with observed laboratory leach response. Data show a large inherent selectivity of oxidant for uranium in the early stages of a leach period. Uranium head grade was found to increase in a nearly linear fashion with hydrogen peroxide concentration in the leach solution. As uranium in the ore is depleted, uranium response decreases and the oxidant serves mainly to leach iron sulfide gangue material. 6 refs

  19. In situ carbon nanotube reinforcements in a plasma-sprayed aluminum oxide nanocomposite coating

    International Nuclear Information System (INIS)

    Balani, K.; Zhang, T.; Karakoti, A.; Li, W.Z.; Seal, S.; Agarwal, A.

    2008-01-01

    Carbon nanotubes (CNT) are potential reinforcements for toughening the ceramic matrix. The critical issue of avoiding CNT agglomeration and introducing CNT-matrix anchoring has challenged many researchers to improve the mechanical properties of the CNT reinforced nanocomposite. In the current work, dispersed CNTs are grown on Al 2 O 3 powder particles in situ by the catalytic chemical vapor deposition (CCVD) technique. Consequently, 0.5 wt.% CNT-reinforced Al 2 O 3 particles were successfully plasma sprayed to obtain a 400 μm thick coating on the steel substrate. In situ CNTs grown on Al 2 O 3 shows a promising enhancement in hardness and fracture toughness of the plasma-sprayed coating attributed to the existence of strong metallurgical bonding between Al 2 O 3 particles and CNTs. In addition, CNT tentacles have imparted multi-directional reinforcement in securing the Al 2 O 3 splats. High-resolution transmission electron microscopy shows interfacial fusion between Al 2 O 3 and CNT and the formation of Y-junction nanotubes

  20. Carbon sequestration in soil by in situ catalyzed photo-oxidative polymerization of soil organic matter.

    Science.gov (United States)

    Piccolo, Alessandro; Spaccini, Riccardo; Nebbioso, Antonio; Mazzei, Pierluigi

    2011-08-01

    Here we describe an innovative mechanism for carbon sequestration in soil by in situ photopolymerization of soil organic matter under biomimetic catalysis. Three different Mediterranean soils were added with a synthetic water-soluble iron-porphyrin, irradiated by solar light, and subjected first to 5 days incubation and, then, 15, and 30 wetting and drying (w/d) cycles. The in situ catalyst-assisted photopolymerization of soil organic carbon (SOC) increased water stability of soil aggregates both after 5 days incubation and 15 w/d cycles, but not after 30 w/d cycles. Particle-size distribution of all treated soils confirmed the induced soil physical improvement, by showing a concomitant lower yield of the clay-sized fraction and larger yields of either coarse sand- or fine sand-size fractions, depending on soil texture, though only after 5 days incubation. The gain in soil physical quality was reflected by the shift of OC content from small to large soil aggregates, thereby suggesting that photopolymerization stabilized OC by both chemical and physical processes. A further evidence of the carbon sequestration capacity of the photocatalytic treatment was provided by the significant reduction of CO(2) respired by all soils after both incubation and w/d cycles. Our findings suggest that "green" catalytic technologies may potentially be the bases for future practices to increase soil carbon stabilization and mitigate CO(2) emissions from arable soils.

  1. In situ iron activated persulfate oxidative fluid sparging treatment of TCE contamination--a proof of concept study.

    Science.gov (United States)

    Liang, Chenju; Lee, I-Ling

    2008-09-10

    In situ chemical oxidation (ISCO) is considered a reliable technology to treat groundwater contaminated with high concentrations of organic contaminants. An ISCO oxidant, persulfate anion (S(2)O(8)(2-)) can be activated by ferrous ion (Fe(2+)) to generate sulfate radicals (E(o)=2.6 V), which are capable of destroying trichloroethylene (TCE). The property of polarity inhibits S(2)O(8)(2-) or sulfate radical (SO(4)(-)) from effectively oxidizing separate phase TCE, a dense non-aqueous phase liquid (DNAPL). Thus the oxidation primarily takes place in the aqueous phase where TCE is dissolved. A bench column study was conducted to demonstrate a conceptual remediation method by flushing either S(2)O(8)(2-) or Fe(2+) through a soil column, where the TCE DNAPL was present, and passing the dissolved mixture through either a Fe(2+) or S(2)O(8)(2-) fluid sparging curtain. Also, the effect of a solubility enhancing chemical, hydroxypropyl-beta-cyclodextrin (HPCD), was tested to evaluate its ability to increase the aqueous TCE concentration. Both flushing arrangements may result in similar TCE degradation efficiencies of 35% to 42% estimated by the ratio of TCE degraded/(TCE degraded+TCE remained in effluent) and degradation byproduct chloride generation rates of 4.9 to 7.6 mg Cl(-) per soil column pore volume. The addition of HPCD did greatly increase the aqueous TCE concentration. However, the TCE degradation efficiency decreased because the TCE degradation was a lower percentage of the relatively greater amount of dissolved TCE by HPCD. This conceptual treatment may serve as a reference for potential on-site application.

  2. In situ secondary organic aerosol formation from ambient pine forest air using an oxidation flow reactor

    Science.gov (United States)

    Palm, Brett B.; Campuzano-Jost, Pedro; Ortega, Amber M.; Day, Douglas A.; Kaser, Lisa; Jud, Werner; Karl, Thomas; Hansel, Armin; Hunter, James F.; Cross, Eben S.; Kroll, Jesse H.; Peng, Zhe; Brune, William H.; Jimenez, Jose L.

    2016-03-01

    An oxidation flow reactor (OFR) is a vessel inside which the concentration of a chosen oxidant can be increased for the purpose of studying SOA formation and aging by that oxidant. During the BEACHON-RoMBAS (Bio-hydro-atmosphere interactions of Energy, Aerosols, Carbon, H2O, Organics & Nitrogen-Rocky Mountain Biogenic Aerosol Study) field campaign, ambient pine forest air was oxidized by OH radicals in an OFR to measure the amount of SOA that could be formed from the real mix of ambient SOA precursor gases, and how that amount changed with time as precursors changed. High OH concentrations and short residence times allowed for semicontinuous cycling through a large range of OH exposures ranging from hours to weeks of equivalent (eq.) atmospheric aging. A simple model is derived and used to account for the relative timescales of condensation of low-volatility organic compounds (LVOCs) onto particles; condensational loss to the walls; and further reaction to produce volatile, non-condensing fragmentation products. More SOA production was observed in the OFR at nighttime (average 3 µg m-3 when LVOC fate corrected) compared to daytime (average 0.9 µg m-3 when LVOC fate corrected), with maximum formation observed at 0.4-1.5 eq. days of photochemical aging. SOA formation followed a similar diurnal pattern to monoterpenes, sesquiterpenes, and toluene+p-cymene concentrations, including a substantial increase just after sunrise at 07:00 local time. Higher photochemical aging (> 10 eq. days) led to a decrease in new SOA formation and a loss of preexisting OA due to heterogeneous oxidation followed by fragmentation and volatilization. When comparing two different commonly used methods of OH production in OFRs (OFR185 and OFR254-70), similar amounts of SOA formation were observed. We recommend the OFR185 mode for future forest studies. Concurrent gas-phase measurements of air after OH oxidation illustrate the decay of primary VOCs, production of small oxidized organic

  3. In situ secondary organic aerosol formation from ambient pine forest air using an oxidation flow reactor

    Directory of Open Access Journals (Sweden)

    B. B. Palm

    2016-03-01

    Full Text Available An oxidation flow reactor (OFR is a vessel inside which the concentration of a chosen oxidant can be increased for the purpose of studying SOA formation and aging by that oxidant. During the BEACHON-RoMBAS (Bio-hydro-atmosphere interactions of Energy, Aerosols, Carbon, H2O, Organics & Nitrogen–Rocky Mountain Biogenic Aerosol Study field campaign, ambient pine forest air was oxidized by OH radicals in an OFR to measure the amount of SOA that could be formed from the real mix of ambient SOA precursor gases, and how that amount changed with time as precursors changed. High OH concentrations and short residence times allowed for semicontinuous cycling through a large range of OH exposures ranging from hours to weeks of equivalent (eq. atmospheric aging. A simple model is derived and used to account for the relative timescales of condensation of low-volatility organic compounds (LVOCs onto particles; condensational loss to the walls; and further reaction to produce volatile, non-condensing fragmentation products. More SOA production was observed in the OFR at nighttime (average 3 µg m−3 when LVOC fate corrected compared to daytime (average 0.9 µg m−3 when LVOC fate corrected, with maximum formation observed at 0.4–1.5 eq. days of photochemical aging. SOA formation followed a similar diurnal pattern to monoterpenes, sesquiterpenes, and toluene+p-cymene concentrations, including a substantial increase just after sunrise at 07:00 local time. Higher photochemical aging (> 10 eq. days led to a decrease in new SOA formation and a loss of preexisting OA due to heterogeneous oxidation followed by fragmentation and volatilization. When comparing two different commonly used methods of OH production in OFRs (OFR185 and OFR254-70, similar amounts of SOA formation were observed. We recommend the OFR185 mode for future forest studies. Concurrent gas-phase measurements of air after OH oxidation illustrate the decay of primary VOCs, production

  4. Structure, nonstoichiometry, sintering and oxygen permeability of perovskite SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.05, 0.10) oxides

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Jin Na [College of Chemistry and Materials Science, Liaoning University of Petroleum and Chemical Technology, Fushun 113001 (China); State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); Lu, Hui, E-mail: huilu@dicp.ac.cn [Greenhouse Gas Research Center, Climate Change Technology Research Division, Korea Institute of Energy Research, Daejeon 305-343 (Korea, Republic of); State Key Laboratory of Catalysis, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023 (China); Gui, Jian Zhou [College of Chemistry and Materials Science, Liaoning University of Petroleum and Chemical Technology, Fushun 113001 (China); Kim, Jong Pyo; Son, Sou Hwan [Greenhouse Gas Research Center, Climate Change Technology Research Division, Korea Institute of Energy Research, Daejeon 305-343 (Korea, Republic of); Park, Jung Hoon, E-mail: pjhoon@kier.re.kr [Greenhouse Gas Research Center, Climate Change Technology Research Division, Korea Institute of Energy Research, Daejeon 305-343 (Korea, Republic of)

    2013-04-20

    Highlights: ► The novel Fe/Nb co-substituted SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.05, 0.10) oxides were characterized by the XRD, DSC, TG and SEM–EDS. ► The high structural stability of the co-substituted SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.05, 0.10) oxides. ► The excellent oxygen permeation performance of the co-substituted SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.10) membrane. -- Abstract: The novel Fe/Nb co-substituted SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.05, 0.10) oxides have been synthesized and characterized by X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetry (TG), and scanning electron microscopy (SEM). The XRD and DSC results demonstrate that the structural stability of the Fe/Nb co-substituted samples x = 0.05, 0.10 is improved greatly compared to the sample x = 0.00. The Fe/Nb co-doping in the SrCoO{sub 3−δ} oxide results in the improved structural stability of the SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.05, 0.10) oxides. The nonstoichiometric and sintering properties were investigated by TG and SEM, and the oxygen permeation fluxes were measured at 800–950 °C for the sample x = 0.10. The improved oxygen permeability of the ceramic SrCo{sub 1−2x}(Fe,Nb){sub x}O{sub 3−δ} (x = 0.10) membrane compared to the (Ba{sub 0.5}Sr{sub 0.5})(Co{sub 0.8}Fe{sub 0.2})O{sub 3−δ} and SrCo{sub 0.8}Fe{sub 0.2}O{sub 3–δ} membranes, was observed under an air/He oxygen partial pressure gradient at 800–950 °C.

  5. Co-sintering of CGO/NIO-CGO bilayers for solid oxide fuel cell; Co-sinterizacao de bi-camadas anodo/eletrolito para celulas a combustivel de oxido solido

    Energy Technology Data Exchange (ETDEWEB)

    Neto, P.P.B.; Grilo, J.P.F.; Souza, G.L.; Macedo, D.A.; Paskocimas, C.A.; Nascimento, R.M., E-mail: pbritoneto@gmail.com [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

    2012-07-01

    Reducing the operating temperature of solid oxide fuel cells (SOFC) for the range between 500 and 700°C is one of the challenges which more has aroused the interest of research in SOFC in recent years. In this context, the bilayer anode/electrolyte composed of a porous support based on Ni-doped ceria (anode) and a ceria doped gadolinia (CGO) electrolyte, presents itself as one of the half-cell configurations of the most interest towards the production of electricity in the operating logic of a SOFC. In this work, CGO films were successfully prepared on NiO-CGO substrates using the resources of the screen-printing technique. The bi-layers were co-sintered between 1350 and 1450 ° C for 4 h and then characterized by scanning electron microscopy and energy dispersive X-ray spectroscopy (EDS). The results showed good adhesion at the film/substrate interface and no cracks in the films. (author)

  6. Reaction and Transport Processes Controlling In Situ Chemical Oxidation of DNAPLs

    Science.gov (United States)

    2006-11-01

    Contact Areas. Ground Water, 36(4):495-502. Atlas , R.M., and R. Bartha (1987). Microbial Ecology , Benjamin/Cummings Publishing Company, Menlo Park...relatively few species ( Atlas and Bartha 1987). If selection for bioremediation processes following oxidation does occur, competition for substrates...Experiments.....................................................................3-23 3.6.3. Microbial Culture Preparation for Evaluation of Coupling

  7. Advances In Groundwater Remediation: Achieving Effective In Situ Delivery Of Chemical Oxidants And Amendments

    DEFF Research Database (Denmark)

    Siegrist, Robert L.; Crimi, Michelle; McCray, John E.

    of organically contaminated sites. Many of the most prevalent organic contaminants of concern (COCs) at sites in urban areas (e.g., chlorinated solvents, motor and heating fuels) can be destroyed using oxidants such as catalyzed hydrogen peroxide (H2O2), potassium permanganate (KMnO4), sodium persulfate (Na2S2O8...

  8. In-Situ Regeneration of Saturated Granular Activated Carbon by an Iron Oxide Nanocatalyst

    Science.gov (United States)

    Granular activated carbon (GAC) can remove trace organic pollutants and natural organic matter (NOM) from industrial and municipal waters. This paper evaluates an iron nanocatalyst approach, based on Fenton-like oxidation reactions, to regenerate spent GAC within a packed bed con...

  9. Improved Modeling Approaches for Constrained Sintering of Bi-Layered Porous Structures

    DEFF Research Database (Denmark)

    Tadesse Molla, Tesfaye; Frandsen, Henrik Lund; Esposito, Vincenzo

    2012-01-01

    Shape instabilities during constrained sintering experiment of bi-layer porous and dense cerium gadolinium oxide (CGO) structures have been analyzed. An analytical and a numerical model based on the continuum theory of sintering has been implemented to describe the evolution of bow and densificat...

  10. Microwave Sintering of Ceramic Materials for Industrial Application Final Report CRADA No. TC-1116-95

    Energy Technology Data Exchange (ETDEWEB)

    Caplan, M. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Tandon, R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Callis, R. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2017-10-19

    The goal of this project was to develop the commercial capability in the US to sinter alumina oxide ceramic parts for the semiconductor manufacturing equipment industry. We planned to use the millimeter microwave (30 GHz) sintering system first developed by IAP in Russia.

  11. Influence of sintering temperature on the properties of pulsed electric current sintered hybrid coreshell powders

    Czech Academy of Sciences Publication Activity Database

    Mahmed, N.; Larismaa, J.; Heczko, Oleg; Cura, M.E.; Hannula, S.-P.

    2013-01-01

    Roč. 33, č. 12 (2013), s. 2233-2239 ISSN 0955-2219 R&D Projects: GA ČR(CZ) GAP107/11/0391 Institutional support: RVO:68378271 Keywords : sintering * silver * iron oxide * SiO 2 * phase transformation Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.307, year: 2013 http://dx.doi.org/10.1016/j.jeurceramsoc.2012.12.023

  12. Insight into the structure of Pd/ZrO2 during the total oxidation of methane using combined in situ XRD, X.-ray absorption and Raman spectroscopy

    DEFF Research Database (Denmark)

    Grunwaldt, Jan-Dierk; van Vegten, Niels; Baiker, Alfons

    2009-01-01

    The structure of palladium during the total combustion of methane has been studied by a combination of the complementary in situ techniques X-ray absorption spectroscopy, Raman spectroscopy and X-ray diffraction. The study demonstrates that finely dispersed and oxidized palladium is most active f...

  13. The effect of water on the stability of iron oxide and iron carbide nanoparticles in hydrogen and syngas followed by in situ X-ray absorption spectroscopy

    NARCIS (Netherlands)

    Thuene, P.C.; Moodley - Gengan, P.; Scheijen, F.J.E.; Fredriksson, H.O.A.; Lancee, R.J.; Kropf, J.; Miller, J.T.; Niemantsverdriet, J.W.

