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Sample records for in-situ high temperature

  1. In situ high-temperature visible microspectroscopy for volcanic materials.

    PubMed

    Yamanoi, Yuta; Nakashima, Satoru

    2005-11-01

    In situ high-temperature visible microspectroscopy has been developed in order to study color change kinetics of volcanic materials. Olivine thin sections put on a synthetic alumina plate are heated on a heating stage at 600-800 degrees C under a visible microspectroscope. Changes in visible absorption spectra are monitored every 60 s for 5 hours. The obtained high-temperature visible spectra showed a gradual increase with time in absorbance in the shorter wavelength region (400-600 nm). The 430 nm absorbance (ligand field transition of Fe3+ increased more with time at higher temperatures. Assuming diffusional transport in plane sheets, apparent diffusion coefficients were determined at temperatures of 600-800 degrees C. The activation energy for this diffusion in olivine is 208 +/- 17 kJ/mol. This activation energy value is similar to those for the metal vacancy diffusion in olivine. This newly developed in situ high-temperature visible microspectroscopy can provide kinetic measurements of visible spectral change of materials at high temperatures such as volcanic materials.

  2. In-situ High Temperature Phase Transformations in Ceramics

    DTIC Science & Technology

    2009-07-28

    in high temperature combustion environments leads to accelerated oxidation of Si-based ceramics and composites, such as silicon carbide ( SiC ) fiber...have been achieved in silicon carbide reinforced with continuous, graphite-coated, silicon carbide fibers. The graphite acts as a debonding layer...reinforced SiC ceramic matrix composites (SiCf/ SiC CMCs) and monolithic silicon nitride (Si3N4), and severely limits their application in gas

  3. Novel High Temperature Materials for In-Situ Sensing Devices

    SciTech Connect

    Florian Solzbacher; Anil Virkar; Loren Rieth; Srinivasan Kannan; Xiaoxin Chen; Hannwelm Steinebach

    2009-12-31

    The overriding goal of this project was to develop gas sensor materials and systems compatible with operation at temperatures from 500 to 700 C. Gas sensors operating at these temperatures would be compatible with placement in fossil-energy exhaust streams close to the combustion chamber, and therefore have advantages for process regulation, and feedback for emissions controls. The three thrusts of our work included investigating thin film gas sensor materials based on metal oxide materials and electroceramic materials, and also development of microhotplate devices to support the gas sensing films. The metal oxide materials NiO, In{sub 2}O{sub 3}, and Ga{sub 2}O{sub 3} were investigated for their sensitivity to H{sub 2}, NO{sub x}, and CO{sub 2}, respectively, at high temperatures (T > 500 C), where the sensing properties of these materials have received little attention. New ground was broken in achieving excellent gas sensor responses (>10) for temperatures up to 600 C for NiO and In{sub 2}O{sub 3} materials. The gas sensitivity of these materials was decreasing as temperatures increased above 500 C, which indicates that achieving strong sensitivities with these materials at very high temperatures (T {ge} 650 C) will be a further challenge. The sensitivity, selectivity, stability, and reliability of these materials were investigated across a wide range of deposition conditions, temperatures, film thickness, as using surface active promoter materials. We also proposed to study the electroceramic materials BaZr{sub (1-x)}Y{sub x}O{sub (3-x/2)} and BaCe{sub (2-x)}Ca{sub x}S{sub (4-x/2)} for their ability to detect H{sub 2}O and H{sub 2}S, respectively. This report focuses on the properties and gas sensing characteristics of BaZr{sub (1-x)}Y{sub x}O{sub (3-x/2)} (Y-doped BaZrO{sub 3}), as significant difficulties were encounter in generating BaCe{sub (2-x)}Ca{sub x}S{sub (4-x/2)} sensors. Significant new results were achieved for Y-doped BaZrO{sub 3}, including

  4. In situ Raman cell for high pressure and temperature studies of metal and complex hydrides.

    PubMed

    Domènech-Ferrer, Roger; Ziegs, Frank; Klod, Sabrina; Lindemann, Inge; Voigtländer, Ralf; Dunsch, Lothar; Gutfleisch, Oliver

    2011-04-15

    A novel cell for in situ Raman studies at hydrogen pressures up to 200 bar and at temperatures as high as 400 °C is presented. This device permits in situ monitoring of the formation and decomposition of chemical structures under high pressure via Raman scattering. The performance of the cell under extreme conditions is stable as the design of this device compensates much of the thermal expansion during heating which avoids defocusing of the laser beam. Several complex and metal hydrides were analyzed to demonstrate the advantageous use of this in situ cell. Temperature calibration was performed by monitoring the structural phase transformation and melting point of LiBH(4). The feasibility of the cell in hydrogen atmosphere was confirmed by in situ studies of the decomposition of NaAlH(4) with added TiCl(3) at different hydrogen pressures and the decomposition and rehydrogenation of MgH(2) and LiNH(2).

  5. Sealed rotors for in situ high temperature high pressure MAS NMR

    SciTech Connect

    Hu, Jian Z.; Hu, Mary Y.; Zhao, Zhenchao; Xu, Souchang; Vjunov, Aleksei; Shi, Hui; Camaioni, Donald M.; Peden, Charles H. F.; Lercher, Johannes A.

    2015-07-06

    Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization, a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.

  6. Sealed rotors for in situ high temperature high pressure MAS NMR

    DOE PAGES

    Hu, Jian Z.; Hu, Mary Y.; Zhao, Zhenchao; ...

    2015-07-06

    Magic angle spinning (MAS) nuclear magnetic resonance (NMR) investigations on heterogeneous samples containing solids, semi-solids, liquid and gases or a mixture of them under non-conventional conditions of a combined high pressure and high temperature, or cold temperature suffer from the unavailability of a perfectly sealed rotor. Here, we report the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are easy to use and are suitable for operation temperatures from below 0 to 250 °C and pressures up to 100 bar. As an example of potential applications we performed in situ MAS NMR investigations of AlPO₄-5 molecular sieve crystallization,more » a kinetic study of the cyclohexanol dehydration reaction using 13C MAS NMR, and an investigation of the metabolomics of intact biological tissue at low temperature using 1H HR-MAS NMR spectroscopy. The in situ MAS NMR experiments performed using the reported rotors allowed reproduction of the results from traditional batch reactions, while offering more detailed quantitative information at the molecular level, as demonstrated for the molecular sieve synthesis and activation energy measurements for cyclohexanol dehydration. The perfectly sealed rotor also shows promising application for metabolomics studies using 1H HR-MAS NMR.« less

  7. In Situ Observation of Gypsum-Anhydrite Transition at High Pressure and High Temperature

    NASA Astrophysics Data System (ADS)

    Liu, Chuan-Jiang; Zheng, Hai-Fei

    2012-04-01

    An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC). The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 MPa. With increasing temperature, the anhydrite (CaSO4) phase precipitates at 250-320°C in the pressure range of 1.0-1.5GPa, indicating that under a saturated water condition, both stable conditions of pressure and temperature and high levels of Ca and SO4 ion concentrations in aqueous solution are essential for the formation of anhydrite. A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(GPa) = 0.0068T-0.7126 (250°C<=T<=320°C). Anhydrite remained stable during rapid cooling of the sample chamber, showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is irreversible at high pressure and high temperature.

  8. MAX200x: In-situ X-ray Measurements at High Pressure and High Temperatures.

    NASA Astrophysics Data System (ADS)

    Lathe, C.; Mueller, H. J.; Wehber, M.; Lauterjung, J.; Schilling, F. R.

    2009-05-01

    Twenty years ago geoscientists from all over the world launched in-situ X-ray diffraction experiments under extreme pressure and temperature conditions at synchrotron beamlines. One of the first apparatus was installed at HASYLAB, MAX80, a single-stage multi-anvil system. MAX80 allows in-situ diffraction studies in conjunction with the simultaneous measurement of elastic properties up to 12 GPa and 1600 K. This very successful experiment, unique in Europe, is operated by Helmholtz Centre Potsdam and is used by more than twenty groups from different countries every year. Experiments for both, applied and basic research are conducted, ranging from life-sciences, chemistry, physics, over material sciences to geosciences. Today new materials and the use of high brilliant synchrotron sources allow constructing double-stage multi-anvil systems for X-ray diffraction to reach much higher pressures. The newly designed high-flux hard wiggler (HARWI-II) beamline is an ideal X-ray source for this kind of experiments. As only the uppermost few kilometres of the Earth (less than 0.1% of its radius) are accessible for direct observations (e.g. deep drilling), sophisticated techniques are required to observe and to understand the processes in the deep interior of our planet. In-situ studies are an excellent tool to investigate ongoing geodynamic processes within the laboratory. One of the fundamental regions to study geodynamic processes seems to be the so-called transition zone, the boundary between upper and lower Earth's mantle between 410 and 670 km depth. Mineral reactions, phase transitions, as wheel as fluid rock interaction in this area might have the potential to strongly influence and control the dynamic motions within our whole planet. Around 25 GPa and 2 000 K are required to simulate these processes in the laboratory. The new MAX200x will be an excellent tool for these ambitious experiments.

  9. Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

    PubMed

    Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

    2013-10-01

    In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

  10. INTEGRATION OF HIGH TEMPERATURE GAS REACTORS WITH IN SITU OIL SHALE RETORTING

    SciTech Connect

    Eric P. Robertson; Michael G. McKellar; Lee O. Nelson

    2011-05-01

    This paper evaluates the integration of a high-temperature gas-cooled reactor (HTGR) to an in situ oil shale retort operation producing 7950 m3/D (50,000 bbl/day). The large amount of heat required to pyrolyze the oil shale and produce oil would typically be provided by combustion of fossil fuels, but can also be delivered by an HTGR. Two cases were considered: a base case which includes no nuclear integration, and an HTGR-integrated case.