    2012-01-01

    The effect of water on iron-based nanoparticles under hydrogen and syngas was investigated by in situ X-ray absorption spectroscopy. The iron oxide (¿-Fe2O3) nanoparticles, dispersed as a monolayer on flat silica surfaces, were readily converted into metallic iron in dry hydrogen at 350 °C and into

  14. Structural evaluation of reduced graphene oxide in graphene oxide during ion irradiation: X-ray absorption spectroscopy and in-situ sheet resistance studies

    Science.gov (United States)

    Saravanan, K.; Jayalakshmi, G.; Suresh, K.; Sundaravel, B.; Panigrahi, B. K.; Phase, D. M.

    2018-03-01

    We report the structural evolution of reduced graphene oxide (rGO) in graphene oxide (GO) flakes during 1 MeV Si+ ion irradiation. In-situ electrical resistivity measurements facilitate monitoring the sheet resistance with the increase in the fluence. The electrical sheet resistance of the GO flake shows the exponential decay behaviour with the increasing ion fluence. Raman spectra of the GO flake reveal the increase in the ID/IG ratio, indicating restoration of the sp2 network upon irradiation. The C/O ratio estimated from resonant Rutherford backscattering spectrometry analysis directly evidenced the reduction of oxygen moieties upon irradiation. C K-edge X-ray absorption near edge structure spectra reveal the restoration of C=C sp2-hybridized carbon atoms and the removal of oxygen-containing functional groups in the GO flake. STM data reveal the higher conductance in the rGO regime in comparison with the regime, where the oxygen functional groups are present. The experimental investigation demonstrates that the ion irradiation can be employed for efficient reduction of GO with tunable electrical and structural properties.

  15. In situ synthesis and catalytic application of reduced graphene oxide supported cobalt nanowires

    Science.gov (United States)

    Xu, Zhiqiang; Long, Qin; Deng, Yi; Liao, Li

    2018-05-01

    Controlled synthesis of magnetic nanocomposite with outstanding catalytic performances is a promising strategy in catalyst industry. We proposed a novel concept for fabrication of reduced graphene oxide-supported cobalt nanowires (RGO/Co-NWs) nanocomposite as high-efficient magnetic catalyst. Unlike the majority of experiments necessitating harsh synthesis conditions such as high-pressure, high-temperature and expensive template, here the RGO/Co-NWs were successfully prepared in aqueous solution under mild conditions with the assistance of external magnetic field. The synthetic process was facile and external magnetic force was adopted to induce the unidirectional self-assembly of cobalt crystals on graphene oxide to form RGO/Co-NWs. The possible formation mechanism laid on the fact that the dipole magnetic moments of the nanoparticles were aligned along the magnetic induction lines with the external magnetic field direction resulting in the formation of nanowires elongating in the direction of the magnetization axis. Simultaneously, a series of controlled reactions were conducted to illuminate the effect of graphene oxide, external magnetic field and PVP on the morphology and size of RGO/Co-NWs in the present approach. More importantly, the nanocomposite exhibited a high catalytic performance towards ammonia borane. Hence the novel nanocomposite holds a great potential for technological applications such as catalyst industry.

  16. Performing in-situ chemical oxidation with Fenton's Reagent at a former gas work in Rotterdam

    Energy Technology Data Exchange (ETDEWEB)

    Plaisier, W.; Pancras, T. [In-situ Technieken BV, Wageningen (Netherlands); Bennen, M.; Bouwhuis, E. [Public Works Rotterdam (Netherlands)

    2003-07-01

    In-Situ Technieken BV is the first company in the Netherlands to apply full-scale in-situ chemical oxidation (ISCO) by means of Fenton's reagent or permanganates. The use of ISCO for soil remediation purposes originated in the USA. After three years of practical experience in the Netherlands it can be stated that ISCO has become a proven technology for source area treatment in the Netherlands as well. We present the results of a pilot ISCO treatment program with Fenton's reagent that was performed at the former gas works facility 'Feyenoord'. The site is one of the largest gas works facilities built in Rotterdam. The former gas production activities have lead to severe pollution of soil and groundwater over an area of approximately 3 hectares. Both laboratory and field observations showed that it would be very difficult to execute an efficient Fenton's reagent ISCO treatment program at this specific site for the following reasons. First of all, the contamination consisting of tar and tar-related compounds is found in an anthropogenic (man-made) soil of 9 meter in thickness. Secondly, high contents of carbonates and organic material were found in the soils, which act as a scavenger for the hydroxyl free radical in a Fenton's reagent ISCO system. The pilot test was performed in two phases with an intermediate period of 2 months. The injection of totally 24 tonnes hydrogen peroxide (50%) was anticipated. Reactions of the reagents in the soil were very strong. The presence of old (forgotten) boreholes and an intensive drainage system, in combination with the aggressive reaction resulted in short-circuiting of reagents to the surface. Out of the proposed 24 tonnes of hydrogen peroxide (50%) only 14.5 tonnes were injected. This would have effect on the amount of contamination oxidized. Nevertheless, the oxidation had a significant effect on the soil contamination. A reduction of approximately 90% for PAH was obtained. Reduction was also

  17. Two-step sintering of ultrafine-grained barium cerate proton conducting ceramics

    International Nuclear Information System (INIS)

    Wang, Siwei; Zhang, Lei; Zhang, Lingling; Brinkman, Kyle; Chen, Fanglin

    2013-01-01

    Ultra-fine grained dense BaZr 0.1 Ce 0.7 Y 0.1 Yb 0.1 O 3−δ (BZCYYb) ceramics have been successfully prepared via a two-step sintering method. Co-precipitation method has been adopted to prepare nano-sized BZCYYb precursors with an average particle size of 30 nm. By controlling the sintering profile, an average grain size of 184 nm was obtained for dense BZCYYb ceramics via the two-step sintering method, compared to 445 nm for the conventional sintered samples. The two-step sintered BZCYYb samples showed less impurity and an enhanced electrical conductivity compared with the conventional sintered ones. Further, the two-step sintering method was applied to fabricate anode supported solid oxide fuel cells (SOFCs) using BZCYYb as the electrolyte, resulting in dense ultrafine-grained electrolyte membranes and porous anode substrates with fine particles. Due to the reduced ohmic as well as polarization resistances, the maximum power output of the cells fabricated from the two-step sintering method reached 349 mW m −2 at 700 °C, significantly improved from 172 mW cm −2 for the conventional sintered cells, suggesting that two-step sintering method is very promising for optimizing the microstructure and thus enhancing the electrochemical performances for barium cerate based proton-conducting SOFCs.

  18. Mechanisms of sintering

    International Nuclear Information System (INIS)

    Mohan, Ashok; Soni, N.C.; Moorthy, V.K.

    1980-01-01

    The basic mechanisms by which the material moves during sintering have not only held a strange fascination but are also very important in determining the properties of the end product. Kuczynski's exponent method has been subsequently refined by several schools to make it increasingly reliable. There is now a fairly good understanding of mechanisms in some of the materials. However in others the issue is complicated by their basic nature. The problems of ambiguity in criterion and that of more than one mechanism being simultaneously operative have been tackled with dexterity by Ashby for drawing sintering mechanism diagrams. The method has been modified to give Relative Contribution Diagrams (RCD). These yield additional information and have been used for analysis. The main criticism against this is that it uses a very large number of rate equations and material properties, which can communicate their inaccuracies to the diagram. A case study of UO 2 was undertaken and it has been shown quantitatively that inaccuracies in a smaller number of properties only affect the diagrams to any significant extent. (auth.)

  19. Development of KMnO(4)-releasing composites for in situ chemical oxidation of TCE-contaminated groundwater.

    Science.gov (United States)

    Liang, S H; Chen, K F; Wu, C S; Lin, Y H; Kao, C M

    2014-05-01

    The objective of this study was to develop a controlled-oxidant-release technology combining in situ chemical oxidation (ISCO) and permeable reactive barrier (PRB) concepts to remediate trichloroethene (TCE)-contaminated groundwater. In this study, a potassium permanganate (KMnO4)-releasing composite (PRC) was designed for KMnO4 release. The components of this PRC included polycaprolactone (PCL), KMnO4, and starch with a weight ratio of 1.14:2:0.96. Approximately 64% (w/w) of the KMnO4 was released from the PRC after 76 days of operation in a batch system. The results indicate that the released KMnO4 could oxidize TCE effectively. The results from a column study show that the KMnO4 released from 200 g of PRC could effectively remediate 101 pore volumes (PV) of TCE-contaminated groundwater (initial TCE concentration = 0.5 mg/L) and achieve up to 95% TCE removal. The effectiveness of the PRC system was verified by the following characteristics of the effluents collected after the PRC columns (barrier): (1) decreased TCE concentrations, (2) increased ORP and pH values, and (3) increased MnO2 and KMnO4 concentrations. The results of environmental scanning electron microscope (ESEM) analysis show that the PCL and starch completely filled up the pore spaces of the PRC, creating a composite with low porosity. Secondary micro-scale capillary permeability causes the KMnO4 release, mainly through a reaction-diffusion mechanism. The PRC developed could be used as an ISCO-based passive barrier system for plume control, and it has the potential to become a cost-effective alternative for the remediation of chlorinated solvent-contaminated groundwater. Copyright © 2014 Elsevier Ltd. All rights reserved.

  20. Steam reforming of methanol over oxide decorated nanoporous gold catalysts: a combined in situ FTIR and flow reactor study.

    Science.gov (United States)

    Shi, J; Mahr, C; Murshed, M M; Gesing, T M; Rosenauer, A; Bäumer, M; Wittstock, A

    2017-03-29

    Methanol as a green and renewable resource can be used to generate hydrogen by reforming, i.e., its catalytic oxidation with water. In combination with a fuel cell this hydrogen can be converted into electrical energy, a favorable concept, in particular for mobile applications. Its realization requires the development of novel types of structured catalysts, applicable in small scale reactor designs. Here, three different types of such catalysts were investigated for the steam reforming of methanol (SRM). Oxides such as TiO 2 and CeO 2 and mixtures thereof (Ce 1 Ti 2 O x ) were deposited inside a bulk nanoporous gold (npAu) material using wet chemical impregnation procedures. Transmission electron and scanning electron microscopy reveal oxide nanoparticles (1-2 nm in size) abundantly covering the strongly curved surface of the nanoporous gold host (ligaments and pores on the order of 40 nm in size). These catalysts were investigated in a laboratory scaled flow reactor. First conversion of methanol was detected at 200 °C. The measured turn over frequency at 300 °C of the CeO x /npAu catalyst was 0.06 s -1 . Parallel investigation by in situ infrared spectroscopy (DRIFTS) reveals that the activation of water and the formation of OH ads are the key to the activity/selectivity of the catalysts. While all catalysts generate sufficient OH ads to prevent complete dehydrogenation of methanol to CO, only the most active catalysts (e.g., CeO x /npAu) show direct reaction with formic acid and its decomposition to CO 2 and H 2 . The combination of flow reactor studies and in operando DRIFTS, thus, opens the door to further development of this type of catalyst.

  1. Iron oxides stimulate microbial monochlorobenzene in situ transformation in constructed wetlands and laboratory systems

    International Nuclear Information System (INIS)

    Schmidt, Marie; Wolfram, Diana; Birkigt, Jan; Ahlheim, Jörg; Paschke, Heidrun; Richnow, Hans-Hermann; Nijenhuis, Ivonne

    2014-01-01

    Natural wetlands are transition zones between anoxic ground and oxic surface water which may enhance the (bio)transformation potential for recalcitrant chloro-organic contaminants due to the unique geochemical conditions and gradients. Monochlorobenzene (MCB) is a frequently detected groundwater contaminant which is toxic and was thought to be persistent under anoxic conditions. Furthermore, to date, no degradation pathways for anoxic MCB removal have been proven in the field. Hence, it is important to investigate MCB biodegradation in the environment, as groundwater is an important drinking water source in many European countries. Therefore, two pilot-scale horizontal subsurface-flow constructed wetlands, planted and unplanted, were used to investigate the processes in situ contributing to the biotransformation of MCB in these gradient systems. The wetlands were fed with anoxic MCB-contaminated groundwater from a nearby aquifer in Bitterfeld, Germany. An overall MCB removal was observed in both wetlands, whereas just 10% of the original MCB inflow concentration was detected in the ponds. In particular in the gravel bed of the planted wetland, MCB removal was highest in summer season with 73 ± 9% compared to the unplanted one with 40 ± 5%. Whereas the MCB concentrations rapidly decreased in the transition zone of unplanted gravel to the pond, a significant MCB removal was already determined in the anoxic gravel bed of the planted system. The investigation of hydro-geochemical parameters revealed that iron and sulphate reduction were relevant redox processes in both wetlands. In parallel, the addition of ferric iron or nitrate stimulated the mineralisation of MCB in laboratory microcosms with anoxic groundwater from the same source, indicating that the potential for anaerobic microbial degradation of MCB is present at the field site. - Highlights: • MCB removal in anoxic gravel bed of a planted and an unplanted constructed wetland was accompanied by iron

  2. Iron oxides stimulate microbial monochlorobenzene in situ transformation in constructed wetlands and laboratory systems

    Energy Technology Data Exchange (ETDEWEB)

    Schmidt, Marie; Wolfram, Diana; Birkigt, Jan [Department of Isotope Biogeochemistry, Helmholtz Centre for Environmental Research — UFZ, Permoserstrasse 15, 04318 Leipzig (Germany); Ahlheim, Jörg [Department of Groundwater Remediation, Helmholtz Centre for Environmental Research — UFZ, Permoserstrasse 15, 04318 Leipzig (Germany); Paschke, Heidrun [Department of Analytical Chemistry, Helmholtz Centre for Environmental Research — UFZ, Permoserstrasse 15, 04318 Leipzig (Germany); Richnow, Hans-Hermann [Department of Isotope Biogeochemistry, Helmholtz Centre for Environmental Research — UFZ, Permoserstrasse 15, 04318 Leipzig (Germany); Nijenhuis, Ivonne, E-mail: ivonne.nijenhuis@ufz.de [Department of Isotope Biogeochemistry, Helmholtz Centre for Environmental Research — UFZ, Permoserstrasse 15, 04318 Leipzig (Germany)

    2014-02-01

    Natural wetlands are transition zones between anoxic ground and oxic surface water which may enhance the (bio)transformation potential for recalcitrant chloro-organic contaminants due to the unique geochemical conditions and gradients. Monochlorobenzene (MCB) is a frequently detected groundwater contaminant which is toxic and was thought to be persistent under anoxic conditions. Furthermore, to date, no degradation pathways for anoxic MCB removal have been proven in the field. Hence, it is important to investigate MCB biodegradation in the environment, as groundwater is an important drinking water source in many European countries. Therefore, two pilot-scale horizontal subsurface-flow constructed wetlands, planted and unplanted, were used to investigate the processes in situ contributing to the biotransformation of MCB in these gradient systems. The wetlands were fed with anoxic MCB-contaminated groundwater from a nearby aquifer in Bitterfeld, Germany. An overall MCB removal was observed in both wetlands, whereas just 10% of the original MCB inflow concentration was detected in the ponds. In particular in the gravel bed of the planted wetland, MCB removal was highest in summer season with 73 ± 9% compared to the unplanted one with 40 ± 5%. Whereas the MCB concentrations rapidly decreased in the transition zone of unplanted gravel to the pond, a significant MCB removal was already determined in the anoxic gravel bed of the planted system. The investigation of hydro-geochemical parameters revealed that iron and sulphate reduction were relevant redox processes in both wetlands. In parallel, the addition of ferric iron or nitrate stimulated the mineralisation of MCB in laboratory microcosms with anoxic groundwater from the same source, indicating that the potential for anaerobic microbial degradation of MCB is present at the field site. - Highlights: • MCB removal in anoxic gravel bed of a planted and an unplanted constructed wetland was accompanied by iron

  3. Ash chemistry and sintering, verification of the mechanisms

    Energy Technology Data Exchange (ETDEWEB)

    Hupa, M.; Skrifvars, B.J. [Aabo Akademi, Turku (Finland)

    1996-12-01

    In this project four sintering mechanisms have been studied, i.e., partial melting with a viscous liquid, partial melting with a non-viscous liquid, chemical reaction sintering and solid state sintering. The work has aimed at improving the understanding of ash sintering mechanisms and quantifying their role in combustion and gasification. The work has been oriented in particular on the understanding of biomass ash behavior. The work has not directly focused on any specific technical application. However, results can also be applied on other fuels such as brown coal, petroleum coke, black liquor and different types of wastes (PDF, RDF, MSW). In one part of study the melting behavior was calculated for ten biomass ashes and compared with lab measurements of sintering tendencies. The comparison showed that the T{sub 15} temperatures, i.e. those temperatures at which the ashes contained 15 % molten phase, correlated fairly well with the temperature at which the sintering measurements detected sintering. This suggests that partial melting can be predicted fairly accurate for some ashes already with the today existing thermodynamic calculation routines. In some cases, however the melting calculations did not correlate with the detected sintering temperatures. In a second part detailed measurements on ash behavior was conducted both in a semi full scale CFB and a lab scale FBC. Ashes and deposits were collected and analyzed in several different ways. These analyses show that the ash chemistry shifts radically when the fuel is shifted. Fuels with silicate based ashes behaved totally different than those with an oxide or salt based ash. The chemistry was also affected by fuel blending. The ultimate goal has been to be able to predict the ash thermal behavior during biomass thermal conversion, using the fuel and ash elemental analyses and a few operational key parameters as the only input data. This goal has not yet today been achieved. (author)

  4. Effect of processing conditions on microstructural features in Mn–Si sintered steels

    Energy Technology Data Exchange (ETDEWEB)

    Oro, Raquel, E-mail: raqueld@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Hryha, Eduard, E-mail: hryha@chalmers.se [Department of Materials and Manufacturing Technology, Chalmers University of Technology, Rännvägen 2A, SE-41296 Gothenburg (Sweden); Campos, Mónica, E-mail: campos@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); Torralba, José M., E-mail: torralba@ing.uc3m.es [Department of Materials Science and Engineering, IAAB, Universidad Carlos III de Madrid, Av. Universidad 30, 28911 Leganés, Madrid (Spain); IMDEA Materials Institute, c/Eric Kandel, 2, 28906 Getafe, Madrid (Spain)

    2014-09-15

    Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain

  5. Effect of processing conditions on microstructural features in Mn–Si sintered steels

    International Nuclear Information System (INIS)

    Oro, Raquel; Hryha, Eduard; Campos, Mónica; Torralba, José M.

    2014-01-01

    Sintering of steels containing oxidation sensitive elements is possible if such elements are alloyed with others which present lower affinity for oxygen. In this work, a master alloy powder containing Fe–Mn–Si–C, specifically designed to create a liquid phase during sintering, has been used for such purpose. The effect of processing conditions such as sintering temperature and atmosphere was studied with the aim of describing the microstructural evolution as well as the morphology and distribution of oxides in the sintered material, evaluating the potential detrimental effect of such oxides on mechanical properties. Chemical analyses, metallography and fractography studies combined with X-ray photoelectron spectroscopy analyses on the fracture surfaces were used to reveal the main mechanism of fracture and their correlation with the chemical composition of the different fracture surfaces. The results indicate that the main mechanism of failure in these steels is brittle fracture in the surrounding of the original master alloy particles due to degradation of grain boundaries by the presence of oxide inclusions. Mn–Si oxide inclusions were observed on intergranular decohesive facets. The use of reducing atmospheres and high sintering temperatures reduces the amount and size of such oxide inclusions. Besides, high heating and cooling rates reduce significantly the final oxygen content in the sintered material. A model for microstructure development and oxide evolution during different stages of sintering is proposed, considering the fact that when the master alloy melts, the liquid formed can dissolve some of the oxides as well as the surface of the surrounding iron base particles. - Highlights: • Oxide distribution in steels containing oxidation-sensitive elements • Mn, Si introduced in a master alloy powder, mixed with a base iron powder • Selective oxidation of Mn and Si on iron grain boundaries • Decohesive fracture caused by degradation of grain

  6. In situ monitoring magnetism and resistance of nanophase platinum upon electrochemical oxidation

    Directory of Open Access Journals (Sweden)

    Eva-Maria Steyskal

    2013-06-01

    Full Text Available Controlled tuning of material properties by external stimuli represents one of the major topics of current research in the field of functional materials. Electrochemically induced property tuning has recently emerged as a promising pathway in this direction making use of nanophase materials with a high fraction of electrode-electrolyte interfaces. The present letter reports on electrochemical property tuning of porous nanocrystalline Pt. Deeper insight into the underlying processes could be gained by means of a direct comparison of the charge-induced response of two different properties, namely electrical resistance and magnetic moment. For this purpose, four-point resistance measurements and SQUID magnetometry were performed under identical in situ electrochemical control focussing on the regime of electrooxidation. Fully reversible variations of the electrical resistance and the magnetic moment of 6% and 1% were observed upon the formation or dissolution of a subatomic chemisorbed oxygen surface layer, respectively. The increase of the resistance, which is directly correlated to the amount of deposited oxygen, is considered to be primarily caused by charge-carrier scattering processes at the metal–electrolyte interfaces. In comparison, the decrease of the magnetic moment upon positive charging appears to be governed by the electric field at the nanocrystallite–electrolyte interfaces due to spin–orbit coupling.

  7. Oxygen supply and oxidative phosphorylation limitation in rat myocardium in situ.

    Science.gov (United States)

    Kreutzer, U; Mekhamer, Y; Chung, Y; Jue, T

    2001-05-01

    The 1H-NMR signal of the proximal histidyl-N(delta)H of deoxymyoglobin is detectable in the in situ rat myocardium and can reflect the intracellular PO2. Under basal normoxic conditions, the cellular PO2 is sufficient to saturate myoglobin (Mb). No proximal histidyl signal of Mb is detectable. On ligation of the left anterior descending coronary artery, the Mb signal at 78 parts/million (ppm) appears, along with a peak shoulder assigned to the corresponding signal of Hb. During dopamine infusion up to 80 microg. kg(-1) x min(-1), both the heart rate-pressure product (RPP) and myocardial oxygen consumption (MVO2) increase by about a factor of 2. Coronary flow increases by 84%, and O2 extraction (arteriovenous O2 difference) rises by 31%. Despite the increased respiration and work, no deoxymyoglobin signal is detected, implying that the intracellular O2 level still saturates MbO2, well above the PO2 at 50% saturation of Mb. The phosphocreatine (PCr) level decreases, however, during dopamine stimulation, and the ratio of the change in P(i) over PCr (DeltaP(i)/PCr) increases by 0.19. Infusion of either pyruvate, as the primary substrate, or dichloroacetate, a pyruvate dehydrogenase activator, abolishes the change in DeltaP(i)/PCr. Intracellular O2 supply does not limit MVO2, and the role of ADP in regulating respiration in rat myocardium in vivo remains an open question.

  8. In situ reduced graphene oxide interlayer for improving electrode performance in ZnO nanorods

    Science.gov (United States)

    Venkatesan, A.; Ramesha, C. K.; Kannan, E. S.

    2016-06-01

    The effect of reduced graphene oxide (RGO) thin film on the transport characteristics of vertically aligned zinc oxide nanorods (ZnO NRs) grown on ITO substrate was studied. GO was uniformly drop casted on ZnO NRs as a passivation layer and then converted into RGO by heating it at 60 °C prior to metal electrode deposition. This low temperature reduction is facilitated by the thermally excited electrons from ZnI interstitial sites (~30 meV). Successful reduction of GO was ascertained from the increased disorder band (D) intensity in the Raman spectra. Temperature (298 K-10 K) dependent transport measurements of RGO-ZnO NRs indicate that the RGO layer not only acts as a short circuiting inhibitor but also reduces the height of the potential barrier for electron tunneling. This is confirmed from the temperature dependent electrical characteristics which revealed a transition of carrier transport from thermionic emission at high temperature (T  >  100 K) to tunneling at low temperature (T  <  100 K) across the interface. Our technique is the most promising approach for making reliable electrical contacts on vertically aligned ZnO NRs and improving the reproducibility of device characteristics.

  9. The Nucleation Potency of In Situ-Formed Oxides in Liquid Iron

    Science.gov (United States)

    Xu, Mingqin; Wang, Lu; Lu, Wenquan; Zeng, Long; Nadendla, Hari-Babu; Wang, Yun; Li, Jun; Hu, Qiaodan; Xia, Mingxu; Li, Jianguo

    2018-03-01

    The nucleation potency of iron oxides was verified experimentally through nucleation undercooling of liquid iron using aerodynamic levitation technology for minimized container contaminations. Steady undercooling values were subsequently obtained from multiple melting and freezing thermal cycles, with the average undercooling values of 223 K ± 3 K and 75 K ± 6 K (223 °C ± 3 °C and 75 °C ± 6 °C) for FeO-contained liquid and Fe3O4-contained liquid, respectively. The statistical results showed a negligible difference in the sizes and numbers of particles between FeO and Fe3O4 particles, indicating that the nucleation potency difference is attributed to the nature of nucleants rather than particle size or numbers. Furthermore, high-resolution transmission electron microscopy analysis showed that the potential nucleation interfaces can be assumed as { 1 1 0}_{{δ {{-Fe}}}} //( 0 0\\bar{2})_{FeO} and { 1 1 2}_{{δ {{-Fe}}}} //(\\bar{2} 0 2 )_{{{Fe}3 {O}4 }} , based on the detected exposed crystal planes of the oxide particles. Both the interfaces have relatively large values of lattice misfit, consistent with the experimentally measured undercooling based on Turnbull's lattice matching theory.

  10. Low sintering temperature glass waste forms for sequestering radioactive iodine

    Science.gov (United States)

    Nenoff, Tina M.; Krumhansl, James L.; Garino, Terry J.; Ockwig, Nathan W.

    2012-09-11

    Materials and methods of making low-sintering-temperature glass waste forms that sequester radioactive iodine in a strong and durable structure. First, the iodine is captured by an adsorbant, which forms an iodine-loaded material, e.g., AgI, AgI-zeolite, AgI-mordenite, Ag-silica aerogel, ZnI.sub.2, CuI, or Bi.sub.5O.sub.7I. Next, particles of the iodine-loaded material are mixed with powdered frits of low-sintering-temperature glasses (comprising various oxides of Si, B, Bi, Pb, and Zn), and then sintered at a relatively low temperature, ranging from 425.degree. C. to 550.degree. C. The sintering converts the mixed powders into a solid block of a glassy waste form, having low iodine leaching rates. The vitrified glassy waste form can contain as much as 60 wt % AgI. A preferred glass, having a sintering temperature of 500.degree. C. (below the silver iodide sublimation temperature of 500.degree. C.) was identified that contains oxides of boron, bismuth, and zinc, while containing essentially no lead or silicon.

  11. Long-Term Stability of Anode-Supported Solid Oxide Fuel Cells with a Co-Sintered Cathode Backbone and Infiltrated La0.95Co0.4Ni0.6O3 (LCN) Electro-Catalyst

    DEFF Research Database (Denmark)

    Küngas, Rainer; Veltzé, Sune; Ovtar, Simona

    2016-01-01

    Infiltration is a fabrication method that is offering potentially significant improvements in cell performance at reduced materials and fabrication costs, especially when combined with co-sintering. However, important questions regarding the long-term performance and microstructural stability of ...

  12. Method to produce sintered carriers for electrodes of galvanic elements

    Energy Technology Data Exchange (ETDEWEB)

    Jost, E M

    1978-03-24

    Carrier plates of precisely uniform thickness can be produced according to the invention by firstly thickening a solution of polyethylene oxide and (preferably) methanol by adding water and then, by adding nickel powder, obtaining an essentially homogeneous suspension of considerable viscosity. This slurry is coated on both sides of a nickel grid, dried and sintered.

  13. Spectroelectrochemical cell for in situ studies of solid oxide fuel cells

    International Nuclear Information System (INIS)

    Hagen, Anke; Lund Traulsen, Marie; Kiebach, Wolff-Ragnar; Johansen, Bjoern Sejr

    2012-01-01

    Solid oxide fuel cells (SOFCs) are able to produce electricity and heat from hydrogen- or carbon-containing fuels with high efficiencies and are considered important cornerstones for future sustainable energy systems. Performance, activation and degradation processes are crucial parameters to control before the technology can achieve breakthrough. They have been widely studied, predominately by electrochemical testing with subsequent micro-structural analysis. In order to be able to develop better SOFCs, it is important to understand how the measured electrochemical performance depends on materials and structural properties, preferably at the atomic level. A characterization of these properties under operation is desired. As SOFCs operate at temperatures around 1073 K, this is a challenge. A spectroelectrochemical cell was designed that is able to study SOFCs at operating temperatures and in the presence of relevant gases. Simultaneous spectroscopic and electrochemical evaluation by using X-ray absorption spectroscopy and electrochemical impedance spectroscopy is possible. (orig.)

  14. Spectroelectrochemical cell for in situ studies of solid oxide fuel cells

    DEFF Research Database (Denmark)

    Hagen, Anke; Traulsen, Marie Lund; Kiebach, Wolff-Ragnar

    2012-01-01

    to control before the technology can achieve breakthrough. They have been widely studied, predominately by electrochemical testing with subsequent micro-structural analysis. In order to be able to develop better SOFCs, it is important to understand how the measured electrochemical performance depends......Solid oxide fuel cells (SOFCs) are able to produce electricity and heat from hydrogen- or carbon-containing fuels with high efficiencies and are considered important cornerstones for future sustainable energy systems. Performance, activation and degradation processes are crucial parameters...... on materials and structural properties, preferably at the atomic level. A characterization of these properties under operation is desired. As SOFCs operate at temperatures around 1073 K, this is a challenge. A spectroelectrochemical cell was designed that is able to study SOFCs at operating temperatures...

  15. Production of pure sintered alumina

    International Nuclear Information System (INIS)

    Rocha, J.C. da; Huebner, H.W.

    1982-01-01

    With the aim of optimizing the sintering parameters, the strength of a large number of alumina samples was determined which were produced under widely varying sintering conditions and with different amounts of MgO content. The strength as a function of sintering time or temperature was found to go through a maximum. With increasing time, this maximum is shifted to lower temperatures, and with decreasing temperature to longer times. Data pairs of sintering times and temperatures which yeld the strength maximum were determined. The value of the strength at the maximum remains unchanged. The strength is high (= 400 MN/m 2 , at a grain size of 3 um and a porosity of 2 per cent) and comparable to foreign aluminas produced for commercial purposes, or even higher. The increase in the sintering time from 1 h to 16 h permits a reduction of the sintering temperature from 1600 to 1450 0 C without losing strength. The practical importance of this fact for a production of sintered alumina on a large scale is emphasized. (Author) [pt

  16. In situ electrochemical creation of cobalt oxide nanosheets with favorable performance as a high tap density anode material for lithium-ion batteries

    International Nuclear Information System (INIS)

    Lin, Qian; Sha, Yujing; Zhao, Bote; Chen, Yubo; Tadé, Moses O.; Shao, Zongping

    2015-01-01

    Highlights: • Cobalt oxide nanosheets in situ electrochemical generated from commercial LiCoO_2. • TEM indicates creation of cobalt oxide nanosheets from coarse layered LiCoO_2_. • Coarse-type LiCoO_2 with high tap density shows promising anode performance. • Optimizing weight ratio of LiCoO_2 in electrode, a high capacity was achieved. - Abstract: Cobalt oxides are attractive alternative anode materials for next-generation lithium-ion batteries (LIBs). To improve the performance of conversion-type anode materials such as cobalt oxides, well dispersed and nanosized particulate morphology is typically required. In this study, we describe the in situ electrochemical generation of cobalt oxide nanosheets from commercial micrometer-sized LiCoO_2 oxide as an anode material for LIBs. The electrode material as prepared was analyzed by XRD, FE-SEM and TEM. The electrochemical properties were investigated by cyclic voltammetry and by a constant current galvanostatic discharge–charge test. The material shows a high tap density and promising anode performance in terms of capacity, rate performance and cycling stability. A capacity of 560 mA h g"−"1 is still achieved at a current density of 1000 mA g"−"1 by increasing the amount of additives in the electrode to 40 wt%. This paper provides a new technique for developing a high-performance conversion-type anode for LIBs.