  11. High-temperature ultrasonic sensor for in-situ monitoring of hot isostatic processing

    NASA Astrophysics Data System (ADS)

    Stubbs, David A.; Dutton, Rollie E.

    1996-11-01

    A sensor has been developed and tested that is capable of emitting and receiving ultrasonic energy at temperatures exceeding 900 degrees C and pressures above 150 MPa. The sensor is based on a unique form of aluminum nitride that retains tits piezoelectric properties at high temperatures. The sensor works with standard ultrasonic pulse-receivers and has demonstrated the capability of measuring workpiece deformation during hot isostatic pressing (HIP). Details of the sensor design, performance, and coupling of the ultrasound to the workpiece are described. Ultrasonic data acquired by the sensor, in situ, during HIP runs and at elevated temperatures in air are presented.

  12. In situ observation and measurement of composites subjected to extremely high temperature

    NASA Astrophysics Data System (ADS)

    Fang, Xufei; Yu, Helong; Zhang, Guobing; Su, Hengqiang; Tang, Hongxiang; Feng, Xue

    2014-03-01

    In this work, we develop an instrument to study the ablation and oxidation process of materials such as C/SiC (carbon fiber reinforced silicon carbide composites) and ultra-high temperature ceramic in extremely high temperature environment. The instrument is integrated with high speed cameras with filtering lens, infrared thermometers and water vapor generator for image capture, temperature measurement, and humid atmosphere, respectively. The ablation process and thermal shock as well as the temperature on both sides of the specimen can be in situ monitored. The results show clearly the dynamic ablation and liquid oxide flowing. In addition, we develop an algorithm for the post-processing of the captured images to obtain the deformation of the specimens, in order to better understand the behavior of the specimen subjected to high temperature.

  13. Low Cost Al-Si Casting Alloy As In-Situ Composite for High Temperature Applications

    NASA Technical Reports Server (NTRS)

    Lee, Jonathan A.

    2000-01-01

    A new aluminum-silicon (Al-Si) alloy has been successfully developed at NASA- Marshall Space Flight Center (MSFC) that has significant improvement in tensile and fatigue strength at elevated temperatures (500 F-700 F). The alloy offers a number of benefits such as light weight, high hardness, low thermal expansion and high surface wear resistance. In hypereutectic form, this alloy is considered as an in-situ Al-Si composite with tensile strength of about 90% higher than the auto industry 390 alloy at 600 F. This composite is very economically produced by using either conventional permanent steel molds or die casting. The projected material cost is less than $0.90 per pound, and automotive components such as pistons can be cast for high production rate using conventional casting techniques with a low and fully accounted cost. Key Words: Metal matrix composites, In-situ composite, aluminum-silicon alloy, hypereutectic alloy, permanent mold casting, die casting.

  14. High-sensitivity in situ QCLAS-based ammonia concentration sensor for high-temperature applications

    NASA Astrophysics Data System (ADS)

    Peng, W. Y.; Sur, R.; Strand, C. L.; Spearrin, R. M.; Jeffries, J. B.; Hanson, R. K.

    2016-07-01

    A novel quantum cascade laser (QCL) absorption sensor is presented for high-sensitivity in situ measurements of ammonia (hbox {NH}_3) in high-temperature environments, using scanned wavelength modulation spectroscopy (WMS) with first-harmonic-normalized second-harmonic detection (scanned WMS-2 f/1 f) to neutralize the effect of non-absorption losses in the harsh environment. The sensor utilized the sQ(9,9) transition of the fundamental symmetric stretch band of hbox {NH}_3 at 10.39 {\\upmu }hbox {m} and was sinusoidally modulated at 10 kHz and scanned across the peak of the absorption feature at 50 Hz, leading to a detection bandwidth of 100 Hz. A novel technique was used to select an optimal WMS modulation depth parameter that reduced the sensor's sensitivity to spectral interference from hbox {H}_2hbox {O} and hbox {CO}_2 without significantly sacrificing signal-to-noise ratio. The sensor performance was validated by measuring known concentrations of hbox {NH}_3 in a flowing gas cell. The sensor was then demonstrated in a laboratory-scale methane-air burner seeded with hbox {NH}_3, achieving a demonstrated detection limit of 2.8 ± 0.26 ppm hbox {NH}_3 by mole at a path length of 179 cm, equivalence ratio of 0.6, pressure of 1 atm, and temperatures of up to 600 K.

  15. Deformation at ambient and high temperature of in situ Laves phases-ferrite composites.

    PubMed

    Donnadieu, Patricia; Pohlmann, Carsten; Scudino, Sergio; Blandin, Jean-Jacques; Babu Surreddi, Kumar; Eckert, Jürgen

    2014-06-01

    The mechanical behavior of a Fe80Zr10Cr10 alloy has been studied at ambient and high temperature. This Fe80Zr10Cr10 alloy, whoose microstructure is formed by alternate lamellae of Laves phase and ferrite, constitutes a very simple example of an in situ CMA phase composite. The role of the Laves phase type was investigated in a previous study while the present work focuses on the influence of the microstructure length scale owing to a series of alloys cast at different cooling rates that display microstructures with Laves phase lamellae width ranging from ∼50 nm to ∼150 nm. Room temperature compression tests have revealed a very high strength (up to 2 GPa) combined with a very high ductility (up to 35%). Both strength and ductility increase with reduction of the lamella width. High temperature compression tests have shown that a high strength (900 MPa) is maintained up to 873 K. Microstructural study of the deformed samples suggests that the confinement of dislocations in the ferrite lamellae is responsible for strengthening at both ambient and high temperature. The microstructure scale in addition to CMA phase structural features stands then as a key parameter for optimization of mechanical properties of CMA in situ composites.

  16. Deformation at ambient and high temperature of in situ Laves phases-ferrite composites

    PubMed Central

    Donnadieu, Patricia; Pohlmann, Carsten; Scudino, Sergio; Blandin, Jean-Jacques; Babu Surreddi, Kumar; Eckert, Jürgen

    2014-01-01

    The mechanical behavior of a Fe80Zr10Cr10 alloy has been studied at ambient and high temperature. This Fe80Zr10Cr10 alloy, whoose microstructure is formed by alternate lamellae of Laves phase and ferrite, constitutes a very simple example of an in situ CMA phase composite. The role of the Laves phase type was investigated in a previous study while the present work focuses on the influence of the microstructure length scale owing to a series of alloys cast at different cooling rates that display microstructures with Laves phase lamellae width ranging from ∼50 nm to ∼150 nm. Room temperature compression tests have revealed a very high strength (up to 2 GPa) combined with a very high ductility (up to 35%). Both strength and ductility increase with reduction of the lamella width. High temperature compression tests have shown that a high strength (900 MPa) is maintained up to 873 K. Microstructural study of the deformed samples suggests that the confinement of dislocations in the ferrite lamellae is responsible for strengthening at both ambient and high temperature. The microstructure scale in addition to CMA phase structural features stands then as a key parameter for optimization of mechanical properties of CMA in situ composites. PMID:27877672

  17. High-temperature in situ crystallographic observation of reversible gas sorption in impermeable organic cages.

    PubMed

    Baek, Seung Bin; Moon, Dohyun; Graf, Robert; Cho, Woo Jong; Park, Sung Woo; Yoon, Tae-Ung; Cho, Seung Joo; Hwang, In-Chul; Bae, Youn-Sang; Spiess, Hans W; Lee, Hee Cheon; Kim, Kwang S

    2015-11-17

    Crystallographic observation of adsorbed gas molecules is a highly difficult task due to their rapid motion. Here, we report the in situ single-crystal and synchrotron powder X-ray observations of reversible CO2 sorption processes in an apparently nonporous organic crystal under varying pressures at high temperatures. The host material is formed by hydrogen bond network between 1,3,5-tris-(4-carboxyphenyl)benzene (H3BTB) and N,N-dimethylformamide (DMF) and by π-π stacking between the H3BTB moieties. The material can be viewed as a well-ordered array of cages, which are tight packed with each other so that the cages are inaccessible from outside. Thus, the host is practically nonporous. Despite the absence of permanent pathways connecting the empty cages, they are permeable to CO2 at high temperatures due to thermally activated molecular gating, and the weakly confined CO2 molecules in the cages allow direct detection by in situ single-crystal X-ray diffraction at 323 K. Variable-temperature in situ synchrotron powder X-ray diffraction studies also show that the CO2 sorption is reversible and driven by temperature increase. Solid-state magic angle spinning NMR defines the interactions of CO2 with the organic framework and dynamic motion of CO2 in cages. The reversible sorption is attributed to the dynamic motion of the DMF molecules combined with the axial motions/angular fluctuations of CO2 (a series of transient opening/closing of compartments enabling CO2 molecule passage), as revealed from NMR and simulations. This temperature-driven transient molecular gating can store gaseous molecules in ordered arrays toward unique collective properties and release them for ready use.

  18. High-temperature in situ crystallographic observation of reversible gas sorption in impermeable organic cages

    PubMed Central

    Baek, Seung Bin; Moon, Dohyun; Graf, Robert; Cho, Woo Jong; Park, Sung Woo; Yoon, Tae-Ung; Cho, Seung Joo; Hwang, In-Chul; Bae, Youn-Sang; Spiess, Hans W.; Lee, Hee Cheon; Kim, Kwang S.

    2015-01-01

    Crystallographic observation of adsorbed gas molecules is a highly difficult task due to their rapid motion. Here, we report the in situ single-crystal and synchrotron powder X-ray observations of reversible CO2 sorption processes in an apparently nonporous organic crystal under varying pressures at high temperatures. The host material is formed by hydrogen bond network between 1,3,5-tris-(4-carboxyphenyl)benzene (H3BTB) and N,N-dimethylformamide (DMF) and by π–π stacking between the H3BTB moieties. The material can be viewed as a well-ordered array of cages, which are tight packed with each other so that the cages are inaccessible from outside. Thus, the host is practically nonporous. Despite the absence of permanent pathways connecting the empty cages, they are permeable to CO2 at high temperatures due to thermally activated molecular gating, and the weakly confined CO2 molecules in the cages allow direct detection by in situ single-crystal X-ray diffraction at 323 K. Variable-temperature in situ synchrotron powder X-ray diffraction studies also show that the CO2 sorption is reversible and driven by temperature increase. Solid-state magic angle spinning NMR defines the interactions of CO2 with the organic framework and dynamic motion of CO2 in cages. The reversible sorption is attributed to the dynamic motion of the DMF molecules combined with the axial motions/angular fluctuations of CO2 (a series of transient opening/closing of compartments enabling CO2 molecule passage), as revealed from NMR and simulations. This temperature-driven transient molecular gating can store gaseous molecules in ordered arrays toward unique collective properties and release them for ready use. PMID:26578758

  19. A hot tip: imaging phenomena using in situ multi-stimulus probes at high temperatures

    NASA Astrophysics Data System (ADS)

    Nonnenmann, Stephen S.

    2016-02-01

    Accurate high temperature characterization of materials remains a critical challenge to the continued advancement of various important energy, nuclear, electronic, and aerospace applications. Future experimental studies must assist these communities to progress past empiricism and derive deliberate, predictable designs of material classes functioning within active, extreme environments. Successful realization of systems ranging from fuel cells and batteries to electromechanical nanogenerators and turbines requires a dynamic understanding of the excitation, surface-mediated, and charge transfer phenomena which occur at heterophase interfaces (i.e. vapor-solid, liquid-solid, solid-solid) and impact overall performance. Advancing these frontiers therefore necessitates in situ (operando) characterization methods capable of resolving, both spatially and functionally, the coherence between these complex, collective excitations, and their respective response dynamics, through studies within the operating regime. This review highlights recent developments in scanning probe microscopy in performing in situ imaging at high elevated temperatures. The influence of and evolution from vacuum-based electron and tunneling microscopy are briefly summarized and discussed. The scope includes the use of high temperature imaging to directly observe critical phase transition, electronic, and electrochemical behavior under dynamic temperature settings, thus providing key physical parameters. Finally, both challenges and directions in combined instrumentation are proposed and discussed towards the end.

  20. In Situ Optical Observation of High-Temperature Geological Processes With the Moissanite Cell

    NASA Astrophysics Data System (ADS)

    Walte, N.; Keppler, H.

    2005-12-01

    A major drawback of existing techniques in experimental earth and material sciences is the inability to observe ongoing high-temperature processes in situ during an experiment. Examples for important time-dependent processes include the textural development of rocks and oxide systems during melting and crystallization, solid-state and melt-present recrystallization and Ostwald ripening, and bubble nucleation and growth during degassing of glasses and melts. The investigation of these processes by post-mortem analysis of a quenched microstructure is time consuming and often unsatisfactory. Here, we introduce the moissanite cell that allows optical in situ observation of long-term experiments at high temperatures. Moissanite is a transparent gem-quality type of SiC that is characterized by its hardness and superior chemical and thermal resistance. Two moissanite windows with a thickness and diameter of several millimeters are placed into sockets of fired pyrophyllite and fixed onto two opposite metal plates. The sockets are wrapped with heating wire and each window is connected to a thermocouple for temperature control. The sample is placed directly between the moissanite windows and the cell is assembled similarly to a large diamond anvil cell. In situ observation of the sample is done with a microscope through observation windows and movies are recorded with an attached digital camera. Our experiments with the new cell show that temperatures above 1200°C can be maintained and observed in a sample for several days without damaging the cell nor the windows. Time-lapse movies of melting and crystallizing natural and synthetic rocks and of degassing glasses and melts will be presented to show the potential of the new technique for experimental earth and material science.

  1. In situ synthesis and characterization of uranium carbide using high temperature neutron diffraction

    NASA Astrophysics Data System (ADS)

    Reiche, H. Matthias; Vogel, Sven C.; Tang, Ming

    2016-04-01

    We investigated the formation of UCx from UO2+x and graphite in situ using neutron diffraction at high temperatures with particular focus on resolving the conflicting reports on the crystal structure of non-quenchable cubic UC2. The agents were UO2 nanopowder, which closely imitates nano grains observed in spent reactor fuels, and graphite powder. In situ neutron diffraction revealed the onset of the UO2 + 2C → UC + CO2 reaction at 1440 °C, with its completion at 1500 °C. Upon further heating, carbon diffuses into the uranium carbide forming C2 groups at the octahedral sites. This resulting high temperature cubic UC2 phase is similar to the NaCl-type structure as proposed by Bowman et al. Our novel experimental data provide insights into the mechanism and kinetics of formation of UC as well as characteristics of the high temperature cubic UC2 phase which agree with proposed rotational rehybridization found from simulations by Wen et al.

  2. Acousto-optic Imaging System for In-situ Measurement of the High Temperature Distribution in Micron-size Specimens

    NASA Astrophysics Data System (ADS)

    Machikhin, Alexander S.; Zinin, Pavel V.; Shurygin, Alexander V.

    We developed a unique acousto-optic imaging system for in-situ measurement of high temperature distribution on micron-size specimens. The system was designed to measure temperature distribution inside minerals and functional material phases subjected to high pressure and high temperatures in a diamond anvil cell (DAC) heated by a high powered laser.

  3. In situ high temperature microscopy study of the surface oxidation and phase transformations in titanium alloys.

    PubMed

    Malinov, S; Sha, W; Voon, C S

    2002-09-01

    Two popular commercial titanium alloys, Ti-6Al-4V and Ti-6Al-2Sn-4Zr-2Mo-0.08Si, were used for in situ high temperature microscopy study. The experiments were performed on an optical microscope equipped with high temperature stage using both normal and florescence lights. Two kinds of experiments were performed, at continuous heating/cooling with different rates and in isothermal conditions at different temperatures. The changes taking place on the sample surface during the experiments were monitored. The morphology of the alpha ==> beta ==> alpha phase transformation was recorded at different heat treatment conditions using the effect of thermal etching. An effect of sample surface oxidation and deoxidation was observed during continuous heating. The appearance and disappearance of ordered titanium oxides Ti3O and Ti2O are discussed based on the phase equilibrium diagram. The kinetics of the surface oxidation was monitored in both isothermal and continuous cooling conditions.

  4. High temperature stable W/O emulsions prepared with in-situ hydrophobically modified rodlike sepiolite.

    PubMed

    Zhang, Li; Li, Zhenbang; Wang, Lei; Sun, Dejun

    2017-05-01

    Hydrophobic modification can influence interparticle interaction, their interfacial adsorption, and stability of particle-stabilized emulsions. Emulsions stabilized by rodlike particles are more stable than those prepared with spherical particles even at low concentrations. Moreover, interfacial adsorption of particles will be tuned by controlling the modification. Thus, it is possible to prepare stable W/O emulsions with in-situ modified rodlike particles. Rodlike sepiolite particles were in-situ modified in oil using dimethyldioctadecylammonium chloride (DODMAC). High salinity solution (water) in paraffin oil (W/O) emulsion was prepared with the modified particles. Stability of emulsions at room temperature and after aging at 160°C for 24h was studied. Mechanism of emulsion stability was explored by rheological measurements and confocal fluorescent microscopy. Remarkable stability against coalescence was found at high temperature. The enhanced stability is due to the high viscosity of continuous phase. Moreover, modification of sepiolite particles at high DOMDAC concentrations enhances particle adsorption at water-oil interfaces and network in continuous phase, which improve the stability against sedimentation and coalescence of the W/O emulsions. Copyright © 2017 Elsevier Inc. All rights reserved.

  5. In situ analysis of texture development from sinusoidal stress at high pressure and temperature

    SciTech Connect

    Li, Li; Weidner, Donald J.

    2015-12-15

    Here, we present a new experimental protocol to investigate the relationship between texture, plastic strain, and the mechanisms of plastic deformation at high pressure and temperature. The method utilizes synchrotron X-ray radiation as the probing tool, coupled with a large-volume high pressure deformation device (D-DIA). The intensity of X-ray diffraction peaks within the spectrum of the sample is used for sampling texture development in situ. The unique feature of this study is given by the sinusoidal variation of the intensity when a sinusoidal strain is applied to the sample. For a sample of magnesium oxide at elevated pressure and temperature, we demonstrate observations that are consistent with elasto-plastic models for texture development and for diffraction-peak measurements of apparent stress. The sinusoidal strain magnitude was 3%.

  6. An experimental system for high temperature X-ray diffraction studies with in situ mechanical loading

    PubMed Central

    Oswald, Benjamin B.; Schuren, Jay C.; Pagan, Darren C.; Miller, Matthew P.

    2013-01-01

    An experimental system with in situ thermomechanical loading has been developed to enable high energy synchrotron x-ray diffraction studies of crystalline materials. The system applies and maintains loads of up to 2250 N in uniaxial tension or compression at a frequency of up to 100 Hz. The furnace heats the specimen uniformly up to a maximum temperature of 1200 °C in a variety of atmospheres (oxidizing, inert, reducing) that, combined with in situ mechanical loading, can be used to mimic processing and operating conditions of engineering components. The loaded specimen is reoriented with respect to the incident beam of x-rays using two rotational axes to increase the number of crystal orientations interrogated. The system was used at the Cornell High Energy Synchrotron Source to conduct experiments on single crystal silicon and polycrystalline Low Solvus High Refractory nickel-based superalloy. The data from these experiments provide new insights into how stresses evolve at the crystal scale during thermomechanical loading and complement the development of high-fidelity material models. PMID:23556825

  7. A new device for high precision in situ sediment temperature profile measurements at the seafloor

    NASA Astrophysics Data System (ADS)

    Feseker, T.; Wetzel, G.; Heesemann, B.