  17. Thermosensitive polymer-grafted iron oxide nanoparticles studied by in situ dynamic light backscattering under magnetic hyperthermia

    Science.gov (United States)

    Hemery, Gauvin; Garanger, Elisabeth; Lecommandoux, Sébastien; Wong, Andrew D.; Gillies, Elizabeth R.; Pedrono, Boris; Bayle, Thomas; Jacob, David; Sandre, Olivier

    2015-12-01

    Thermometry at the nanoscale is an emerging area fostered by intensive research on nanoparticles (NPs) that are capable of converting electromagnetic waves into heat. Recent results suggest that stationary gradients can be maintained between the surface of NPs and the bulk solvent, a phenomenon sometimes referred to as ‘cold hyperthermia’. However, the measurement of such highly localized temperatures is particularly challenging. We describe here a new approach to probing the temperature at the surface of iron oxide NPs and enhancing the understanding of this phenomenon. This approach involves the grafting of thermosensitive polymer chains to the NP surface followed by the measurement of macroscopic properties of the resulting NP suspension and comparison to a calibration curve built up by macroscopic heating. Superparamagnetic iron oxide NPs were prepared by the coprecipitation of ferrous and ferric salts and functionalized with amines, then azides using a sol-gel route followed by a dehydrative coupling reaction. Thermosensitive poly[2-(dimethylamino)ethyl methacrylate] (PDMAEMA) with an alkyne end-group was synthesized by controlled radical polymerization and was grafted using a copper assisted azide-alkyne cycloaddition reaction. Measurement of the colloidal properties by dynamic light scattering (DLS) indicated that the thermosensitive NPs exhibited changes in their Zeta potential and hydrodynamic diameter as a function of pH and temperature due to the grafted PDMAEMA chains. These changes were accompanied by changes in the relaxivities of the NPs, suggesting application as thermosensitive contrast agents for magnetic resonance imaging (MRI). In addition, a new fibre-based backscattering setup enabled positioning of the DLS remote-head as close as possible to the coil of a magnetic heating inductor to afford in situ probing of the backscattered light intensity, hydrodynamic diameter, and temperature. This approach provides a promising platform for

  18. In situ formation of low friction ceramic coatings on carbon steel by plasma electrolytic oxidation in two types of electrolytes

    International Nuclear Information System (INIS)

    Wang Yunlong; Jiang Zhaohua

    2009-01-01

    In situ formation of ceramic coatings on Q235 carbon steel was achieved by plasma electrolytic oxidation (PEO) in carbonate electrolyte and silicate electrolyte, respectively. The surface and cross-section morphology, phase and elemental composition of PEO coatings were examined by means of scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy-dispersive X-ray spectroscopy (EDS). The bond strength of the coating was determined using a direct pull-off test. The hardness as well as tribological properties of the ceramic coating was primarily studied. The results indicated that the coating obtained in carbonate electrolyte was Fe 3 O 4 , while the coating achieved from silicate electrolyte was proved to be amorphous. Both kinds of coatings showed coarse and porous surface. The Fe 3 O 4 coatings obtained in carbonate electrolyte showed a high bonding strength to the substrate up to 20 ± 2 MPa and the value was 15 ± 2 MPa for the amorphous coatings obtained in carbonate electrolyte. The micro hardness of the amorphous coating and the Fe 3 O 4 coating was 1001 Hv and 1413 Hv, respectively, which was more than two and three times as that of the Q235 alloy substrate (415 Hv). The friction coefficient exhibited by amorphous coating and Fe 3 O 4 coating was 0.13 and 0.11, respectively, both lower than the uncoated Q235 substrate which ranged from 0.17 to 0.35.

  19. In situ synthesized SnO2 nanorod/reduced graphene oxide low-dimensional structure for enhanced lithium storage.

    Science.gov (United States)

    Zhang, Wei; Xiao, Xuezhang; Zhang, Yiwen; Li, Junpeng; Zhong, Jiayi; Li, Meng; Fan, Xiulin; Wang, Chuntao; Chen, Lixin

    2018-03-09

    A unique SnO 2 nanorod (NR)/reduced graphene oxide (RGO) composite morphology has been synthesized using the in situ hydrothermal method, for use as an anode material in lithium-ion batteries. The SnO 2 NR adhering to the RGO exhibits a length of 250-400 nm and a diameter of 60-80 nm without any obvious aggregation. The initial discharge/charge capacities of the SnO 2 NR/RGO composite are 1761.3 mAh g -1 and 1233.1 mAh g -1 , with a coulombic efficiency (CE) of 70% under a current density of 200 mA g -1 , and a final capacity of 1101 mAh g -1 after 50 cycles. The rate capability of the SnO 2 NR/RGO is also improved compared to that of bare SnO 2 NR. The superior electrochemical performance is ascribed to the special morphology of the SnO 2 NRs-which plays a role in shorting the transmission path-and the sheet-like 2D graphene, which prevents the agglomeration of SnO 2 and enhances conductivity during the electrochemical reaction of SnO 2 NR/RGO.

  20. In situ synthesized SnO2 nanorod/reduced graphene oxide low-dimensional structure for enhanced lithium storage

    Science.gov (United States)

    Zhang, Wei; Xiao, Xuezhang; Zhang, Yiwen; Li, Junpeng; Zhong, Jiayi; Li, Meng; Fan, Xiulin; Wang, Chuntao; Chen, Lixin

    2018-03-01

    A unique SnO2 nanorod (NR)/reduced graphene oxide (RGO) composite morphology has been synthesized using the in situ hydrothermal method, for use as an anode material in lithium-ion batteries. The SnO2 NR adhering to the RGO exhibits a length of 250-400 nm and a diameter of 60-80 nm without any obvious aggregation. The initial discharge/charge capacities of the SnO2 NR/RGO composite are 1761.3 mAh g-1 and 1233.1 mAh g-1, with a coulombic efficiency (CE) of 70% under a current density of 200 mA g-1, and a final capacity of 1101 mAh g-1 after 50 cycles. The rate capability of the SnO2 NR/RGO is also improved compared to that of bare SnO2 NR. The superior electrochemical performance is ascribed to the special morphology of the SnO2 NRs—which plays a role in shorting the transmission path—and the sheet-like 2D graphene, which prevents the agglomeration of SnO2 and enhances conductivity during the electrochemical reaction of SnO2 NR/RGO.

  1. Synthesis of HNTs@PEDOT composites via in situ chemical oxidative polymerization and their application in electrode materials

    Science.gov (United States)

    Wang, Fang; Zhang, Xianhong; Ma, Yuhong; Yang, Wantai

    2018-01-01

    The hybrid composite of poly(3,4-ethylenedioxythiophene) (PEDOT) and halloysite nanotubes (HNTs) was synthesized by a two-step process. First, poly(sodium styrene sulfonate) (PSSNa) was grafted onto HNTs via surface initiated atom transfer radical polymerization. Then with the HNTs-g-PSS as a template and the grafted PSS chains as the counterion dopant, PEDOT was precipitated onto the template via in situ oxidization polymerization of EDOT to form HNTs@PEDOT hybrid composites. The conductivity of HNTs@PEDOT can reach up to 9.35 S/cm with the content of 40% HNTs-g-PSS, which increased almost 78 times than that of pure PEDOT (about 0.12 S/cm) prepared at the similar condition. Further treated with p-toluenesulfonic acid (TsOH) as external dopant, the conductivity of HNTs@PEDOT increased to 24.3 S/cm. The electrochemical properties of the composites were investigated with cyclic voltammetry, galvanostatic charge-discharge and electrochemical impedance spectroscopy with three-electrode cell configuration. The results showed that the capacitance of HNTs@PEDOT composite increased 55% than that of pure PEDOT.

  2. Multifunctional properties of cotton fabrics coated with in situ synthesis of zinc oxide nanoparticles capped with date seed extract.

    Science.gov (United States)

    El-Naggar, Mehrez E; Shaarawy, S; Hebeish, A A

    2018-02-01

    In situ formation of zinc oxide nanoparticles (ZnO-NPs) was studied within the framework of several factors. variables examined include (i) innovation of a new capping agent; (ii) nature of the cotton fabric related to its processing; (iii) formation of Zinc hydroxide (Zn(OH) 2 ) due to reduction of zinc acetate with sodium hydroxide (iv) treatment of the differently processed cotton fabrics with (Zn(OH) 2 ) functionalized dispersion as per the exhaustion method, (v) further treatment of the cotton fabrics with (Zn(OH) 2 ) dispersion according to the pad-dry-cure method and (Vi) conversion of (Zn(OH) 2 ) to ZnO-NPs during the curing step in the latter method. Results depict that the incorporation of the bio-extract obtained from date seed waste works effectively as capping material which stabilize ZnO-NPs. Mercerized bleached cotton fabric proves to be a better candidate than mercerized loomstate cotton fabric in conferring sustainable bactericidal and UV blocking. Copyright © 2017 Elsevier Ltd. All rights reserved.

  3. Enhanced electrochemical performance of in situ reduced graphene oxide-polyaniline nanotubes hybrid nanocomposites using redox-additive aqueous electrolyte

    Science.gov (United States)

    Devi, Madhabi; Kumar, A.

    2018-02-01

    Reduced graphene oxide (RGO)-polyaniline nanotubes (PAniNTs) nanocomposites have been synthesized by in situ reduction of GO. The morphology and structure of the nanocomposites are characterized by HRTEM, XRD and micro-Raman spectroscopy. The electrical and electrochemical performances of the nanocomposites are investigated for different RGO concentrations by conductivity measurements, cyclic voltammetry, charge-discharge and electrochemical impedance spectroscopy. Highest gravimetric specific capacitance of 448.71 F g-1 is obtained for 40 wt.% of RGO-PAniNTs nanocomposite as compared to 194.92 F g-1 for pure PAniNTs in 1 M KCl electrolyte. To further improve the electrochemical performance of the nanocomposite electrode, KI is used as redox-additive with 1 M KCl electrolyte. Highest gravimetric specific capacitance of 876.43 F g-1 and an improved cyclic stability of 91% as compared to 79% without KI after 5000 cycles is achieved for an optimized 0.1 M KI concentration. This is attributed to the presence of different ionic species of I- ions that give rise to a number of possible redox reactions improving the pseudocapacitance of the electrode. This improved capacitive performance is compared with that of catechol redox-additive in 1 M KCl electrolyte, and that of KI and catechol redox-additives added to 1 M H2SO4 electrolyte.

  4. Anomalous Resistance Hysteresis in Oxide ReRAM: Oxygen Evolution and Reincorporation Revealed by In Situ TEM.

    Science.gov (United States)

    Cooper, David; Baeumer, Christoph; Bernier, Nicolas; Marchewka, Astrid; La Torre, Camilla; Dunin-Borkowski, Rafal E; Menzel, Stephan; Waser, Rainer; Dittmann, Regina

    2017-06-01

    The control and rational design of redox-based memristive devices, which are highly attractive candidates for next-generation nonvolatile memory and logic applications, is complicated by competing and poorly understood switching mechanisms, which can result in two coexisting resistance hystereses that have opposite voltage polarity. These competing processes can be defined as regular and anomalous resistive switching. Despite significant characterization efforts, the complex nanoscale redox processes that drive anomalous resistive switching and their implications for current transport remain poorly understood. Here, lateral and vertical mapping of O vacancy concentrations is used during the operation of such devices in situ in an aberration corrected transmission electron microscope to explain the anomalous switching mechanism. It is found that an increase (decrease) in the overall O vacancy concentration within the device after positive (negative) biasing of the Schottky-type electrode is associated with the electrocatalytic release and reincorporation of oxygen at the electrode/oxide interface and is responsible for the resistance change. This fundamental insight presents a novel perspective on resistive switching processes and opens up new technological opportunities for the implementation of memristive devices, as anomalous switching can now be suppressed selectively or used deliberately to achieve the desirable so-called deep Reset. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. In situ studies of uranium-plutonium mixed oxides. Influence of composition on phase equilibria and thermodynamic properties

    International Nuclear Information System (INIS)

    Strach, Michal

    2015-01-01

    Due to their physical and chemical properties, mixed uranium-plutonium oxides are considered for fuel in 4. generation nuclear reactors. In this frame, complementary experimental studies are necessary to develop a better understanding of the phenomena that take place during fabrication and operation in the reactor. The focus of this work was to study the U-Pu-O phase diagram in a wide range of compositions and temperatures to ameliorate our knowledge of the phase equilibria in this system. Most of experiments were done using in situ X-ray diffraction at elevated temperatures. The control of the oxygen partial pressure during the treatments made it possible to change the oxygen stoichiometry of the sample, which gave us an opportunity to study rapidly different compositions and the processes involved. The experimental approach was coupled with thermodynamic modeling using the CALPHAD method, to precisely plan the experiments and interpret the obtained results. This approach enabled us to enhance the knowledge of phase equilibria in the U-Pu-O system. (author) [fr

  6. In-situ preparation of poly(ethylene oxide)/Li3PS4 hybrid polymer electrolyte with good nanofiller distribution for rechargeable solid-state lithium batteries

    Science.gov (United States)

    Chen, Shaojie; Wang, Junye; Zhang, Zhihua; Wu, Linbin; Yao, Lili; Wei, Zhenyao; Deng, Yonghong; Xie, Dongjiu; Yao, Xiayin; Xu, Xiaoxiong

    2018-05-01

    Nano-sized fillers in a polymer matrix with good distribution can play a positive role in improving polymer electrolytes in the aspects of ionic conductivity, mechanical property and electrochemical performance of Li-ion cells. Herein, polyethylene oxide (PEO)/Li3PS4 hybrid polymer electrolyte is prepared via a new in-situ approach. The ionic conductivities of the novel hybrid electrolytes with variable proportions are measured, and the optimal electrolyte of PEO-2%vol Li3PS4 presents a considerable ionic conductivity of 8.01 × 10-4 S cm-1 at 60 °C and an electrochemical window up to 5.1 V. The tests of DSC and EDXS reveal that the Li3PS4 nanoparticles with better distribution, as active fillers scattering in the PEO, exhibit a positive effect on the transference of lithium ion and electrochemical interfacial stabilities. Finally, the assembled solid-state LiFePO4/Li battery presents a decent cycling performance (80.9% retention rate after 325 cycles at 60 °C) and excellent rate capacities with 153, 143, 139 and 127 mAh g-1 at the discharging rate of 0.1 C, 0.2 C, 0.5 C and 1 C at 60 °C. It is fully proved that it is an advanced strategy to preparing the new organic/inorganic hybrid electrolytes for lithium-ion batteries applications.

  7. Sinterability and microstructure evolution during sintering of ferrous powder mixtures

    Directory of Open Access Journals (Sweden)

    Kétner Bendo Demétrio

    2013-01-01

    Full Text Available The present work is focused on ferrous powder metallurgy and presents some results of a development of a suitable masteralloy for use as an additive to iron powder for the production of sintered steels. The masteralloy was produced by melting a powder mixture containing approximately Fe + 20% Ni + 20% Mn + 20% Si + 1% C (wt%, in order to obtain a cast billet that was converted into fine powder by crushing and milling. It was observed presence of SiC in the masteralloy after melting that is undesirable in the alloy. Si element should be introduced by using ferrosilicon. Sintered alloys with distinct contents of alloying elements were prepared by mixing the masteralloy powder to plain iron powder. Samples were produced by die compaction of the powder mixtures and sintering at 1200 °C in a differential dilatometer in order to record their linear dimensional behaviour during heating up and isothermal sintering, aiming at studying the sinterability of the compacts. Microstructure development during sintering was studied by SEM, XRD and microprobe analyses.

  8. The pressureless sintering and mechanical properties of AlON ceramic

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, N., E-mail: zhangning5832@163.com [Key Lab. of Advanced Materials and Manufacturing Technology of Liaoning Province, Shenyang University, Shenyang, Liaoning 110044 (China); Liang, B.; Wang, X.Y.; Kan, H.M.; Zhu, K.W. [Key Lab. of Advanced Materials and Manufacturing Technology of Liaoning Province, Shenyang University, Shenyang, Liaoning 110044 (China); Zhao, X.J. [Department of Materials Science and Engineering, School of Materials and Metallurgy, Northeastern University, Shenyang, Liaoning 110004 (China)

    2011-07-25

    Highlights: {yields} A one-step pressureless sintering process was proposed, which is simple and viable. {yields} Cheap and easily available {alpha}-Al{sub 2}O{sub 3} and aluminum powders were chosen as raw materials substituting for expensive AlN ultrafine powders. {yields} The sintering temperature of AlON ceramic was reduced by 50 deg. C and the flexural strength was enhanced by 29.4%. - Abstract: Aluminum oxynitride (AlON) ceramic was synthesized by one-step pressureless sintering technology using low cost and easily available {alpha}-Al{sub 2}O{sub 3} and aluminum powders as raw materials. The sintering temperature was reduced because aluminum powders were nitridized into high activity AlN under the flowing nitrogen atmosphere. The curves of thermal analysis, microstructure and atomic distribution were investigated. The influence of sintering temperatures on phase composition, sintering densification and flexural strength was also explored. The experimental results showed that {alpha}-Al{sub 2}O{sub 3} and aluminum powders were acceptable substitutes for more expensive AlN ultrafine powders. Under the optimum sintering process at 1750 deg. C for 2 h, the sintered density and flexural strength of AlON ceramic were higher, 3.62 g/cm{sup 3} and 321 MPa, respectively. The sintering temperature was decreased by 50 deg. C because newly formed high activity AlN in situ reacted with Al{sub 2}O{sub 3} into Al{sub 23}O{sub 27}N{sub 5}, enhancing flexural strength by 29.4%. However, the sintering temperature could not be too high because grain growth and displacement of oxygen atoms from AlON ceramics by nitrogen atoms caused a decline in sintering densification and flexural strength.