    2012-04-01

    In situ sediment temperature profile measurements at the seafloor provide valuable information on fluid seepage, hydrate stability, and ambient temperature of samples. In addition, it can be convenient to approximate other parameters such as concentrations of porewater constituents from temperature or temperature gradient using transfer functions if their distribution is controlled by the same processes and direct quantification involves time-consuming sampling and laboratory analyses. We present a new instrument that can be used to obtain precisely positioned sediment temperature profile measurements from the seafloor during ROV dives. Consisting of a 0.4 m-long sensor rod equipped with eight temperature sensors and a standard data logger, the new T-Stick can be operated by an ROV in a fully autonomous mode. The temperature range of the instrument is -5 °C to 35 °C and it can withstand pressures of up to 600 bar. Compared to previously used instruments, the smaller diameter of the new T-Stick reduces the thermal inertia of the lance and results in shorter equilibration times. Virtual measurements generated by a numerical model showed that the T-Stick provides highly accurate temperature profile measurements with a root mean square error of 0.0027 K for a wide range of thermal sediment properties. Modeled temperature gradients are representative of both normal deep sea settings and cold seep environments with elevated temperature gradients of up to three orders of magnitude above normal background values, which are the primary target areas for T-Stick measurements. Deviations from the true in situ temperature profiles are caused by disturbance of the temperature field by the probe itself and may lead to underestimation of gradients and curvature in the profiles. A first field test of the T-Stick was conducted at the Håkon Mosby mud volcano at 1250 m water depth on the Barents Sea slope, where the new instrument provided useful information about the origin and

  8. High-Temperature Nuclear Reactors for In-Situ Recovery of Oil from Oil Shale

    SciTech Connect

    Forsberg, Charles W.

    2006-07-01

    The world is exhausting its supply of crude oil for the production of liquid fuels (gasoline, jet fuel, and diesel). However, the United States has sufficient oil shale deposits to meet our current oil demands for {approx}100 years. Shell Oil Corporation is developing a new potentially cost-effective in-situ process for oil recovery that involves drilling wells into oil shale, using electric heaters to raise the bulk temperature of the oil shale deposit to {approx}370 deg C to initiate chemical reactions that produce light crude oil, and then pumping the oil to the surface. The primary production cost is the cost of high-temperature electrical heating. Because of the low thermal conductivity of oil shale, high-temperature heat is required at the heater wells to obtain the required medium temperatures in the bulk oil shale within an economically practical two to three years. It is proposed to use high-temperature nuclear reactors to provide high-temperature heat to replace the electricity and avoid the factor-of-2 loss in converting high-temperature heat to electricity that is then used to heat oil shale. Nuclear heat is potentially viable because many oil shale deposits are thick (200 to 700 m) and can yield up to 2.5 million barrels of oil per acre, or about 125 million dollars/acre of oil at $50/barrel. The concentrated characteristics of oil-shale deposits make it practical to transfer high-temperature heat over limited distances from a reactor to the oil shale deposits. (author)

  9. High temperature phase transitions and critical exponents of Samarium orthoferrite determined by in situ optical ellipsometry

    NASA Astrophysics Data System (ADS)

    Berini, B.; Fouchet, A.; Popova, E.; Scola, J.; Dumont, Y.; Franco, N.; da Silva, R. M. C.; Keller, N.

    2012-03-01

    Determining phase transitions has always been a great challenge in material science due to their important fundamental and technological aspects. Recently, iron-based perovskites (RFeO3), exhibiting phase transitions at high temperatures, have attracted much interest for their functional properties at room temperature, such as multiferroicity (BiFeO3) and ultrafast spin dynamics (TmFeO3). In this family of materials, Samarium orthoferrite (SmFeO3) is a weak ferromagnet, ordering at high temperatures and exhibiting an intrinsic spin reorientation transition above room temperature, which is "hidden" in macroscopic magnetization measurements in polycrystalline samples. In the present article, we show that the related magnetic high temperature phase transitions can be studied through their dielectric functions by spectroscopic ellipsometry in situ and without any need for an applied external magnetic field. The presence of this intrinsic spin reorientation transition is demonstrated for textured SmFeO3 films and we have determined a critical exponent of β = 0.45 ± 0.01 for the magnetic phase transition, coherently from optical, magneto-optical, and structural investigations.

  10. In Situ XANES of U and Th in Silicate Liquids at High Pressure and Temperature

    NASA Astrophysics Data System (ADS)

    Mallmann, G.; Wykes, J.; Berry, A.; O'Neill, H. S.; Cline, C. J., II; Turner, S.; Rushmer, T. A.

    2016-12-01

    Although the chemical environments of elements in silicate melts at specific conditions of temperature, pressure and oxygen fugacity (fO2) are often inferred from measurements after quenching the melts to glasses, it is widely recognized that changes may occur during the quenching process, making measurements in situ at high pressure and temperature highly desirable. A case of importance in geochemistry is the speciation of uranium in silicate melts as a function of pressure. Evidence from mineral-melt partitioning and XANES (X-ray Absorption Near-Edge Structure) spectroscopy of glasses suggests that U5+ may be stable at low pressures in the Earth's crust (along with U4+ or U6+, depending on fO2) where basaltic liquids crystallize, but not in the Earth's upper mantle where peridotite partially melts to produce such liquids. To test these observations we recorded in situ transmission U and Th L3-edge XANES spectra of U and Th-doped silicate liquids at 1.6 GPa and 1350°C using the D-DIA apparatus at the X-ray Absorption Spectroscopy Beamline of the Australian Synchrotron. Data for thorium, which occurs exclusively as a tetravalent cation under terrestrial fO2 conditions, were collected as a `control' to monitor for changes in coordination. The cell assembly consisted of a boron-epoxy cube as pressure medium, alumina sleeve and cylindrical graphite heater. The starting mix, a powdered synthetic average MORB silicate glass doped with 2 wt.% of U and Th, was loaded into San Carlos olivine capsules along with solid oxygen buffers (either Re-ReO2 or Ru-RuO2) in a sandwich arrangement. The capsule was then placed inside the graphite heater and insulated with crushable MgO powder. Temperature was monitored using a type D thermocouple. U and Th L3-edge XANES spectra were recorded throughout the heating/compression cycle and then after quenching. Our preliminary assessment indicates that the U-XANES spectra recorded for the liquid in situ at high pressure and temperature and

  11. Molecular Tagging Velocimetry Development for In-situ Measurement in High-Temperature Test Facility

    NASA Technical Reports Server (NTRS)

    Andre, Matthieu A.; Bardet, Philippe M.; Burns, Ross A.; Danehy, Paul M.

    2015-01-01

    The High Temperature Test Facility, HTTF, at Oregon State University (OSU) is an integral-effect test facility designed to model the behavior of a Very High Temperature Gas Reactor (VHTR) during a Depressurized Conduction Cooldown (DCC) event. It also has the ability to conduct limited investigations into the progression of a Pressurized Conduction Cooldown (PCC) event in addition to phenomena occurring during normal operations. Both of these phenomena will be studied with in-situ velocity field measurements. Experimental measurements of velocity are critical to provide proper boundary conditions to validate CFD codes, as well as developing correlations for system level codes, such as RELAP5 (http://www4vip.inl.gov/relap5/). Such data will be the first acquired in the HTTF and will introduce a diagnostic with numerous other applications to the field of nuclear thermal hydraulics. A laser-based optical diagnostic under development at The George Washington University (GWU) is presented; the technique is demonstrated with velocity data obtained in ambient temperature air, and adaptation to high-pressure, high-temperature flow is discussed.

  12. High-temperature cyclic fatigue-crack growth behavior in an in situ toughened silicon carbide

    SciTech Connect

    Chen, D.; Gilbert, C.J.; Zhang, X.F.; Ritchie, R.O.

    2000-02-09

    The growth of fatigue cracks at elevated temperatures (25--1,300 C) is examined under cyclic loading in an in situ toughened, monolithic silicon carbide with Al-B-C additions (termed ABC-SiC), with specific emphasis on the roles of temperature, load ratio, cyclic frequency, and loading mode (static vs cyclic). Extensive crack-growth data are presented, based on measurements form an electrical potential-drop crack-monitoring technique, adapted for use on ceramics at high temperatures. It was found that at equivalent stress-intensity levels, crack velocities under cyclic loads were significantly faster than those under static loads. Fatigue thresholds were found to decrease with increasing temperature up to 1,200 C; behavior at 1,300 C, however, was similar to that at 1,200 C. Moreover, no effect of frequency was detected (between 3 and 1,000 Hz), no evidence of creep cavitation or crack bridging by viscous ligaments of grain-boundary glassy phases in the crack wake. Indeed, fractography and crack-path sectioning revealed a fracture mode at 1,200--1,300 C that was essentially identical to that at room temperature, i.e., predominantly intergranular cracking with evidence of grain bridging in the crack wake. Such excellent crack-growth resistance is attributed to a process of grain-boundary microstructural evolution at elevated temperatures, specifically involving crystallization of the amorphous grain-boundary films/phases.

  13. High Temperature In Situ Compression of Thermoplastically Formed Nano-scale Metallic Glass

    NASA Astrophysics Data System (ADS)

    Mridha, Sanghita; Arora, Harpreet Singh; Lefebvre, Joseph; Bhowmick, Sanjit; Mukherjee, Sundeep

    2017-01-01

    The mechanical behavior of nano-scale metallic glasses was investigated by in situ compression tests in a scanning electron microscope. Platinum-based metallic glass nano-pillars were fabricated by thermoplastic forming. The nano-pillars and corresponding bulk substrate were tested in compression over the range of room temperature to glass transition. Stress-strain curves of the nano-pillars were obtained along with in situ observation of their deformation behavior. The bulk substrate as well as nano-pillars showed an increase in elastic modulus with temperature which is explained by diffusive rearrangement of atomic-scale viscoelastic units.

  14. Strontium titanate (100) surfaces monitoring by high temperature in situ ellipsometry

    NASA Astrophysics Data System (ADS)

    Hrabovsky, D.; Berini, B.; Fouchet, A.; Aureau, D.; Keller, N.; Etcheberry, A.; Dumont, Y.

    2016-03-01

    We report monitoring and analysis of the contamination overlayer on the surface of different SrTiO3 (STO) substrates by in situ spectroscopic ellipsometry (SE) and ex situ X-ray photoelectron spectroscopy (XPS) and atomic force microscopy (AFM). Substrates of STO with different terminations, random and TiO2 terminated, were heated from room temperature up to 720 °C under oxygen pressure in UHV chamber similar to conditions commonly used for epitaxial growth of perovskite oxides. Contamination layer on the substrate was modeled as an equivalent dielectric overlayer with a thickness of 2 nm at room temperature which decreases progressively during the heating up to reach its minimum (around 1 unit cell) at the temperature around 550 °C. After exposition to air, surface recovers a contamination layer on both types of substrates (with random termination and TiO2 termination). XPS analysis confirmed that water and carbon dioxide as adventitious carbon species present in air are chemically adsorbed on the STO surface, providing evidence of desorption process which persists until 550 °C. This condition is an important issue in order to obtain clean controlled interface between STO and deposited film for low temperature growth as for instance atomic layer deposition and integration of STO buffer layer on silicon. In situ SE commonly present in thin layer deposition systems is a powerful tool to monitor in situ surface contamination and decontamination temperature as it can be performed in situ even in operando.

  15. In Situ Measurements of Spectral Emissivity of Materials for Very High Temperature Reactors

    SciTech Connect

    G. Cao; S. J. Weber; S. O. Martin; T. L. Malaney; S. R. Slattery; M. H. Anderson; K. Sridharan; T. R. Allen

    2011-08-01

    An experimental facility for in situ measurements of high-temperature spectral emissivity of materials in environments of interest to the gas-cooled very high temperature reactor (VHTR) has been developed. The facility is capable of measuring emissivities of seven materials in a single experiment, thereby enhancing the accuracy in measurements due to even minor systemic variations in temperatures and environments. The system consists of a cylindrical silicon carbide (SiC) block with seven sample cavities and a deep blackbody cavity, a detailed optical system, and a Fourier transform infrared spectrometer. The reliability of the facility has been confirmed by comparing measured spectral emissivities of SiC, boron nitride, and alumina (Al2O3) at 600 C against those reported in literature. The spectral emissivities of two candidate alloys for VHTR, INCONEL{reg_sign} alloy 617 (INCONEL is a registered trademark of the Special Metals Corporation group of companies) and SA508 steel, in air environment at 700 C were measured.

  16. In situ measurement of dissolved chloride in high temperature hydrothermal fluids

    NASA Astrophysics Data System (ADS)

    Larson, B. I.; Olson, E. J.; Lilley, M. D.

    2007-05-01

    The ability to continuously monitor chemical properties of hydrothermal vent effluents for extended periods of time is essential to understanding dynamic processes responsible for the temporally variable nature of mid-ocean ridge hydrothermal systems. Although instruments do exist for some parameters, there has been no sensor capable of measuring the chloride concentration, an indicator of possible phase separation, on a real-time and long-term basis. In this article, we discuss the construction of a novel instrument which measures solution resistance as a proxy for chloride concentration. The sensor consists of four gold electrodes embedded in a cylindrical ZrO 2 ceramic housing. It has been successfully deployed in several high temperature vents at the Main Endeavour Field (MEF) on the Juan de Fuca ridge in the NE Pacific, and calibrated under simulated hydrothermal conditions ranging up to 380 °C and 300 bar. The in situ data clearly demonstrate a tidal influence on the effluent from some high temperature vents possibly relating to a subsurface mixing process involving non-seawater end-members. Non-tidal changes are used to constrain the sequence and type of controls operating on fluids circulating within the subsurface.

  17. In situ spectroscopic investigation of hyperthermophilic metal-respiring archaea at high-temperature

    NASA Astrophysics Data System (ADS)

    Ménez, B.; Bureau, H.; Gouget, B.; Avoscan, L.; Simionovici, A.; Somogyi, A.

    2003-04-01

    The main issue of this study is developing methodologies that can improve abilities to characterize life in extreme habitats. In particular, it aims at evaluating the possibility of monitoring microorganisms mediated reactions involving metals by using non destructive X-ray microprobe combined with high pressure and temperature micro-reactors. The first step was dedicated to the study of metal-respiring organisms that achieve growth with oxyanions of arsenate and selenate as their electron acceptors for the oxidation of organic substrates or H2, forming elemental selenium or arsenite, respectively, as the reduction products. We focused on a strictly anaerobic hyperthermophilic archaea, Pyrobaculum arsenaticum, recently isolated and well adapted to high levels of arsenate and selenate (Huber et al., 2000, System. Appl. Microbiol., 23, 305). We report here the first in situ X-ray Absorption Near Edge Structure (XANES) spectroscopic characterization of the oxidation state of selenium following microbial respiration at high temperature. A Basset-modified Hydrothermal Diamond Anvil Cell (HDAC) acts as anaerobic micro-reactor to reproduce extreme temperature and pressure conditions for life and allows, together with the direct visual observation of the organisms, the microbeam characterization of the changes of metal concentration and speciation induced by microbial activity. The measurements were performed at the ESRF on undulator beamline ID22. P. arsenaticum together with its culture medium, doped with selenate (50 μM), were loaded under N_2 atmosphere in the HDAC. High-resolution X-ray fluorescence and selenium K-edge XANES spectra were collected alternatively and continuously at high temperature (up to 95^oC), allowing for the time-resolved monitoring of the chemical evolution of the culture medium. Data processing is still in progress. In the long-term, our aim is, on one hand, to shed light on the tolerance in terms of temperature, pressure and metal

  18. In situ high-pressure and high-temperature experiments on n-heptane.

    PubMed

    Qiao, Erwei; Zheng, Haifei; Long, Changxing

    2012-02-01

    The Raman spectroscopy of n-heptane was investigated in a moissanite anvil cell at ambient temperatures and a diamond anvil cell under pressures of up to ~2000 MPa and at temperature range from 298 to 588 K. The results show that at room temperature the vibration modes, assigned to the symmetric and antisymmetric stretching of CH(3) and CH(2) stretching, shifted to higher frequency according to quasi-linearity with increasing pressure, and a liquid-solid phase transition occurred at near 1150 MPa. The high-temperature solidus line of n-heptane follows a quadratic function of P = 0.00737T(2) + 5.27977T - 1195.76556. Upon phase change, fitting the experimental data obtained in the temperature range of 183∼412 K to the Clausius-Clapeyron equation allows one to define the thermodynamic parameters of n-heptane of dP/dT = 0.01474T + 5.27977.

  19. Oxidation of UC: An in situ high temperature environmental scanning electron microscopy study

    NASA Astrophysics Data System (ADS)

    Gasparrini, Claudia; Podor, Renaud; Horlait, Denis; Rushton, Michael J. D.; Fiquet, Olivier; Lee, William Edward

    2017-10-01

    In situ HT-ESEM oxidation of sintered UC fragments revealed the morphological changes occurring during the transformation between UC to UO2 and UO2 to U3O8 at 723-848 K and in an atmosphere of 10-100 Pa O2. Two main oxidation pathways were revealed. Oxidation at 723 K in atmospheres ≤25 Pa O2 showed the transformation from UC to UO2+x, as confirmed by post mortem HRTEM analysis. This oxidation pathway was comprised of three steps: (i) an induction period, where only surface UC particles oxidised, (ii) a sample area expansion accompanied by crack formation and propagation, (iii) a stabilisation of the total crack length inferring that crack propagation had stopped. Samples oxidised under 50 Pa O2 at 723 K and at 773-848 K for 10-100 Pa O2 showed an ;explosive; oxidation pathway: (i) sample area expansion occurred as soon as oxygen was inserted into the chamber and crack propagation and crack length followed an exponential law; (ii) cracks propagated as a network and the oxide layer fragmented, (iii) an ;explosion; occurred causing a popcorn-like transformation, typical for oxidation from UO2 to U3O8. HRTEM characterisation revealed U3O8 preferentially grow in the [001] direction. The explosive growth, triggered by ignition of UC, proceeded as a self-propagating high-temperature synthesis reaction, with a propagation speed of 150-500 ± 50 μm/s.

  20. In situ high-temperature characterization of AlN-based surface acoustic wave devices

    NASA Astrophysics Data System (ADS)

    Aubert, Thierry; Bardong, Jochen; Legrani, Ouarda; Elmazria, Omar; Badreddine Assouar, M.; Bruckner, Gudrun; Talbi, Abdelkrim

    2013-07-01

    We report on in situ electrical measurements of surface acoustic wave delay lines based on AlN/sapphire structure and iridium interdigital transducers between 20 °C and 1050 °C under vacuum conditions. The devices show a great potential for temperature sensing applications. Burnout is only observed after 60 h at 1050 °C and is mainly attributed to the agglomeration phenomena undergone by the Ir transducers. However, despite the vacuum conditions, a significant oxidation of the AlN film is observed, pointing out the limitation of the considered structure at least at such extreme temperatures. Original structures overcoming this limitation are then proposed and discussed.

  1. In situ observation of crystallographic preferred orientation of deforming olivine at high pressure and high temperature

    NASA Astrophysics Data System (ADS)

    Ohuchi, T.; Nishihara, Y.; Seto, Y.; Kawazoe, T.; Nishi, M.; Maruyama, G.; Hashimoto, M.; Higo, Y.; Funakoshi, K. I.; Suzuki, A.; Kikegawa, T.; Irifune, T.