  9. Lanthanide (Nd, Gd) compounds with garnet and monazite structures. Powders synthesis by “wet” chemistry to sintering ceramics by Spark Plasma Sintering

    Energy Technology Data Exchange (ETDEWEB)

    Potanina, Ekaterina, E-mail: ekaterina.potanina@list.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Golovkina, Ludmila, E-mail: golovkina_lyudmila@mail.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Orlova, Albina, E-mail: albina.orlova@inbox.ru [Department of Solid State Chemistry, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 2, 603950 Nizhny Novgorod (Russian Federation); Nokhrin, Aleksey, E-mail: nokhrin@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation); Boldin, Maksim, E-mail: boldin@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation); Sakharov, Nikita, E-mail: nvsaharov@nifti.unn.ru [Research Institute of Physics and Technology, Lobachevsky State University of Nizhni Novgorod, National Research University, 23 Prospekt Gagarina, BLDG 3, 603950 Nizhny Novgorod (Russian Federation)

    2016-05-15

    Complex oxide Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} with garnet structure and phosphates NdPO{sub 4} and GdPO{sub 4} with monazite structure were obtained by using precipitation methods. Ceramics Y{sub 2.5}Nd{sub 0.5}Al{sub 5}O{sub 12} and NdPO{sub 4} were processed by Spark Plasma Sintering (SPS). Relative density more 98%, sintering time did not exceed 8 min, sintering temperature 1330–1390 °C. Leaching rates of elements from ceramics were 10{sup −6}–10{sup −7} g/(cm{sup 2} d). The process of ceramics sintering has two-stage character: the first step of sintering-compaction process is related to the plastic flow of the material, the second step–to the process of grain boundary diffusion and grain growth. - Highlights: • Powders were obtained by precipitation (sol–gel) method. • Ceramics were sintering by Spark Plasma Sintering method (ρ{sub rel} > 98%); shrinkage time does not exceed 8 min. • The process of ceramics sintering has two-stage character.

  10. Special metallurgy - the electrical butt-welding by flashing of sintered magnesium-magnesium oxide composites (1963); Metallurgie speciale - le soudage electrique en bout par etincelage du composite fritte magnesium-magnesie (1963)

    Energy Technology Data Exchange (ETDEWEB)

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

    1963-07-01

    Electrical resistance welding has become quite important since World War II because of the need of a high yield in aeronautical production. Progress has been due in particular to the improvements made in electronically controlled apparatus making possible the automatic control of welding. For the butt-welding of sections requiring either a high production rate or a high quality weld, the flash butt-welding system has been very much developed these last few years. The use of this welding method is of great importance in the field of the bonding of oxidisable metals such as magnesium or aluminium and its alloys, because the welded joint is free from oxides. This study consists of general considerations on the flash-welding process with regard to temperature distribution in the parts during welding, and to electrical phenomena connected with flashing. Besides this general or theoretical section, we have applied the welding process to the bonding of sintered magnesium, a magnesium-magnesium oxide composite, whose use as a structural element in nuclear reactors is considered. (author) [French] Le soudage electrique par resistance a pris un essor important depuis la derniere guerre mondiale a cause du besoin de haut rendement pour la production aeronautique. Les progres ont ete possibles surtout par l'amelioration des appareils de commande electronique qui permettent un controle automatique de la soudure. Pour le soudage bout a bout de profiles, demandant soit un haut debit de fabrication, soit une haute qualite du joint soude, le procede de soudage en bout par etincelage a ete tres developpe ces dernieres annees. Ce mode de soudage a un domaine d'utilisation important dans la liaison des metaux oxydables tels le magnesium ou l'aluminium et ses alliages, du fait de la proprete du joint soude exempt d'oxydes. Cette etude comporte une consideration generale du processus de l'etincelage, quant a la repartition de la temperature dans les pieces pendant le soudage et aux

  11. Special metallurgy - the electrical butt-welding by flashing of sintered magnesium-magnesium oxide composites (1963); Metallurgie speciale - le soudage electrique en bout par etincelage du composite fritte magnesium-magnesie (1963)

    Energy Technology Data Exchange (ETDEWEB)

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

    1963-07-01

    Electrical resistance welding has become quite important since World War II because of the need of a high yield in aeronautical production. Progress has been due in particular to the improvements made in electronically controlled apparatus making possible the automatic control of welding. For the butt-welding of sections requiring either a high production rate or a high quality weld, the flash butt-welding system has been very much developed these last few years. The use of this welding method is of great importance in the field of the bonding of oxidisable metals such as magnesium or aluminium and its alloys, because the welded joint is free from oxides. This study consists of general considerations on the flash-welding process with regard to temperature distribution in the parts during welding, and to electrical phenomena connected with flashing. Besides this general or theoretical section, we have applied the welding process to the bonding of sintered magnesium, a magnesium-magnesium oxide composite, whose use as a structural element in nuclear reactors is considered. (author) [French] Le soudage electrique par resistance a pris un essor important depuis la derniere guerre mondiale a cause du besoin de haut rendement pour la production aeronautique. Les progres ont ete possibles surtout par l'amelioration des appareils de commande electronique qui permettent un controle automatique de la soudure. Pour le soudage bout a bout de profiles, demandant soit un haut debit de fabrication, soit une haute qualite du joint soude, le procede de soudage en bout par etincelage a ete tres developpe ces dernieres annees. Ce mode de soudage a un domaine d'utilisation important dans la liaison des metaux oxydables tels le magnesium ou l'aluminium et ses alliages, du fait de la proprete du joint soude exempt d'oxydes. Cette etude comporte une consideration generale du processus de l'etincelage, quant a la repartition de la temperature dans les pieces

  12. In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

    Science.gov (United States)

    Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

    2017-09-01

    The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

  13. Solidification of high level liquid waste (HLLW) into ceramics by sintering process

    International Nuclear Information System (INIS)

    Masuda, Sumio; Oguino, Naohiko; Tsunoda, Naomi; O-oka, Kazuo; Ohta, Takao.

    1979-01-01

    One of the alternatives to vitrified solid which is acceptable and well characterized for storing radioactive HLLW with desirable long-term stability is ceramics. On the other hand, the solidification process of highly radioactive wastes should be simple and suitable for continuous production. On the above described basis, the authors have made preliminary study on the production of sintered ceramics by the addition of several oxides to HLLW. The simulated waste and additive oxides were pressed in a mold to make the preforms of 50 mm diameter and 10 to 15 mm thick. The preforms were then normally sintered at temperature from 1000 to 1400 deg C for 2 to 4 hours. The characterization of the sintered solids revealed the following facts. (1) X-ray diffraction analysis showed that the expected crystals were formed by normal-sintering as well as by hot-pressing. (2) The bulk density of the ceramics by normal-sintering was around 90 to 95% of the assumed theoretical values. (3) The leach-rate of the solids was affected by the bulk density. (4) Other properties of the solids, such as thermal expansion or thermal conductivity, are dominantly determined by those of main crystals in the solids. Sintering process is generally simple and productive as far as normal sintering is concerned. However, hot-pressing is an intermittent and time consuming process. From this fact, the authors intended to adopt the normal sintering process for the ceramic solidification of high level liquid wastes. (Wakatsuki, Y.)

  14. Sintering of MSW fly ash for reuse as a concrete aggregate.

    Science.gov (United States)

    Mangialardi, T

    2001-10-12

    The sintering process of municipal solid waste (MSW) fly ash was investigated in order to manufacture sintered products for reuse as concrete aggregates. Four types of fly ash resulting from different Italian MSW incineration plants were tested in this study. A modification of the chemical composition of MSW fly ash--through a preliminary four-stage washing treatment of this material with water--was attempted to improve the chemical and mechanical characteristics of sintered products.The sintering treatment of untreated or washed fly ash was performed on cylindrical compact specimens (15 mm in diameter and 20mm in height) at different compact pressures, sintering temperatures and times.The sintering process of untreated MSW fly ashes proved to be ineffective for manufacturing sintered products for reuse as a construction material, because of the adverse chemical characteristics of these fly ashes in terms of sulfate, chloride, and vitrifying oxide contents.A preliminary washing treatment of MSW fly ash with water greatly improved the chemical and mechanical characteristics of sintered products and, for all the types of fly ash tested, the sintered products satisfied the Italian requirements for normal weight aggregates for use in concretes having a specified strength not greater than 12 and 15N/mm(2), when measured on cylindrical and cubic specimens, respectively.A compact pressure of 28 N/mm(2), a sintering temperature of 1140 degrees C, and a sintering time of 60 min were the best operating conditions for manufacturing sintered products of washed MSW fly ash.

  15. Two step sintering of zirconia-escandia-ceria

    International Nuclear Information System (INIS)

    Grosso, R.L.; Muccillo, E.N.S.

    2011-01-01

    Recent reports show that the ceramic system based on zirconia-scandia-ceria is a good candidate to act as solid electrolyte in solid oxide fuel cells operating at intermediate temperatures (600-800 °C). In this work, commercial ZrO_2 containing 10 mol% scandium oxide and 1 mol% cerium oxide was sintered by the two stage method. This technique was proposed to in order to obtain ceramic materials with high density along with fine grain sizes, because it avoids the grain growth occurring in the last stage of sintering. A number of experimental conditions were fully exploited by varying the dwell temperature (T_2) and the dwell time. The peak temperature (T_1) was chosen from linear shrinkage results. High (>98%) density values were obtained using this method. The medium grain size was evaluated for selected sintered samples. X-ray diffraction patterns reveal a secondary (rhombohedral) phase in sintered samples. The intensity of the secondary phase is a function of T_1 being small for relatively higher peak temperatures. (author)

  16. Applications of x ray absorption fine structure to the in situ study of the effect of cobalt in nickel hydrous oxide electrodes for fuel cells and rechargeable batteries

    Science.gov (United States)

    Kim, Sunghyun; Tryk, Donald A.; Scherson, Daniel A.; Antonio, Mark R.

    1993-01-01

    Electronic and structural aspects of composite nickel-cobalt hydrous oxides have been examined in alkaline solutions using in situ X-ray absorption fine structure (XAFS). The results obtained have indicated that cobalt in this material is present as cobaltic ions regardless of the oxidation state of nickel in the lattice. Furthermore, careful analysis of the Co K-edge Extended X-ray absorption fine structure data reveals that the co-electrodeposition procedure generates a single phase, mixed metal hydrous oxide, in which cobaltic ions occupy nickel sites in the NiO2 sheet-like layers and not two intermixed phases each consisting of a single metal hydrous oxide.

  17. Spectroscopic identification of the active site for CO oxidation on Rh/Al{sub 2}O{sub 3} by concentration modulation in situ DRIFTS

    Energy Technology Data Exchange (ETDEWEB)

    Cavers, M.; Davidson, J.M.; Harkness, I.R.; Rees, L.V.C.; McDougall, G.S.

    1999-12-10

    Diffuse reflectance infrared spectroscopy experiments are described in which the concentrations of the reactant gases passing over a solid catalyst are modulated. This simple modification to the normal in situ experiment enables direct correlation of specific surface species with the production of gaseous products. Spectra of solely the active surface intermediates with no contribution from so called spectator species are generated. For CO oxidation over a Rh/alumina catalyst at 576 K, the active CO species is identified as linearly adsorbed CO on oxidized Rh sites ({nu}{sub CO} = 2,100 cm{sup {minus}1}) on a catalyst surface apparently otherwise dominated by CO adsorbed as unreactive geminal dicarbonyl.

  18. Evaluation of dilatometric techniques for studies of sintering kinetics

    International Nuclear Information System (INIS)

    El-Sayed Ali, M.; Toft Soerensen, O.

    1985-04-01

    The kinetics of the initial sintering stage of CeO 2 is evaluated by three different techniques: constant heating rate dilatometry, constant shrinkage rate dilatometry and a new technique recently introduced by the authors called Stepwise Isothermal Dilatometry (SID). Comparative measurements with these techniques showed that too high activation energies were obtained with the two first techniques, both of which can be termed as nonisothermal, whereas activation energies comparable to those reported for cation diffusion in other fluorite oxides were obtained with the latter technique. Of the three techniques SID is thus considered to be the most accurate for studies of the sintering kinetics. In contrast to the two nonisothermal techniques SID has the further advantage that both the controlling mechanism and its activation energy can be determined in a single experiment. From the SID-measurement it was concluded that the initial sintering stage of CeO 2 is controlled by grain-boundary diffusion. (author)

  19. Sintering and annealing effects on undoped yttria transparent ceramics

    Energy Technology Data Exchange (ETDEWEB)

    Letue, Laetitia; Petit, Johan, E-mail: johan.petit@onera.fr; Ritti, Marie-Hélène; Lalanne, Sylvie; Landais, Stéphane

    2017-06-15

    Transparent yttrium oxide (Y{sub 2}O{sub 3}) ceramics were processed by several densifications steps without any doping species. The green bodies were obtained by the aqueous way and sintered at high temperature under vacuum and then under high pressure. We studied the effects of different sintering cycles and air annealing at different steps of the process on the density and the grain growth. We also focused on the reaction between yttria ceramics and BN-coated graphite crucible which occurs during HIP. We noted that a low heating rate and two annealing steps are necessary to improve our samples’ transparency. - Highlights: • The quality of transparent ceramics is compared with the tested process parameters. • Air annealing is critical when using a carbon environment in the process. • Intra-granular pores, and so the final transparency, are directly linked to the sintering heating rates.

  20. N-nitrosodimethylamine (NDMA) formation potential of amine-based water treatment polymers: Effects of in situ chloramination, breakpoint chlorination, and pre-oxidation.

    Science.gov (United States)

    Park, Sang Hyuck; Padhye, Lokesh P; Wang, Pei; Cho, Min; Kim, Jae-Hong; Huang, Ching-Hua

    2015-01-23

    Recent studies show that cationic amine-based water treatment polymers may be important precursors that contribute to formation of the probable human carcinogen N-nitrosodimethylamine (NDMA) during water treatment and disinfection. To better understand how water treatment parameters affect NDMA formation from the polymers, the effects of in situ chloramination, breakpoint chlorination, and pre-oxidation on the NDMA formation from the polymers were investigated. NDMA formation potential (NDMA-FP) as well as dimethylamine (DMA) residual concentration were measured from poly(epichlorohydrin dimethylamine) (polyamine) and poly(diallyldimethylammonium chloride) (polyDADMAC) solutions upon reactions with oxidants including free chlorine, chlorine dioxide, ozone, and monochloramine under different treatment conditions. The results supported that dichloramine (NHCl2) formation was the critical factor affecting NDMA formation from the polymers during in situ chloramination. The highest NDMA formation from the polymers occurred near the breakpoint of chlorination. Polymer chain breakdown and transformation of the released DMA and other intermediates were important factors affecting NDMA formation from the polymers in pre-oxidation followed by post-chloramination. Pre-oxidation generally reduced NDMA-FP of the polymers; however, the treatments involving pre-ozonation increased polyDADMAC's NDMA-FP and DMA release. The strategies for reducing NDMA formation from the polymers may include the avoidance of the conditions favorable to NHCl2 formation and the avoidance of polymer exposure to strong oxidants such as ozone. Copyright © 2014 Elsevier B.V. All rights reserved.

  1. A study on the electro-oxidation and electropolymerization of a new OPE linear molecule by EQCM and in situ FTIR spectroelectrochemistry

    International Nuclear Information System (INIS)

    Luo Jiao; Liu Meiling; Zhao Qiangqin; Zhao Jie; Zhang Youyu; Tan Liang; Tang Hao; Xie Qingji; Li Haitao; Yao Shouzhuo

    2010-01-01

    A novel symmetric conjugated oligo(phenylene-ethynylene) (OPE) linear molecule (1,4-bis(4-aminophenylethynyl)benzene); BAB) was synthesized by Sonogashira cross-coupling reactions. The structure and purity of the compound were confirmed by 1 H NMR, 13 C NMR and infrared (IR) and mass spectrometry (MS). The electrochemical oxidation process and mechanism of BAB were investigated via in situ Fourier transform infrared (FTIR) spectroelectrochemistry and electrochemical quartz crystal microbalance (EQCM). The electrochemical oxidation mechanism of BAB was proposed. The studies revealed that the BAB concentration and oxidation potential had a significant influence on the growth of the polymer film. A densely packed polymer film, which exhibited nonelectroactivity, was formed when a high monomer concentration and a high oxidation potential were used. When the electropolymerization of BAB was conducted at a lower concentration, a new pair of redox peaks appeared, and the resultant thin film had better electroactivity. The in situ FTIR studies confirmed that BAB could be electro-oxidized into radical cations and then electropolymerized via para (N-N) and/or ortho (N-C) coupling reactions to form polymers with a larger conjugated π-electron system. The surface morphology of the poly-BAB was also investigated with atomic force microscopy (AFM) and scanning electron microscopy (SEM).

  2. Mineral Phases and Release Behaviors of As in the Process of Sintering Residues Containing As at High Temperature

    Directory of Open Access Journals (Sweden)

    Xingrun Wang

    2014-01-01

    Full Text Available To investigate the effect of sintering temperature and sintering time on arsenic volatility and arsenic leaching in the sinter, we carried out experimental works and studied the structural changes of mineral phases and microstructure observation of the sinter at different sintering temperatures. Raw materials were shaped under the pressure of 10 MPa and sintered at 1000~1350°C for 45 min with air flow rate of 2000 mL/min. The results showed that different sintering temperatures and different sintering times had little impact on the volatilization of arsenic, and the arsenic fixed rate remained above 90%; however, both factors greatly influenced the leaching concentration of arsenic. Considering the product’s environmental safety, the best sintering temperature was 1200°C and the best sintering time was 45 min. When sintering temperature was lower than 1000°C, FeAsS was oxidized into calcium, aluminum, and iron arsenide, mainly Ca3(AsO42 and AlAsO4, and the arsenic leaching was high. When it increased to 1200°C, arsenic was surrounded by a glass matrix and became chemically bonded inside the matrix, which lead to significantly lower arsenic leaching.