    2015-12-01

    Olivine is the main constituent mineral in Earth's upper mantle, and its crystallographic preferred orientation (CPO) controls the seismic anisotropy in the upper mantle. Because the relationship between fabric strength and seismic anisotropy shows an exponential form (Ismail and Mainprice, 1998), seismic anisotropy in the upper mantle is expected to have an upperlimit value. Hansen et al., (2014) demonstrated that a steady-state fabric of olivine is not reached until a very large shear strain (γ> 10) and fabric strength of olivine increases up to the J-index of 10-30 at 0.3 GPa. However, the strain dependency on the fabric strength of olivine needs to be evaluated at asthenospheric upper mantle pressures (2-13 GPa) because the relative activity of each slip system in olivine changes depending on pressure (e.g., Raterron et al., 2007). We experimentally evaluated the strain dependency of fabric strength of olivine in simple-shear geometry under upper mantle conditions (pressures of 1.3-3.8 GPa and temperatures of 1223-1573 K). The CPO of olivine was calculated from in-situ two-dimensional X-ray diffraction patterns. In the calculation, we simulated the optimized CPO which reproduces the two-dimensional X-ray diffraction pattern adopted from the experiments. The steady-state fabric strength of the A-type fabric was achieved within total shear strain of γ = 2. At strains higher than γ = 1, an increase in concentration of the [010] axes mainly contributes to an increase in fabric strength. At strains higher than γ = 2, the magnitude of VSH/VSV (i.e., ratio of horizontally and vertically polarized shear wave velocities) scarcely increased in most of the runs. The VSH/VSV of peridotite having the steady-state A-type olivine fabric coincides with that of recent global one-dimensional models under the assumption of horizontal flow, suggesting that the seismic anisotropy observed in the shallow upper mantle is mostly explained by the development of A-type olivine

  2. Rapid, in Situ Synthesis of High Capacity Battery Anodes through High Temperature Radiation-Based Thermal Shock.

    PubMed

    Chen, Yanan; Li, Yiju; Wang, Yanbin; Fu, Kun; Danner, Valencia A; Dai, Jiaqi; Lacey, Steven D; Yao, Yonggang; Hu, Liangbing

    2016-09-14

    High capacity battery electrodes require nanosized components to avoid pulverization associated with volume changes during the charge-discharge process. Additionally, these nanosized electrodes need an electronically conductive matrix to facilitate electron transport. Here, for the first time, we report a rapid thermal shock process using high-temperature radiative heating to fabricate a conductive reduced graphene oxide (RGO) composite with silicon nanoparticles. Silicon (Si) particles on the order of a few micrometers are initially embedded in the RGO host and in situ transformed into 10-15 nm nanoparticles in less than a minute through radiative heating. The as-prepared composites of ultrafine Si nanoparticles embedded in a RGO matrix show great performance as a Li-ion battery (LIB) anode. The in situ nanoparticle synthesis method can also be adopted for other high capacity battery anode materials including tin (Sn) and aluminum (Al). This method for synthesizing high capacity anodes in a RGO matrix can be envisioned for roll-to-roll nanomanufacturing due to the ease and scalability of this high-temperature radiative heating process.

  3. In situ visualization of magma deformation at high temperature using time-lapse 3D tomography

    NASA Astrophysics Data System (ADS)

    Godinho, jose; Lee, Peter; Lavallee, Yan; Kendrick, Jackie; Von-Aulock, Felix

    2016-04-01

    We use synchrotron based x-ray computed micro-tomography (sCT) to visualize, in situ, the microstructural evolution of magma samples 3 mm diameter with a resolution of 3 μm during heating and uniaxial compression at temperatures up to 1040 °C. The interaction between crystals, melt and gas bubbles is analysed in 4D (3D + time) during sample deformation. The ability to observe the changes of the microstructure as a function of time allow us to: a) study the effect of temperature in the ability of magma to fracture or deform; b) quantify bubble nucleation and growth rates during heating; c) study the relation between crystal displacement and volatile exsolution. We will show unique beautiful videos of how bubbles grow and coalescence, how samples and crystals within the sample fracture, heal and deform. Our study establishes in situ sCT as a powerful tool to quantify and visualize with micro-scale resolution fast processes taking place in magma that are essential to understand ascent in a volcanic conduit and validate existing models for determining the explosivity of volcanic eruptions. Tracking simultaneously the time and spatial changes of magma microstructures is shown to be primordial to study disequilibrium processes between crystals, melt and gas phases.

  4. Use of Atomic Layer Deposition to Improve the Stability of Silver Substrates for In-Situ, High Temperature SERS Measurements

    SciTech Connect

    John, Joshy; Mahurin, Shannon Mark; Dai, Sheng; Sepaniak, Michael

    2010-01-01

    A method to stabilize silver surface-enhanced Raman spectroscopy (SERS) substrates for in-situ, high temperature applications is demonstrated. Silver island films grown by thermal evaporation were coated with a thin layer (from 2.5nm to 5nm) of alumina by atomic layer deposition (ALD), which protects and stabilizes the SERS-active substrate without eliminating the Raman enhancement. The temporal stability of the alumina-coated silver island films was examined by measurement of the Raman intensity of rhodamine 6G molecules deposited onto bare and alumina-coated silver substrates over the course of thirty-four days. The coated substrates showed almost no change in SERS enhancement while the uncoated substrates exhibited a significant decrease in Raman intensity. To demonstrate the feasibility of the alumina-coated silver substrate as a probe of adsorbates and reactions at elevated temperatures, an in-situ SERS measurement of calcium nitrate tetrahydrate on bare and alumina-coated silver was performed at temperatures ranging from 25 C to 400 C. ALD deposition of an ultrathin alumina layer significantly improved the thermal stability of the SERS substrate thus enabling in-situ detection of the dehydration of the calcium nitrate tetrahydrate at elevated temperature. Despite some loss of Raman signal, the coated substrate exhibited greater thermal stability compared to the uncoated substrate. These experiments show that ALD can be used to synthesize stable SERS substrates capable of measuring adsorbates and processes at high temperature.

  5. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

    SciTech Connect

    Jacobsen, Matthew K.; Ridley, Christopher J.; Bocian, Artur; Kamenev, Konstantin V.; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J. Paul

    2014-04-15

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO{sub 3} have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  6. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures

    NASA Astrophysics Data System (ADS)

    Jacobsen, Matthew K.; Ridley, Christopher J.; Bocian, Artur; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J. Paul; Kamenev, Konstantin V.

    2014-04-01

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO3 have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  7. High-pressure cell for neutron diffraction with in situ pressure control at cryogenic temperatures.

    PubMed

    Jacobsen, Matthew K; Ridley, Christopher J; Bocian, Artur; Kirichek, Oleg; Manuel, Pascal; Khalyavin, Dmitry; Azuma, Masaki; Attfield, J Paul; Kamenev, Konstantin V

    2014-04-01

    Pressure generation at cryogenic temperatures presents a problem for a wide array of experimental techniques, particularly neutron studies due to the volume of sample required. We present a novel, compact pressure cell with a large sample volume in which load is generated by a bellow. Using a supply of helium gas up to a pressure of 350 bar, a load of up to 78 kN is generated with leak-free operation. In addition, special fiber ports added to the cryogenic center stick allow for in situ pressure determination using the ruby pressure standard. Mechanical stability was assessed using finite element analysis and the dimensions of the cell have been optimized for use with standard cryogenic equipment. Load testing and on-line experiments using NaCl and BiNiO3 have been done at the WISH instrument of the ISIS pulsed neutron source to verify performance.

  8. High-pressure, high-temperature deformation of dunite, eclogite, clinopyroxenite and garnetite using in situ X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Farla, R.; Rosenthal, A.; Bollinger, C.; Petitgirard, S.; Guignard, J.; Miyajima, N.; Kawazoe, T.; Crichton, W. A.; Frost, D. J.

    2017-09-01

    The rheology of eclogite, garnetite and clinopyroxenite in the peridotitic upper mantle was experimentally investigated in a large volume press combined with in situ synchrotron X-ray diffraction techniques to study the impact on mantle convection resulting from the subduction of oceanic lithosphere. Experiments were carried out over a range of constant strain rates (2 ×10-6- 3 ×10-5 s-1), pressures (4.3 to 6.7 GPa) and temperatures (1050 to 1470 K). Results show substantial strength variations among eclogitic garnet and clinopyroxene and peridotitic olivine. At low temperatures (<1200 K), eclogite is over 1 GPa stronger than dunite. On the other hand, at high temperatures (>1400 K) eclogite is weaker than dunite by 0.2 GPa or more. Garnetite and clinopyroxenite exhibit higher strength than dunite at approximately 1200 K. However, at higher temperature (1370 K), clinopyroxenite is significantly weaker than garnetite (and dunite) by more than a factor of five. We explain these observations by transitions in deformation mechanisms among the mineral phases. In clinopyroxene, high temperature dislocation creep resulting in a strength reduction replaces low temperature twinning. Whereas garnet remains very rigid at all experimental conditions when nominally anhydrous ('dry'). Microstructural observations show phase segregation of clinopyroxene and garnet, development of a crystallographic and shape preferred orientation in the former but not in the latter, suggesting an overall weak seismic anisotropy. Detection of eclogite bodies in the peridotite-dominated mantle may only be possible via observation of high VP /VS1 ratios. A comparable or weaker rheology of eclogite to dunite suggests effective stirring and mixing of eclogite in the convecting mantle.

  9. In situ high-temperature X-ray diffraction characterization of yttrium-implanted extra low-carbon steel

    SciTech Connect

    Caudron, E.; Buscail, H.; Perrier, S.