  3. Luminescent hybrid lanthanide sulfates and lanthanide sulfonate-carboxylates with 1,10-phenanthroline involving in-situ oxidation of 2-mercaptonbenzoic acid

    International Nuclear Information System (INIS)

    Zhong, Jie-Cen; Wan, Fang; Sun, Yan-Qiong; Chen, Yi-Ping

    2015-01-01

    A series of lanthanide sulfates and lanthanide sulfonate-carboxylates, [Ln 2 (phen) 2 (SO 4 ) 3 (H 2 O) 2 ] n (I:Ln=Nd(1a), Sm(1b), Eu(1c), phen=1,10-phenanthroline) and [Ln(phen)(2-SBA)(BZA)] n (II: Ln=Sm(2a), Eu(2b), Dy(2c), 2-SBA=2-sulfobenzoate, BZA=benzoate) have been hydrothermally synthesized from lanthanide oxide, 2-mercaptonbenzoic acid with phen as auxiliary ligand and characterized by single-crystal X-ray diffraction, elemental analyses, IR spectra, TG analyses and luminescence spectroscopy. Interestingly, SO 4 2− anions in I came from the in situ deep oxidation of thiol groups of 2-mercaptonbenzoic acid while 2-sulfobenzoate and benzoate ligands in II from the middle oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. Compounds I are organic–inorganic hybrid lanthanide sulfates, which have rare one-dimensional column-like structures. Complexes II are binuclear lanthanide sulfonate-carboxylates with 2-sulfobenzoate and benzoate as bridges and 1,10-phenanthroline as terminal. Photoluminescence studies reveal that complexes I and II exhibit strong lanthanide characteristic emission bands in the solid state at room temperature. - Graphical abstract: Lanthanide sulfates and lanthanide sulfonate-carboxylates have been hydrothermally synthesized. Interestingly, sulfate anions, 2-sulfobenzoate and benzoate ligands came from the in situ oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. - Highlights: • In situ oxidation and desulfuration reactions of 2-mercaptonbenzoic acid. • The organic–inorganic hybrid lanthanide sulfates with one-dimensional column-like structure. • The dinuclear lanthanide sulfonate-carboxylates. • The emission spectra exhibit the characteristic transition of 5 D 0 → 7 F J (J=0–4) of the Eu(III)

  4. Efficient oxidative dissolution of V2O3 by the in situ electro-generated reactive oxygen species on N-doped carbon felt electrodes

    International Nuclear Information System (INIS)

    Xue, Yudong; Wang, Yunting; Zheng, Shili; Sun, Zhi; Zhang, Yi; Jin, Wei

    2017-01-01

    Highlights: • Novel alkaline electro-Fenton-like was applied for V 2 O 3 oxidative dissolution. • N-doped carbon felt electrode was fabricated for the two-electron ORR. • ROS including ·OH and HO 2 − was in-situ generated from the electrochemical system. • A significant enhancement of V 2 O 3 dissolution was achieved due to the ROS. - Abstract: Oxidative dissolution is a critical step for the efficient remediation of heavy metal oxides in large-scale solid wastes. In the present study, a novel electro-oxidative dissolution process of V 2 O 3 to VO 4 3− is achieved by the in-situ generated reactive oxygen species on the N-doped carbon felt cathode in alkaline media. The electro-catalytic HO 2 − generation and hydrophilic behavior were significantly enhanced by the introduction of nitrogen-containing functional groups. Besides, the mechanism of electrochemical vanadium conversion is systematically illustrated, and a vanadium self-induced electro-Fenton-like reaction is proposed. By employing the radical quenching and ESR measurements, the contributions for V(III) dissolution is determined to be 43.5% by HO 2 − and 56.5% by hydroxyl radicals, respectively. It should be noted that the V 2 O 3 solid particles can be efficiently dissolved via adsorption-reaction scheme on the carbon felt electrode. This novel electrochemical strategy provides a promising solution for the heavy metal oxide treatment and further understanding for the in situ reactive oxygen species.

  5. In situ sonochemical reduction and direct functionalization of graphene oxide: A robust approach with thermal and biomedical applications.

    Science.gov (United States)

    Maktedar, Shrikant S; Mehetre, Shantilal S; Avashthi, Gopal; Singh, Man

    2017-01-01

    The rapid, robust, scalable and non-hazardous sonochemical approach for in situ reduction and direct functionalization of graphene oxide has been developed for non-toxic biomedical applications. The graphene oxide (GrO) was directly functionalized with tryptamine (TA) without using any hazardous acylating and coupling reagents. The reaction was completed within 20min. An impact of ultrasound was inferred for a direct functionalization with other conventional methods. The evolved electronic states were confirmed with near edge X-ray absorption fine structure (NEXAFS). The direct covalent functionalization and formation of f-(TA) GrO was proven with FTIR, 13 C solid state NMR, XPS, XRD, Raman' HRTEM, AFM and TGA. The total percentage weight loss in TGA confirms an enhanced thermal stability of f-(TA) GrO. The f-(TA) GrO was further explored for an investigation of in vitro antimicrobial activity to ensure the health and environmental safety. An outstanding antibacterial activity of f-(TA) GrO was found against gram positive Staphylococcus aureus at MIC 128mgmL -1 . It confirms a suitability of f-(TA) GrO for thermally stable antibacterial coating. The f-(TA) GrO showed 39.14-48.9% antioxidant activities, evaluated with 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radical assay. The inherent cytotoxicity of f-(TA) GrO was evaluated with SRB assay to living cells, MCF-7 and Vero. The estimated cell viabilities were >80% upon addition of f-(TA) GrO over a wide concentration range of 10-80μgmL -1 . The high cytocompatibility of f-(TA) GrO confirms the low toxicity and an excellent biocompatibility. The morphological effect on Vero cell line, evidently confirmed the biocompatibility of f-(TA) GrO. Therefore, f-(TA) GrO was emerged as an advanced functional biomaterial for thermal and biomedical applications. Copyright © 2016 Elsevier B.V. All rights reserved.

  6. Electromagnetic interference shielding effectiveness of microcellular polyimide/in situ thermally reduced graphene oxide/carbon nanotubes nanocomposites

    Science.gov (United States)

    Yang, Hongli; Yu, Zhi; Wu, Peng; Zou, Huawei; Liu, Pengbo

    2018-03-01

    A simple and effective method was adopted to fabricate microcellular polyimide (PI)/reduced graphene oxide (GO)/multi-walled carbon nanotubes (MWCNTs) nanocomposites. Firstly, microcellular poly (amic acid) (PAA)/GO/MWCNTs nanocomposites were prepared through solvent evaporation induced phase separation. In this process, PAA and dibutyl phthalate (DBP) co-dissolved in N,N-dimethylacetamide (DMAc) underwent phase separation with DMAc evaporating, and DBP microdomains were formed in continuous PAA phase. Subsequently, PAA was thermally imidized and simultaneously GO was in situ reduced. After DBP was removed, the microcellular PI/reduced GO (RGO)/MWCNTs nanocomposites were finally obtained. When the initial filler loading was 8 wt%, the electrical conductivity of microcellular PI/RGO, PI/MWCNTs and PI/RGO/MWCNTs nanocomposites were 0.05, 0.02 and 1.87 S·m-1, respectively, and the electromagnetic interference (EMI) shielding efficiency (SE) of microcellular PI/RGO, PI/MWCNTs and PI/RGO/MWCNTs nanocomposites were 13.7-15.1, 13.0-14.3 and 16.6-18.2 dB, respectively. The synergistic effect between RGO and MWCNTs enhanced both the electrical conductivity and EMI shielding performance of the microcellular PI/RGO/MWCNTs nanocomposites. The dominating EMI shielding mechanism for these materials was microwave absorption. While the initial loading of GO and MWCNT was 8 wt%, the microcellular PI/RGO/MWCNTs nanocomposite (500 μm thickness) had extremely high specific EMI SE value of 755-823 dB·cm2·g-1. Its thermal stability was also obviously improved, the 5% weight loss temperature in nitrogen was 548 °C. In addition, it also possessed a high Young's modulus of 789 MPa.

  7. Aluminum doped nickel oxide thin film with improved electrochromic performance from layered double hydroxides precursor in situ pyrolytic route

    International Nuclear Information System (INIS)

    Shi, Jingjing; Lai, Lincong; Zhang, Ping; Li, Hailong; Qin, Yumei; Gao, Yuanchunxue; Luo, Lei; Lu, Jun

    2016-01-01

    Electrochromic materials with unique performance arouse great interest on account of potential application values in smart window, low-power display, automobile anti-glare rearview mirror, and e-papers. In this paper, high-performing Al-doped NiO porous electrochromic film grown on ITO substrate has been prepared via a layered double hydroxides(LDHs) precursor in situ pyrolytic route. The Al 3+ ions distributed homogenously within the NiO matrix can significantly influence the crystallinity of Ni-Al LDH and NiO:Al 3+ films. The electrochromic performance of the films were evaluated by means of UV–vis absorption spectroscopy, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry(CA) measurements. In addition, the ratio of Ni 3+ /Ni 2+ also varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range (58.4%), fast switching speed (bleaching/coloration times are 1.8/4.2 s, respectively) and excellent durability (30% decrease after 2000 cycles). The improved performance was owed to the synergy of large NiO film specific surface area and porous morphology, as well as Al doping stifled the formation of Ni 3+ making bleached state more pure. This LDHs precursor pyrolytic method is simple, low-cost and environmental benign and is feasible for the preparation of NiO:Al and other Al-doped oxide thin film. - Graphical abstract: The ratio of Ni 3+ /Ni 2+ varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range, fast switching speed and excellent durability. Display Omitted

  8. "In-Situ Chemical Oxidation" - Sessions: #6 Technology Development, Process Fundamentals, Mechanisms;#7 Advantages and Disadvantages; #9 Oxidant Selection; #10 Bench- and Pilot-Scale Studies; #11 Monitoring; #12 Field-Scale Implementation; #13 Chemical Oxidation Regeneration of Granular Activated Carbon

    Science.gov (United States)

    A series of seven technical presentations involving chemical oxidation will be given to faculty, graduate students, and environmental professionals at the Chinese Academy of Sciences in Beijing, China (April 21-22, 2010). Chemical oxidation technologies include in-situ chemical o...

  9. Sintering process of Eu doped luminescent glass prepared from porous glass

    International Nuclear Information System (INIS)

    Akai, T; Murakami, M; Yamashita, M; Okajima, T; Umesaki, N

    2011-01-01

    Eu doped high silica glass prepared by sintering porous glass exhibits blue luminescence with high quantum efficiency. In this work, we studied effects of sintering temperature on valance state of europium ion. To investigate a change of valance state of Eu, X-ray absorption near edge structure (XANES) spectroscopy measurements were carried out. Intensity of blue emission at around 430nm drastically increases when the sintering temperature is above 1000 deg. C. From XANES spectra, it is found that almost all the Eu exist as Eu 3+ in a samples sintered below 900 deg. C, while more than 70% of Eu exist as Eu 2+ in the sample sintered at 1050 deg. C and 1100 deg. C. The drastic change of oxidation state of europium ion between 900 and 1050 deg. C is discussed in relation to the structural change probed by infrared (IR) spectroscopy.

  10. Superior sinterability of nano-crystalline gadolinium doped ceria powders synthesized by co-precipitation method

    International Nuclear Information System (INIS)

    Hari Prasad, D.; Kim, H.-R.; Park, J.-S.; Son, J.-W.; Kim, B.-K.; Lee, H.-W.; Lee, J.-H.

    2010-01-01

    Reduced sintering temperature of doped ceria can greatly simplify the fabrication process of solid oxide fuel cells (SOFCs) by utilizing the co-firing of all cell components with a single step. In the present study, nano-crystalline gadolinium doped ceria (GDC) powders of high sinterability at lower sintering temperature has been synthesized by co-precipitation at room temperature. The successful synthesis of nano-crystalline GDC was confirmed by XRD, TEM and Raman spectroscopy analysis. Dilatometry studies showed that GDC prepared by this method can be fully densified (97% relative density) at a sintering temperature of 950 o C which is fairly lower than ever before. It has also been found that the sintered samples have a higher ionic conductivity of 1.64 x 10 -2 S cm -1 at 600 o C which is suitable for the intermediate temperature SOFC application.

  11. Influence of spark plasma sintering conditions on the sintering and functional properties of an ultra-fine grained 316L stainless steel obtained from ball-milled powder

    Energy Technology Data Exchange (ETDEWEB)

    Keller, C., E-mail: clement.keller@insa-rouen.fr [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Tabalaiev, K.; Marnier, G. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Noudem, J. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France); Sauvage, X. [Groupe de Physique des Matériaux, CNRS-UMR 6634, Université de Rouen, INSA de Rouen, Avenue de l' Université, 76800 Saint-Etienne du Rouvray (France); Hug, E. [Laboratoire de Cristallographie des Matériaux, CNRS-UMR 6508, Université de Caen, ENSICAEN, 7 bd du Maréchal Juin, 14050 Caen (France)

    2016-05-17

    In this work, 316L samples with submicrometric grain size were sintered by spark plasma sintering. To this aim, 316L powder was first ball-milled with different conditions to obtain nanostructured powder. The process control agent quantity and milling time were varied to check their influence on the crystallite size of milled powder. Samples were then sintered by spark plasma sintering using different sets of sintering parameters (temperature, dwell time and pressure). For each sample, grain size and density were systematically measured in order to investigate the influence of the sintering process on these two key microstructure parameters. Results show that suitable ball-milling and subsequent sintering can be employed to obtain austenitic stainless steel samples with grain sizes in the nanometer range with porosity lower than 3%. However, ball-milling and subsequent sintering enhance chromium carbides formation at the sample surface in addition to intragranular and intergranular oxides in the sample as revealed by X-ray diffraction and transmission electron microscopy. It has been shown that using Boron nitride together with graphite foils to protect the mold from powder welding prevent such carbide formation. For mechanical properties, results show that the grain size refinement strongly increases the hardness of the samples without deviation from Hall-Petch relationship despite the oxides formation. For corrosion resistance, grain sizes lower than a few micrometers involve a strong decrease in the pitting potential and a strong increase in passivation current. As a consequence, spark plasma sintering can be considered as a promising tool for ultra-fine grained austenitic stainless steel.

  12. Understanding of catalysis on early transition metal oxide-based catalysts through exploration of surface structure and chemistry during catalysis using in-situ approaches

    Energy Technology Data Exchange (ETDEWEB)

    Tao, Franklin [Univ. of Kansas, Lawrence, KS (United States). Dept. of Chemical and Petroleum Engineering. Dept. of Chemistry

    2015-09-14

    Two main categories of heterogeneous catalysts are metal and metal oxide which catalyze 80% chemical reactions at solid-gas and solid-liquid interfaces. Metal oxide catalysts are much more complicated than metal catalysts. The reason is that the cations of the metal atoms could exhibit a few different oxidation states on surface of the same catalyst particle such as Co3O4 or change of their oxidation states under different reactive environments. For a metal catalyst, there is only one oxidation state typically. In addition, surface of a metal oxide can be terminated with multiple surface functionalities including O atoms with different binding configurations and OH group. For metal, only metal atoms are exposed typically. Obviously, the complication of surface chemistry and structure of a metal oxide makes studies of surface of an oxide catalyst very challenging. Due to the complication of surface of a meal oxide, the electronic and geometric structures of surface of a metal oxide and the exposed species have received enormous attention since oxide catalysts catalyze at least 1/3 chemical reactions in chemical and energy industries. Understanding of catalytic reactions on early transition metal oxide-based catalysts is fundamentally intriguing and of great practical interest in energy- and environment-related catalysis. Exploration of surface chemistry of oxide-based catalysts at molecular level during catalysis has remained challenging though it is critical in deeply understanding catalysis on oxide-based catalysts and developing oxide-based catalysts with high activity and selectivity. Thus, the overall objective of this project is to explore surface chemistry and structure of early transition metal oxide-based catalysts through in-situ characterization of surface of catalysts, measurements of catalytic performances, and then build an intrinsic correlation of surface chemistry and structure with their catalytic performances in a few

  13. Development of a Sinter/HIP process for the superalloy Udimet 700 with investigations of the influence of the sinteratmosphere

    International Nuclear Information System (INIS)

    Wenning, L.

    1991-03-01

    The oxidation free treatment of reactive metalpowders like the nickel base alloy Udimet 700 demands sufficient oxygen free sinteratmospheres in nowadays sinter-HIP plants are not reachable. The reported work deals with the development of a sinter-HIP process which enables a sufficient low partial pressure of oxygen by scavenging the Udimet 700 powder packings with argon during vacuum sintering. By this the sinter hindering oxidation is avoided. Intensive investigations of the sinteratmosphere with a mass spectrometer and a zirconium oxide probe verify the reduction of the oxygen content of the residual gas atmosphere reached with different processes. In a second part the applicability of the scavenging gas process during the capsule free sinter-HIP treatment of metall injection moulded (MIM) samples is shown. (orig.) [de

  14. In situ Fourier transform infrared spectroscopy and on-line differential electrochemical mass spectrometry study of the NH3BH3 oxidation reaction on gold electrodes

    International Nuclear Information System (INIS)

    Belén Molina Concha, M.; Chatenet, Marian; Lima, Fabio H.B.; Ticianelli, Edson A.

    2013-01-01

    The ammonia borane (NH 3 BH 3 ) oxidation reaction (ABOR) was studied on gold electrodes using the rotating disk electrode (RDE) setup and coupled physical techniques: on-line differential electrochemical mass spectrometry (DEMS) and in situ Fourier transform infrared spectroscopy (FTIR). Non-negligible heterogeneous hydrolysis in the low-potential region was asserted via molecular H 2 detection. As a consequence, the number of electron exchanged per BH 3 OH − species is ca. 3 at low potential, and only reaches ca. 6 above 0.6 V vs. RHE. These figures were confirmed by Levich and Koutecki–Levich calculations using the RDE experiments data. The nature of the ABOR intermediates and products was determined using in situ FTIR. While BH 2 species were detected during the ABOR, it seems that its adsorption onto the Au electrode proceeds via the O atom, in opposition to what happens during the borohydride oxidation reaction (BOR). Therefore, it is likely that the mechanism of the ABOR differs from that of the BOR. From the whole set of data (RDE, DEMS, FTIR), a relevant reaction pathway was proposed, including competition between the BH 3 OH − heterogeneous hydrolysis and oxidation at low potential, and preponderant oxidation at higher potential. Finally, a simplified kinetic modeling accounting with this reaction pathway was proposed, which nicely fits the stationary (i vs. E) ABOR plot

  15. Designing a miniaturised heated stage for in situ optical measurements of solid oxide fuel cell electrode surfaces, and probing the oxidation of solid oxide fuel cell anodes using in situ Raman spectroscopy

    KAUST Repository

    Brightman, E.; Maher, R.; Offer, G. J.; Duboviks, V.; Heck, C.; Cohen, L. F.; Brandon, N. P.

    2012-01-01

    A novel miniaturised heated stage for in operando optical measurements on solid oxide fuel cell electrode surfaces is described. The design combines the advantages of previously reported designs, namely, (i) fully controllable dual atmosphere operation enabling fuel cell pellets to be tested in operando with either electrode in any atmosphere being the focus of study, and (ii) combined electrochemical measurements with optical spectroscopy measurements with the potential for highly detailed study of electrochemical processes; with the following advances, (iii) integrated fitting for mounting on a mapping stage enabling 2-D spatial characterisation of the surface, (iv) a compact profile that is externally cooled, enabling operation on an existing microscope without the need for specialized lenses, (v) the ability to cool very rapidly, from 600 °C to 300 °C in less than 5 min without damaging the experimental apparatus, and (vi) the ability to accommodate a range of pellet sizes and thicknesses. © 2012 American Institute of Physics.

  16. Mechanical characterization of microwave sintered zinc oxide

    Indian Academy of Sciences (India)

    Unknown

    ultrasonic time of flight measurement using a 15 MHz transducer. .... Figure 1. Microwave heating system (a. thermocouple, b. porous refractory box, c. sample, d. fibrous insulation material, e. power control, f. timer and g. display panel). a b c d.

  17. Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

    Science.gov (United States)

    Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

    2014-01-01

    Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

  18. Development of a 16S rRNA-targeted fluorescence in situ hybridization probe for quantification of the ammonia-oxidizer Nitrosotalea devanaterra and its relatives.

    Science.gov (United States)

    Restrepo-Ortiz, C X; Merbt, S N; Barrero-Canossa, J; Fuchs, B M; Casamayor, E O

    2018-04-28

    The Thaumarchaeota SAGMCG-1 group and, in particular, members of the genus Nitrosotalea have high occurrence in acidic soils, the rhizosphere, groundwater and oligotrophic lakes, and play a potential role in nitrogen cycling. In this study, the specific oligonucleotide fluorescence in situ hybridization probe SAG357 was designed for this Thaumarchaeota group based on the available 16S rRNA gene sequences in databases, and included the ammonia-oxidizing species Nitrosotalea devanaterra. Cell permeabilization for catalyzed reporter deposition fluorescence in situ detection and the hybridization conditions were optimized on enrichment cultures of the target species N. devanaterra, as well as the non-target ammonia-oxidizing archaeon Nitrosopumilus maritimus. Probe specificity was improved with a competitor oligonucleotide, and fluorescence intensity and cell visualization were enhanced by the design and application of two adjacent helpers. Probe performance was tested in soil samples along a pH gradient, and counting results matched the expected in situ distributions. Probe SAG357 and the CARD-FISH protocol developed in the present study will help to improve the current understanding of the ecology and physiology of N. devanaterra and its relatives in natural environments. Copyright © 2018 Elsevier GmbH. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2004-01-01

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

  20. Liquid phase sintered SiC. Processing and transformation controlled microstructure tailoring

    Directory of Open Access Journals (Sweden)

    V.A. Izhevskyi

    2000-10-01

    Full Text Available Microstructure development and phase formation processes during sintering of silicon carbide based materials with AlN-Y2O3, AlN-Yb2O3, and AlN-La2O3 sintering additives were investigated. Densification of the materials occurred by liquid-phase sintering mechanism. Proportion of alpha- and beta-SiC powders in the initial mixtures was a variable parameter, while the molar ratio of AlN/RE2O3, and the total amount of additives (10 vol. % were kept constant. Shrinkage behavior during sintering in interrelation with the starting composition of the material and the sintering atmosphere was investigated by high temperature dilatometry. Kinetics of b-SiC to a-SiC phase transformation during post-sintering heat treatment at temperatures 1900-1950 °C was studied, the degree of phase transformation being determined by quantitative x-ray analysis using internal standard technique. Evolution of microstructure resulting from beta-SiC to alpha-SiC transformation was followed up by scanning electron microscopy on polished and chemically etched samples. Transformation-controlled grain growth mechanism similar to the one observed for silicon nitride based ceramics was established. Possibility of in-situ platelet reinforced dense SiC-based ceramics fabrication with improved mechanical properties by means of sintering was shown.

  1. Sintering of micro-trusses created by extrusion-3D-printing of lunar regolith inks

    Science.gov (United States)

    Taylor, Shannon L.; Jakus, Adam E.; Koube, Katie D.; Ibeh, Amaka J.; Geisendorfer, Nicholas R.; Shah, Ramille N.; Dunand, David C.

    2018-02-01

    The development of in situ fabrication methods for the infrastructure required to support human life on the Moon is necessary due to the prohibitive cost of transporting large quantities of materials from the Earth. Cellular structures, consisting of a regular network (truss) of micro-struts with ∼500 μm diameters, suitable for bricks, blocks, panels, and other load-bearing structural elements for habitats and other infrastructure are created by direct-extrusion 3D-printing of liquid inks containing JSC-1A lunar regolith simulant powders, followed by sintering. The effects of sintering time, temperature, and atmosphere (air or hydrogen) on the microstructures, mechanical properties, and magnetic properties of the sintered lunar regolith micro-trusses are investigated. The air-sintered micro-trusses have higher relative densities, linear shrinkages, and peak compressive strengths, due to the improved sintering of the struts within the micro-trusses achieved by a liquid or glassy phase. Whereas the hydrogen-sintered micro-trusses show no liquid-phase sintering or glassy phase, they contain metallic iron 0.1-2 μm particles from the reduction of ilmenite, which allows them to be lifted with magnets.

  2. Sintering diagrams of UO2

    International Nuclear Information System (INIS)

    Mohan, A.; Soni, N.C.; Moorthy, V.K.

    1979-01-01

    Ashby's method (see Acta Met., vol. 22, p. 275, 1974) of constructing sintering diagrams has been modified to obtain contribution diagrams directly from the computer. The interplay of sintering variables and mechanisms are studied and the factors that affect the participation of mechanisms in UO 2 are determined. By studying the physical properties, it emerges that the order of inaccuracies is small in most cases and do not affect the diagrams. On the other hand, even a 10% error in activation energies, which is quite plausible, would make a significant difference to the diagram. The main criticism of Ashby's approach is that the numerous properties and equations used, communicate their inaccuracies to the diagrams and make them unreliable. The present study has considerably reduced the number of factors that need to be refined to make the sintering diagrams more meaningful. (Auth.)

  3. Effect of sintering atmosphere on the hardness of ThO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Baena, Angela; Cardinaels, Thomas [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium); KU Leuven, Department of Chemistry, Celestijnenlaan 200F, P.O. Box 2404, B-3001, Heverlee (Belgium); Van Eyken, Jelle; Puzzolante, Jean Louis [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium); Binnemans, Koen [KU Leuven, Department of Chemistry, Celestijnenlaan 200F, P.O. Box 2404, B-3001, Heverlee (Belgium); Verwerft, Marc, E-mail: marc.verwerft@sckcen.be [Belgian Nuclear Research Centre (SCK-CEN), Institute for Nuclear Materials Science, Fuel Materials Group, Boeretang 200, B-2400, Mol (Belgium)

    2016-08-15

    The hardness and toughness of ThO{sub 2} sintered under reducing and oxidizing conditions has been investigated and, quite unexpectedly, a significant difference in hardness was observed for the entire range of porosities studied. Reducing conditions systematically yielded higher hardness values than oxidizing conditions. Extrapolated to zero porosity, the hardness for ThO{sub 2} is H{sub 0} = 10.5 ± 0.3 GPa for oxidizing conditions and H{sub 0} = 12.4 ± 0.7 GPa for reducing conditions. Toughness values have been derived from Vickers indentations; differences in toughness were insignificant and only a single value is proposed: K{sub IC} = 0.97 ± 0.12 MPa √m. The difference in hardness is attributed to the presence of point defects, also acting as color centers and causing grey coloration of ThO{sub 2} sintered under reducing conditions. Furthermore, and of interest for nuclear fuel production, is the finding that ThO{sub 2} sintered under reducing conditions is significantly easier to grind compared to material sintered under oxidizing conditions. - Highlights: • Reducing sintering conditions increase the hardness of polycrystalline ThO{sub 2}. • Systematic series of hardness versus porosity of ThO{sub 2} were obtained. • Reducing sintering conditions improve grinding of ThO{sub 2}.

  4. Effect of sintering atmosphere on the hardness of ThO_2

    International Nuclear Information System (INIS)

    Baena, Angela; Cardinaels, Thomas; Van Eyken, Jelle; Puzzolante, Jean Louis; Binnemans, Koen; Verwerft, Marc

    2016-01-01

    The hardness and toughness of ThO_2 sintered under reducing and oxidizing conditions has been investigated and, quite unexpectedly, a significant difference in hardness was observed for the entire range of porosities studied. Reducing conditions systematically yielded higher hardness values than oxidizing conditions. Extrapolated to zero porosity, the hardness for ThO_2 is H_0 = 10.5 ± 0.3 GPa for oxidizing conditions and H_0 = 12.4 ± 0.7 GPa for reducing conditions. Toughness values have been derived from Vickers indentations; differences in toughness were insignificant and only a single value is proposed: K_I_C = 0.97 ± 0.12 MPa √m. The difference in hardness is attributed to the presence of point defects, also acting as color centers and causing grey coloration of ThO_2 sintered under reducing conditions. Furthermore, and of interest for nuclear fuel production, is the finding that ThO_2 sintered under reducing conditions is significantly easier to grind compared to material sintered under oxidizing conditions. - Highlights: • Reducing sintering conditions increase the hardness of polycrystalline ThO_2. • Systematic series of hardness versus porosity of ThO_2 were obtained. • Reducing sintering conditions improve grinding of ThO_2.

  5. Phosphorus containing sintered alloys (review)

    International Nuclear Information System (INIS)

    Muchnik, S.V.

    1984-01-01

    Phosphorus additives are considered for their effect on the properties of sintered alloys of different applications: structural, antifriction, friction, magnetic, hard, superhard, heavy etc. Data are presented on compositions and properties of phosphorus-containing materials produced by the powder metallurgy method. Phosphorus is shown to be an effective activator of sintering in some cases. When its concentration in the material is optimal it imparts the material such properties as strength, viscosity, hardness, wear resistance. Problems concerning powder metallurgy of amorphous phosphorus-containing alloys are reported

  6. Kinetics of sintering of uranium dioxide

    International Nuclear Information System (INIS)

    Soni, N.C.; Moorthy, V.K.

    1978-01-01

    The kinetics of sintering of UO 2 powders derived from ADU route and calcined at different temperatures was studied. The activation energy for sintering was found to depend on the calcination temperature, the density chosen and the sintering temperature range. The motive force for sintering is the excess free energy in the particle system. This exists in the powder compact in the form of surface energy and the excess lattice energy due to defects. The defects which can be eliminated at the operating temperature are responsible for the mobility and hence sintering. This concept of the motive force for sintering has been used to explain the difference in the activation energies observed in the present study. This would also explain phenomena such as attainment of limiting density, presence of optimum sintering temperature and the influence of calcination treatments on the sintering behaviour of powders. (author)

  7. Effect of the sintering temperature and time on phase assemblage and electrical conductivity of zirconia-scandia-ceria

    International Nuclear Information System (INIS)

    Grosso, R.L.; Muccillo, E.N.S.

    2012-01-01

    ZrO 2 -based solid electrolytes have been extensively studied over the last decades for application in solid oxide fuel cells (SOFCs). Zirconia containing scandia and ceria solid electrolyte is a potential candidate in SOFCs operating at intermediate temperatures (600 - 800 deg C). In this work, commercial ZrO 2 containing 10 mol% Sc 2 O 3 and 1 mol% CeO 2 was sintered by the conventional and two-step methods. Several sintering conditions were evaluated by varying the temperature as well as the residence time. High values of sintered density (> 98%) were obtained. A careful selection of the sintering conditions is necessary in order to obtain a single cubic phase, as revealed by X-ray diffraction results. The grain growth can be controlled in specimens sintered by the two-step method. The electrical conductivity show similar behavior for the grain component independent on the sintering method. (author)

  8. Performance optimization of AlGaN-based LEDs by use of ultraviolet-transparent indium tin oxide: Effect of in situ contact treatment

    Science.gov (United States)

    Tu, Wenbin; Chen, Zimin; Zhuo, Yi; Li, Zeqi; Ma, Xuejin; Wang, Gang

    2018-05-01

    Ultraviolet (UV)-transparent indium tin oxide (ITO) grown by metal–organic chemical vapor deposition (MOCVD) is used as the current-spreading layer for 368 nm AlGaN-based light-emitting diodes (LEDs). By performing in situ contact treatment on the LED/ITO interface, the morphology, resistivity, and contact resistance of electrodes become controllable. Resistivity of 2.64 × 10‑4 Ω cm and transmittance at 368 nm of 95.9% are realized for an ITO thin film grown with Sn-purge in situ treatment. Therefore, the high-power operating voltage decreases from 3.94 V (without treatment) to 3.83 V (with treatment). The improved performance is attributed to the lowering of the tunneling barrier at the LED/ITO interface.

  9. Aluminum doped nickel oxide thin film with improved electrochromic performance from layered double hydroxides precursor in situ pyrolytic route

    Energy Technology Data Exchange (ETDEWEB)

    Shi, Jingjing; Lai, Lincong; Zhang, Ping; Li, Hailong; Qin, Yumei; Gao, Yuanchunxue; Luo, Lei; Lu, Jun, E-mail: lujun@mail.buct.edu.cn

    2016-09-15

    Electrochromic materials with unique performance arouse great interest on account of potential application values in smart window, low-power display, automobile anti-glare rearview mirror, and e-papers. In this paper, high-performing Al-doped NiO porous electrochromic film grown on ITO substrate has been prepared via a layered double hydroxides(LDHs) precursor in situ pyrolytic route. The Al{sup 3+} ions distributed homogenously within the NiO matrix can significantly influence the crystallinity of Ni-Al LDH and NiO:Al{sup 3+} films. The electrochromic performance of the films were evaluated by means of UV–vis absorption spectroscopy, cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS), and chronoamperometry(CA) measurements. In addition, the ratio of Ni{sup 3+}/Ni{sup 2+} also varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range (58.4%), fast switching speed (bleaching/coloration times are 1.8/4.2 s, respectively) and excellent durability (30% decrease after 2000 cycles). The improved performance was owed to the synergy of large NiO film specific surface area and porous morphology, as well as Al doping stifled the formation of Ni{sup 3+} making bleached state more pure. This LDHs precursor pyrolytic method is simple, low-cost and environmental benign and is feasible for the preparation of NiO:Al and other Al-doped oxide thin film. - Graphical abstract: The ratio of Ni{sup 3+}/Ni{sup 2+} varies with Al content which can lead to different electrochemical performances. Among the as-prepared films, NiO film prepared from Ni-Al (19:1) LDH show the best electrochromic performance with a high transparency of 96%, large optical modulation range, fast switching speed and excellent durability. Display Omitted.