    1999-11-01

    Yttrium-implanted and unimplanted extra low-carbon steel samples were analyzed at T = 700 C and under an oxygen partial pressure P{sub O2} = 0.041Pa for 24 h to show the yttrium implantation effect on extra low-carbon steel high-temperature corrosion resistance. Sample oxidation weight gains were studied by thermogravimetry, and structural analyses were performed using in situ high-temperature X-ray diffraction with the same experimental conditions. The aim of this paper is to show the initial nucleation stage of the main compounds induced by oxidation at high temperatures according to the initial sample treatment (yttrium-implanted or unimplanted). The results obtained by in situ high-temperature X-ray diffraction will be compared to those by thermogravimetry to show the existing correlation between weight gain curves and structural studies. Results allow one to understand the improved corrosion resistance of yttrium-implanted extra low-carbon steel at high temperatures.

  10. A High Temperature Capacitive Pressure Sensor Based on Alumina Ceramic for in Situ Measurement at 600 °C

    PubMed Central

    Tan, Qiulin; Li, Chen; Xiong, Jijun; Jia, Pinggang; Zhang, Wendong; Liu, Jun; Xue, Chenyang; Hong, Yingping; Ren, Zhong; Luo, Tao

    2014-01-01

    In response to the growing demand for in situ measurement of pressure in high-temperature environments, a high temperature capacitive pressure sensor is presented in this paper. A high-temperature ceramic material-alumina is used for the fabrication of the sensor, and the prototype sensor consists of an inductance, a variable capacitance, and a sealed cavity integrated in the alumina ceramic substrate using a thick-film integrated technology. The experimental results show that the proposed sensor has stability at 850 °C for more than 20 min. The characterization in high-temperature and pressure environments successfully demonstrated sensing capabilities for pressure from 1 to 5 bar up to 600 °C, limited by the sensor test setup. At 600 °C, the sensor achieves a linear characteristic response, and the repeatability error, hysteresis error and zero-point drift of the sensor are 8.3%, 5.05% and 1%, respectively. PMID:24487624

  11. An in situ synchrotron XAS methodology for surface analysis under high temperature, pressure, and shear

    NASA Astrophysics Data System (ADS)

    Dorgham, A.; Neville, A.; Ignatyev, K.; Mosselmans, F.; Morina, A.

    2017-01-01

    The complex tribochemical nature of lubricated tribological contacts is inaccessible in real time without altering their initial state. To overcome this issue, a new design of a pin-on-disc tribological apparatus was developed and combined with synchrotron X-ray absorption spectroscopy (XAS). Using the designed apparatus, it is possible to study in situ the transient decomposition reactions of various oil additives on different surfaces under a wide range of realistic operating conditions of contact pressure (1.0-3.0 GPa), temperature (25-120 °C), and sliding speed (30-3000 rpm or 0.15-15 m/s). To test the apparatus, several tribological tests were performed at different shearing times ranging from 2.5 to 60 min. These tests were carried out under helium atmosphere at a temperature of 80 °C, contact pressure of 2.2 GPa, and sliding speed of 50 rpm. The XAS experiments indicate that the zinc dialkyldithiophosphate antiwear additive decomposes in the oil to form a tribofilm on the iron surface at different reaction kinetics from the ones of the thermal film. The tribofilm composition evolves much faster than the one of the thermal film, which confirms that the formation of the tribofilm is a thermally activated process similar to the one of the thermal film but accelerated by shear. Furthermore, the results indicate that the sulfur of the formed film, whether a tribofilm or a thermal film, appears initially in the form of sulfate, with some sulfide, which under heat or shear is reduced into mainly sulfide.

  12. An in situ synchrotron XAS methodology for surface analysis under high temperature, pressure, and shear.

    PubMed

    Dorgham, A; Neville, A; Ignatyev, K; Mosselmans, F; Morina, A

    2017-01-01

    The complex tribochemical nature of lubricated tribological contacts is inaccessible in real time without altering their initial state. To overcome this issue, a new design of a pin-on-disc tribological apparatus was developed and combined with synchrotron X-ray absorption spectroscopy (XAS). Using the designed apparatus, it is possible to study in situ the transient decomposition reactions of various oil additives on different surfaces under a wide range of realistic operating conditions of contact pressure (1.0-3.0 GPa), temperature (25-120 °C), and sliding speed (30-3000 rpm or 0.15-15 m/s). To test the apparatus, several tribological tests were performed at different shearing times ranging from 2.5 to 60 min. These tests were carried out under helium atmosphere at a temperature of 80  °C, contact pressure of 2.2 GPa, and sliding speed of 50 rpm. The XAS experiments indicate that the zinc dialkyldithiophosphate antiwear additive decomposes in the oil to form a tribofilm on the iron surface at different reaction kinetics from the ones of the thermal film. The tribofilm composition evolves much faster than the one of the thermal film, which confirms that the formation of the tribofilm is a thermally activated process similar to the one of the thermal film but accelerated by shear. Furthermore, the results indicate that the sulfur of the formed film, whether a tribofilm or a thermal film, appears initially in the form of sulfate, with some sulfide, which under heat or shear is reduced into mainly sulfide.

  13. In situ optical studies of methane and simulated biogas oxidation on high temperature solid oxide fuel cell anodes.

    PubMed

    Kirtley, John D; Steinhurst, Daniel A; Owrutsky, Jeffery C; Pomfret, Michael B; Walker, Robert A

    2014-01-07

    Novel integration of in situ near infrared (NIR) thermal imaging, vibrational Raman spectroscopy, and Fourier-transform infrared emission spectroscopy (FTIRES) coupled with traditional electrochemical measurements has been used to probe chemical and thermal properties of Ni-based, solid oxide fuel cell (SOFC) anodes operating with methane and simulated biogas fuel mixtures at 800 °C. Together, these three non-invasive optical techniques provide direct insight into the surface chemistry associated with device performance as a function of cell polarization. Specifically, data from these complementary methods measure with high spatial and temporal resolution thermal gradients and changes in material and gas phase composition in operando. NIR thermal images show that SOFC anodes operating with biogas undergo significant cooling (ΔT = -13 °C) relative to the same anodes operating with methane fuel (ΔT = -3 °C). This result is general regardless of cell polarization. Simultaneous Raman spectroscopic measurements are unable to detect carbon formation on anodes operating with biogas. Carbon deposition is observable during operation with methane as evidenced by a weak vibrational band at 1556 cm(-1). This feature is assigned to highly ordered graphite. In situ FTIRES corroborates these results by identifying relative amounts of CO2 and CO produced during electrochemical removal of anodic carbon previously formed from an incident fuel feed. Taken together, these three optical techniques illustrate the promise that complementary, in situ methods have for identifying electrochemical oxidation mechanisms and carbon-forming pathways in high temperature electrochemical devices.

  14. In situ characterization of catalysts and membranes in a microchannel under high-temperature water gas shift reaction conditions

    NASA Astrophysics Data System (ADS)

    Cavusoglu, G.; Dallmann, F.; Lichtenberg, H.; Goldbach, A.; Dittmeyer, R.; Grunwaldt, J.-D.

    2016-05-01

    Microreactor technology with high heat transfer in combination with stable catalysts is a very attractive approach for reactions involving major heat effects such as methane steam reforming and to some extent, also the high temperature water gas shift (WGS) reaction. For this study Rh/ceria catalysts and an ultrathin hydrogen selective membrane were characterized in situ in a microreactor specially designed for x-ray absorption spectroscopic measurements under WGS conditions. The results of these experiments can serve as a basis for further development of the catalysts and membranes.

  15. In-situ Diffraction Study of Magnetite at Simultaneous High Pressure and High Temperature Using Synchrotron Radiation

    NASA Astrophysics Data System (ADS)

    Wang, L.; Zhang, J.; Wang, S.; Chen, H.; Zhao, Y.

    2014-12-01

    Magnetite intertwined with the evolution of human civilizations, and remains so today. It is technologically and scientifically important by virtue of its unique magnetic and electrical properties. Magnetite is a common mineral found in a variety of geologic environments, and plays an important role in deciphering the oxygen evolution in the Earth's atmosphere and its deep interiors. The latter application asks for the knowledge of the thermal and elastic properties of magnetite at high pressures and temperatures, which is currently not available in literature. We have carried out a few in-situ diffraction experiments on magnetite using white synchrotron radiation at beamline X17B2 of National Synchrotron Light Source (NSLS). A DIA module in an 1100-ton press and WC anvils were employed for compression, and diffraction spectra were collected at simultaneous high pressures (P) and temperatures (T) (up to 9 GPa and 900 oC). Mixture of amorphous boron and epoxy resin was used as pressure medium, and NaCl as pressure marker. Temperature was recorded by W-Re thermocouples. Commercially purchased magnetite powder and a mixture of the said powder and NaCl (1:1) were used as starting material in separate experiments. Preliminary data analyses have yielded following observations: (1) Charge disordering seen at ambient pressure remains active in current experiments, especially at lower pressures (< 6 GPa); (2) Though at each condition potentially complicated by charge disordering process, isothermal compression curves remains simple and reproducible; (3) During cooling, the reversibility and degree of cation disordering depend on the starting material and/or experimental P-T path; and (4) cation disordering notably reduces the apparent bulk moduli of magnetite.

  16. Construction and in-situ characterisation of high-temperature fixed point cells devoted to industrial applications

    NASA Astrophysics Data System (ADS)

    Sadli, Mohamed; Bourson, Frédéric; Diril, Ahmet; Journeau, Christophe; Lowe, Dave; Parga, Clemente

    2014-08-01

    Among the activities of the European Metrology Research Programme (EMRP) project HiTeMS one work package is devoted to the development and testing of industrial solutions for long-standing temperature measurement problems at the highest temperatures. LNE-Cnam, NPL, TUBITAK-UME have worked on the design of high temperature fixed points (HTFP) suitable for in-situ temperature monitoring to be implemented in the facilities of CEA (Commissariat à l'énergie atomique et aux énergies alternatives). Several high temperature fixed point cells were constructed in these three national metrology institutes (NMIs) using a rugged version of cells based on the hybrid design of the laboratory HTFP developed and continuously improved at LNE-Cnam during the last years. The fixed points of interest were Co-C, Ru-C and Re-C corresponding to melting temperatures of 1324 °C, 1953 °C and 2474 °C respectively. The cells were characterised at the NMIs after their construction. Having proved robust enough, they were transported to CEA and tested in an induction furnace and cycled from room temperature to temperatures much above the melting temperatures (> +400 °C) with extremely high heating and cooling rates (up to 10 000 K/h). All the cells withstood the tests and the melting plateaus could be observed in all cases.