  10. Sintering of nanoscale silver coated textiles, a new approach to attain conductive fabrics for electromagnetic shielding

    Energy Technology Data Exchange (ETDEWEB)

    Kardarian, Kasra [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Busani, Tito [CENIMAT/I3N, Departamento de Ciência dos Materiais, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Osório, Inês [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Domingos, Helena; Igreja, Rui [CENIMAT/I3N, Departamento de Ciência dos Materiais, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Franco, Ricardo [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Cortez, João, E-mail: j.cortez@fct.unl.pt [REQUIMTE, Departamento de Química, Faculdade de Ciências e Tecnologia, Universidade Nova de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal)

    2014-10-15

    The demand for conductive textiles is increasing, owing to the need for lightweight and flexible conductive materials for a variety of applications, including electromagnetic shielding of electronic equipment. Herein we propose a process that combines the in situ synthesis of silver nanoparticles at the textile fibre surface followed by sintering of the nanoparticles to obtain highly conductive fabrics. The formation of silver particles at the nanoscale allowed for sintering to be performed efficiently, at reduced temperature and time, bestowing fabrics with high conductivity and capability of shielding electromagnetic radiation. The nanoparticle synthesis method entailed the precipitation of 2.0 g L{sup −1} silver nitrate and further reduction with citrate, with the formation of a deposit of silver nanoparticles at the fabric surface. The amount of silver deposited (up to 195 mg of silver per g of fabric) resulted in moderate electrical conductivity with sheet resistance of 803 Ω/sq. Upon sintering, this value decreased dramatically to 5.2 Ω/sq. The sintering process was monitored by SEM, which showed that sintering at 200 °C for 30 min resulted in maximal electrical conductivity with the lowest amount of silver deposited, while forming a homogenous surface. Fabrics submitted to these sintering conditions maintained their sheet resistance and shielding effectiveness values, even after eight washing cycles. - Highlights: • Assembly of highly conductive textiles capable of shielding electromagnetic radiation. • Procedure combines in situ synthesis of AgNPs at the textile surface and sintering. • AgNPs formed by precipitation of AgNO{sub 3} and reduction with citrate, as observed by SEM. • Sintering increased dramatically conductivity and shielding effectiveness. • Treated fabrics maintained conductivity and shielding effectiveness after 8 washes.

  11. Sintering of nanoscale silver coated textiles, a new approach to attain conductive fabrics for electromagnetic shielding

    International Nuclear Information System (INIS)

    Kardarian, Kasra; Busani, Tito; Osório, Inês; Domingos, Helena; Igreja, Rui; Franco, Ricardo; Cortez, João

    2014-01-01

    The demand for conductive textiles is increasing, owing to the need for lightweight and flexible conductive materials for a variety of applications, including electromagnetic shielding of electronic equipment. Herein we propose a process that combines the in situ synthesis of silver nanoparticles at the textile fibre surface followed by sintering of the nanoparticles to obtain highly conductive fabrics. The formation of silver particles at the nanoscale allowed for sintering to be performed efficiently, at reduced temperature and time, bestowing fabrics with high conductivity and capability of shielding electromagnetic radiation. The nanoparticle synthesis method entailed the precipitation of 2.0 g L −1 silver nitrate and further reduction with citrate, with the formation of a deposit of silver nanoparticles at the fabric surface. The amount of silver deposited (up to 195 mg of silver per g of fabric) resulted in moderate electrical conductivity with sheet resistance of 803 Ω/sq. Upon sintering, this value decreased dramatically to 5.2 Ω/sq. The sintering process was monitored by SEM, which showed that sintering at 200 °C for 30 min resulted in maximal electrical conductivity with the lowest amount of silver deposited, while forming a homogenous surface. Fabrics submitted to these sintering conditions maintained their sheet resistance and shielding effectiveness values, even after eight washing cycles. - Highlights: • Assembly of highly conductive textiles capable of shielding electromagnetic radiation. • Procedure combines in situ synthesis of AgNPs at the textile surface and sintering. • AgNPs formed by precipitation of AgNO 3 and reduction with citrate, as observed by SEM. • Sintering increased dramatically conductivity and shielding effectiveness. • Treated fabrics maintained conductivity and shielding effectiveness after 8 washes

  12. Influences of chemical packing and the chemical composition in porcelain sintering: from theory to practice

    International Nuclear Information System (INIS)

    Conceicao, E.S.; Gouvea, D.; Romano, R.C.O.; Pileggi, R.G.

    2011-01-01

    Studies have been conducted using the size distribution particles as a tool to obtain maximum packing in porcelain bodies. However, little attention has been given for the maximum size of particles and its effect in the sintering. While some particles are relatively large (63 μ m) for some oxides in the porcelain composition, they could compromise the sintering if a liquid phase is formed during heat processing. In this work, a comparative analysis showed that compositions with a maximum green packing density does not always lead to a maximum final densification in sintering if there is no control of the maximum size of the particles. (author)

  13. Ratiometric two-photon excited photoluminescence of quantum dots triggered by near-infrared-light for real-time detection of nitric oxide release in situ

    International Nuclear Information System (INIS)

    Jin, Hui; Gui, Rijun; Sun, Jie; Wang, Yanfeng

    2016-01-01

    Probe-donor integrated nanocomposites were developed from conjugating silica-coated Mn"2"+:ZnS quantum dots (QDs) with MoS_2 QDs and photosensitive nitric oxide (NO) donors (Fe_4S_3(NO)_7"−, RBS). Under excitation with near-infrared (NIR) light at 808 nm, the Mn"2"+:ZnS@SiO_2/MoS_2-RBS nanocomposites showed the dual-emissive two-photon excited photoluminescence (TPEPL) that induced RBS photolysis to release NO in situ. NO caused TPEPL quenching of Mn"2"+:ZnS QDs, but it produced almost no impact on the TPEPL of MoS_2 QDs. Hence, the nanocomposites were developed as a novel QDs-based ratiometric TPEPL probe for real-time detection of NO release in situ. The ratiometric TPEPL intensity is nearly linear (R"2 = 0.9901) with NO concentration in the range of 0.01∼0.8 μM, which corresponds to the range of NO release time (0∼15 min). The detection limit was calculated to be approximately 4 nM of NO. Experimental results confirmed that this novel ratiometric TPEPL probe possessed high selectivity and sensitivity for the detection of NO against potential competitors, and especially showed high detection performance for NIR-light triggered NO release in tumor intracellular microenvironments. These results would promote the development of versatile probe-donor integrated systems, also providing a facile and efficient strategy to real-time detect the highly controllable drug release in situ, especially in physiological microenvironments. - Highlights: • Mn"2"+:ZnS@SiO_2/MoS_2-RBS nanocomposites were developed as a novel ratiometric two-photon excited fluorescence probe. • This probe could conduct real-time detection of nitric oxide release in situ. • High feasibility of this probe was confirmed in tumor intracellular microenvironments.

  14. In situ Ni-doping during cathodic electrodeposition of hematite for excellent photoelectrochemical performance of nanostructured nickel oxide-hematite p-n junction photoanode

    Science.gov (United States)

    Phuan, Yi Wen; Ibrahim, Elyas; Chong, Meng Nan; Zhu, Tao; Lee, Byeong-Kyu; Ocon, Joey D.; Chan, Eng Seng

    2017-01-01

    Nanostructured nickel oxide-hematite (NiO/α-Fe2O3) p-n junction photoanodes synthesized from in situ doping of nickel (Ni) during cathodic electrodeposition of hematite were successfully demonstrated. A postulation model was proposed to explain the fundamental mechanism of Ni2+ ions involved, and the eventual formation of NiO on the subsurface region of hematite that enhanced the potential photoelectrochemical water oxidation process. Through this study, it was found that the measured photocurrent densities of the Ni-doped hematite photoanodes were highly dependent on the concentrations of Ni dopant used. The optimum Ni dopant at 25 M% demonstrated an excellent photoelectrochemical performance of 7-folds enhancement as compared to bare hematite photoanode. This was attributed to the increased electron donor density through the p-n junction and thus lowering the energetic barrier for water oxidation activity at the optimum Ni dopant concentration. Concurrently, the in situ Ni-doping of hematite has also lowered the photogenerated charge carrier transfer resistance as measured using the electrochemical impedance spectroscopy. It is expected that the fundamental understanding gained through this study is helpful for the rational design and construction of highly efficient photoanodes for application in photoelectrochemical process.

  15. Effects of pressure and temperature on sintering of Cr-doped Al2O3 by pulsed electric current sintering process

    Science.gov (United States)

    Dang, K. Q.; Nanko, M.

    2011-03-01

    The aluminium oxide crystal, Al2O3, which contains a small amount of chromium, Cr, is called ruby. Pulsed electric current sintering (PECS) was applied to sinter ruby polycrystals. Cr2O3-Al2O3 powder mixture prepared by drying an aqueous slurry containing amounts of Al2O3 and Cr(NO3)3 was consolidated by PECS process. The PECS process was performed in vacuum at sintering temperature raging from 1100 to 1300°C with heating rate of 2 K/min under applied uniaxial pressure varied from 40 to 100 MPa. This study found that highly densified and transparent Cr-doped Al2O3 can be obtained by the PECS process with the high applied pressure at sintering temperature of 1200°C.

  16. A study on sintering aids for Sm{sub 0.2}Ce{sub 0.8}O{sub 1.9} electrolyte

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xinge; Deces-Petit, Cyrille; Yick, Sing; Robertson, Mark; Kesler, Olivera; Maric, Radenka; Ghosh, Dave [Institute for Fuel Cell Innovation, National Research Council Canada, 3250 East Mall, Vancouver, BC (Canada V6T 1W5)

    2006-11-08

    In this study, an addition of Co oxide or Cu oxide to Sm{sub 0.2}Ce{sub 0.8}O{sub 1.9} (SDC) was studied to improve the sinterability of SDC. It has been found that both Co and Cu oxide are very effective as sintering aids, and the SDC sintering temperature can be reduced from 1400{sup o}C without aids to below 1000{sup o}C with only 1at.% of either Cu oxide or Co oxide. As compared to the pure SDC, a slight decrease of ionic conductivity was observed in SDC with Cu sintering aid. There is no obvious effect on electrochemical property of SDC with Co sintering aid under 2.5at.%. (author)

  17. Technological parameter effect on properties of sintered hard-magnetic type Nd-Fe-B materials

    International Nuclear Information System (INIS)

    Rastegaev, V.S.; Stepanova, G.I.; Gudim, Z.Yu.

    1989-01-01

    The effect of each technological operation on manufacturing hard magnets from Nd-Fe-B alloys on properties of sintered permanent magnets is studied. It is noted that violation of the metting regime can result in burn-up of boron and rare earths, and violation of the grinding mode-formation of nonmagnetic powder fractions, etc. Special attention is paid to material protection against oxidation by introducing passivating additions and creating of particular conditions for alloy sintering and heat treatment

  18. On the Mechanism of Microwave Flash Sintering of Ceramics

    Directory of Open Access Journals (Sweden)

    Yury V. Bykov

    2016-08-01

    Full Text Available The results of a study of ultra-rapid (flash sintering of oxide ceramic materials under microwave heating with high absorbed power per unit volume of material (10–500 W/cm3 are presented. Ceramic samples of various compositions—Al2O3; Y2O3; MgAl2O4; and Yb(LaO2O3—were sintered using a 24 GHz gyrotron system to a density above 0.98–0.99 of the theoretical value in 0.5–5 min without isothermal hold. An analysis of the experimental data (microwave power; heating and cooling rates along with microstructure characterization provided an insight into the mechanism of flash sintering. Flash sintering occurs when the processing conditions—including the temperature of the sample; the properties of thermal insulation; and the intensity of microwave radiation—facilitate the development of thermal runaway due to an Arrhenius-type dependency of the material’s effective conductivity on temperature. The proper control over the thermal runaway effect is provided by fast regulation of the microwave power. The elevated concentration of defects and impurities in the boundary regions of the grains leads to localized preferential absorption of microwave radiation and results in grain boundary softening/pre-melting. The rapid densification of the granular medium with a reduced viscosity of the grain boundary phase occurs via rotation and sliding of the grains which accommodate their shape due to fast diffusion mass transport through the (quasi-liquid phase. The same mechanism based on a thermal runaway under volumetric heating can be relevant for the effect of flash sintering of various oxide ceramics under a dc/ac voltage applied to the sample.

  19. In situ characterization of nanoscale catalysts during anodic redox processes

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Renu [National Institute of Standards and Technology; Crozier, Peter [Arizona State University; Adams, James [Arizona State University

    2013-09-19

    Controlling the structure and composition of the anode is critical to achieving high efficiency and good long-term performance. In addition to being a mixed electronic and ionic conductor, the ideal anode material should act as an efficient catalyst for oxidizing hydrogen, carbon monoxide and dry hydrocarbons without de-activating through either sintering or coking. It is also important to develop novel anode materials that can operate at lower temperatures to reduce costs and minimized materials failure associated with high temperature cycling. We proposed to synthesize and characterize novel anode cermets materials based on ceria doped with Pr and/or Gd together with either a Ni or Cu metallic components. Ceria is a good oxidation catalyst and is an ionic conductor at room temperature. Doping it with trivalent rare earths such as Pr or Gd retards sintering and makes it a mixed ion conductor (ionic and electronic). We have developed a fundamental scientific understanding of the behavior of the cermet material under reaction conditions by following the catalytic oxidation process at the atomic scale using a powerful Environmental Scanning Transmission Electron Microscope (ESTEM). The ESTEM allowed in situ monitoring of structural, chemical and morphological changes occurring at the cermet under conditions approximating that of typical fuel-cell operation. Density functional calculations were employed to determine the underlying mechanisms and reaction pathways during anode oxidation reactions. The dynamic behavior of nanoscale catalytic oxidation of hydrogen and methane were used to determine: ? Fundamental processes during anodic reactions in hydrogen and carbonaceous atmospheres ? Interfacial effects between metal particles and doped ceria ? Kinetics of redox reaction in the anode material

  20. Master Sintering Surface: A practical approach to its construction and utilization for Spark Plasma Sintering prediction

    Directory of Open Access Journals (Sweden)

    Pouchly V.

    2012-01-01

    Full Text Available The sintering is a complex thermally activated process, thus any prediction of sintering behaviour is very welcome not only for industrial purposes. Presented paper shows the possibility of densification prediction based on concept of Master Sintering Surface (MSS for pressure assisted Spark Plasma Sintering (SPS. User friendly software for evaluation of the MSS is presented. The concept was used for densification prediction of alumina ceramics sintered by SPS.

  1. In situ Ni-doping during cathodic electrodeposition of hematite for excellent photoelectrochemical performance of nanostructured nickel oxide-hematite p-n junction photoanode

    Energy Technology Data Exchange (ETDEWEB)

    Phuan, Yi Wen, E-mail: phuan.yi.wen@monash.edu [School of Engineering, Chemical Engineering Discipline, Monash University Malaysia, Jalan Lagoon Selatan, Bandar Sunway, Selangor DE 47500 (Malaysia); Ibrahim, Elyas, E-mail: meibr2@student.monash.edu [School of Engineering, Chemical Engineering Discipline, Monash University Malaysia, Jalan Lagoon Selatan, Bandar Sunway, Selangor DE 47500 (Malaysia); Chong, Meng Nan, E-mail: Chong.Meng.Nan@monash.edu [School of Engineering, Chemical Engineering Discipline, Monash University Malaysia, Jalan Lagoon Selatan, Bandar Sunway, Selangor DE 47500 (Malaysia); Sustainable Water Alliance, Advanced Engineering Platform, Monash University Malaysia, Jalan Lagoon Selatan, Bandar Sunway, Selangor DE 47500 (Malaysia); Zhu, Tao, E-mail: zhu.tao@monash.edu [School of Engineering, Chemical Engineering Discipline, Monash University Malaysia, Jalan Lagoon Selatan, Bandar Sunway, Selangor DE 47500 (Malaysia); Lee, Byeong-Kyu, E-mail: bklee@ulsan.ac.kr [Department of Civil and Environmental Engineering, University of Ulsan, Nam-gu, Daehakro 93, Ulsan 680-749 (Korea, Republic of); Ocon, Joey D., E-mail: jdoco