  17. In Situ Neutron Diffraction Study of NiTi-21Pt High-Temperature Shape Memory Alloys

    NASA Astrophysics Data System (ADS)

    Benafan, O.; Gaydosh, D. J.; Noebe, R. D.; Qiu, S.; Vaidyanathan, R.

    2016-12-01

    In situ neutron diffraction was used to investigate the microstructural features of stoichiometric and Ti-rich NiTiPt high-temperature shape memory alloys with target compositions of Ni29Ti50Pt21 and Ni28.5Ti50.5Pt21 (in atomic percent), respectively. The alloys' isothermal and thermomechanical properties (i.e., moduli, thermal expansion, transformation strains, and dimensional stability) were correlated to the lattice strains, volume-averaged elastic moduli, and textures as determined by neutron diffraction. In addition, the unique aspects of this technique when applied to martensitic transformations in shape memory alloys are highlighted throughout the paper.

  18. In situ observation of partial melting in superplastic aluminum alloy composites at high temperature

    SciTech Connect

    Koike, J. . Dept. of Mechanical Engineering); Mabuchi, M. ); Higashi, K. . Dept. of Mechanical Systems Engineering)

    1995-01-01

    The possibility of partial melting and its relations to the superplasticity at high strain rates were studied with transmission electron microscopy and differential scanning calorimetry in Al-Cu-Mg(2124), Al-Mg (5052), and Al-Mg-Si (6061) alloys reinforced with Si[sub 3]N[sub 4] particles. Calorimetry measurements of all three composites showed a sharp endothermic peak at an optimum superplastic temperature. At the same temperature, transmission electron microscopy showed the melting of grain boundaries and interfaces, suggesting direct correlations between partial melting and the superplasticity. Solute segregation was also observed at boundaries and interfaces, and was discussed as causes for partial melting.

  19. In-situ Phase Transformation and Deformation of Iron at High Pressure andTemperature

    SciTech Connect

    Miyagi, Lowell; Kunz, Martin; Knight, Jason; Nasiatka, James; Voltolini, Marco; Wenk, Hans-Rudolf

    2008-07-01

    With a membrane based mechanism to allow for pressure change of a sample in aradial diffraction diamond anvil cell (rDAC) and simultaneous infra-red laser heating, itis now possible to investigate texture changes during deformation and phasetransformations over a wide range of temperature-pressure conditions. The device isused to study bcc (alpha), fcc (gamma) and hcp (epislon) iron. In bcc iron, room temperature compression generates a texture characterized by (100) and (111) poles parallel to the compression direction. During the deformation induced phase transformation to hcp iron, a subset of orientations are favored to transform to the hcp structure first and generate a texture of (01-10) at high angles to the compression direction. Upon further deformation, the remaining grains transform, resulting in a texture that obeys the Burgers relationship of (110)bcc // (0001)hcp. This is in contrast to high temperature results that indicate that texture is developed through dominant pyramidal {2-1-12}<2-1-13> and basal (0001)-{2-1-10} slip based on polycrystal plasticity modeling. We also observe that the high temperature fcc phase develops a 110 texture typical for fcc metals deformed in compression.

  20. In-Situ Observation of Crystallization and Growth in High-Temperature Melts Using the Confocal Laser Microscope

    NASA Astrophysics Data System (ADS)

    Sohn, Il; Dippenaar, Rian

    2016-08-01

    This review discusses the innovative efforts initiated by Emi and co-workers for in-situ observation of phase transformations at high temperatures for materials. By using the high-temperature confocal laser-scanning microscope (CLSM), a robust database of the phase transformation behavior during heating and cooling of slags, fluxes, and steel can be developed. The rate of solidification and the progression of solid-state phase transformations can be readily investigated under a variety of atmospheric conditions and be correlated with theoretical predictions. The various research efforts following the work of Emi and co-workers have allowed a deeper fundamental understanding of the elusive solidification and phase transformation mechanisms in materials beyond the ambit of steels. This technique continues to evolve in terms of its methodology, application to other materials, and its contribution to technology.

  1. In-situ Formation of Reinforcement Phases in Ultra High Temperature Ceramic Composites

    NASA Technical Reports Server (NTRS)

    Stackpoole, Margaret M (Inventor); Gasch, Matthew J (Inventor); Olson, Michael W (Inventor); Hamby, Ian W. (Inventor); Johnson, Sylvia M (Inventor)

    2013-01-01

    A tough ultra-high temperature ceramic (UHTC) composite comprises grains of UHTC matrix material, such as HfB.sub.2, ZrB.sub.2 or other metal boride, carbide, nitride, etc., surrounded by a uniform distribution of acicular high aspect ratio reinforcement ceramic rods or whiskers, such as of SiC, is formed from uniformly mixing a powder of the UHTC material and a pre-ceramic polymer selected to form the desired reinforcement species, then thermally consolidating the mixture by hot pressing. The acicular reinforcement rods may make up from 5 to 30 vol % of the resulting microstructure.

  2. Thin film thermocouples for in situ membrane electrode assembly temperature measurements in a polybenzimidazole-based high temperature proton exchange membrane unit cell

    NASA Astrophysics Data System (ADS)

    Ali, Syed Talat; Lebæk, Jesper; Nielsen, Lars Pleth; Mathiasen, Claus; Møller, Per; Kær, Søren Knudsen

    This paper presents Type-T thin film thermocouples (TFTCs) fabricated on Kapton (polyimide) substrate for measuring the internal temperature of PBI (polybenzimidazole)-based high temperature proton exchange membrane fuel cell (HT-PEMFC). Magnetron sputtering technique was employed to deposit a 2 μm thick layer of TFTCs on 75 μm thick Kapton foil. The Kapton foil was treated with in situ argon plasma etching to improve the adhesion between TFTCs and the Kapton substrate. The TFTCs were covered with a 7 μm liquid Kapton layer using spin coating technique to protect them from environmental degradation. This Kapton foil with deposited TFTCs was used as sealing inside a PBI (polybenzimidazole)-based single cell test rig, which enabled measurements of in situ temperature variations of the working fuel cell MEA. The performance of the TFTCs was promising with minimal interference to the operation of the fuel cell.

  3. In Situ Determination of the NiAs Phase of FeO at High Pressure and Temperature.

    PubMed

    Fei, Y; Mao, H K

    1994-12-09

    In situ synchrotron x-ray diffraction measurements of FeO at high pressures and high temperatures revealed that the high-pressure phase of FeO has the NiAs structure (B8). The lattice parameters of this NiAs phase at 96 gigapascals and 800 kelvin are a = 2.574(2) angstroms and c = 5.172(4) angstroms (the number in parentheses is the error in the last digit). Metallic behavior of the high-pressure phase is consistent with a covalently and metallically bonded NiAs structure of FeO. Transition to the NiAs structure of FeO would enhance oxygen solubility in molten iron. This transition thus provides a physiochemical basis for the incorporation of oxygen into the Earth's core.

  4. High-Temperature Phase Equilibria of Duplex Stainless Steels Assessed with a Novel In-Situ Neutron Scattering Approach

    NASA Astrophysics Data System (ADS)

    Pettersson, Niklas; Wessman, Sten; Hertzman, Staffan; Studer, Andrew

    2017-04-01

    Duplex stainless steels are designed to solidify with ferrite as the parent phase, with subsequent austenite formation occurring in the solid state, implying that, thermodynamically, a fully ferritic range should exist at high temperatures. However, computational thermodynamic tools appear currently to overestimate the austenite stability of these systems, and contradictory data exist in the literature. In the present work, the high-temperature phase equilibria of four commercial duplex stainless steel grades, denoted 2304, 2101, 2507, and 3207, with varying alloying levels were assessed by measurements of the austenite-to-ferrite transformation at temperatures approaching 1673 K (1400 °C) using a novel in-situ neutron scattering approach. All grades became fully ferritic at some point during progressive heating. Higher austenite dissolution temperatures were measured for the higher alloyed grades, and for 3207, the temperature range for a single-phase ferritic structure approached zero. The influence of temperatures in the region of austenite dissolution was further evaluated by microstructural characterization using electron backscattered diffraction of isothermally heat-treated and quenched samples. The new experimental data are compared to thermodynamic calculations, and the precision of databases is discussed.

  5. High-Temperature Phase Equilibria of Duplex Stainless Steels Assessed with a Novel In-Situ Neutron Scattering Approach

    NASA Astrophysics Data System (ADS)

    Pettersson, Niklas; Wessman, Sten; Hertzman, Staffan; Studer, Andrew

    2017-01-01

    Duplex stainless steels are designed to solidify with ferrite as the parent phase, with subsequent austenite formation occurring in the solid state, implying that, thermodynamically, a fully ferritic range should exist at high temperatures. However, computational thermodynamic tools appear currently to overestimate the austenite stability of these systems, and contradictory data exist in the literature. In the present work, the high-temperature phase equilibria of four commercial duplex stainless steel grades, denoted 2304, 2101, 2507, and 3207, with varying alloying levels were assessed by measurements of the austenite-to-ferrite transformation at temperatures approaching 1673 K (1400 °C) using a novel in-situ neutron scattering approach. All grades became fully ferritic at some point during progressive heating. Higher austenite dissolution temperatures were measured for the higher alloyed grades, and for 3207, the temperature range for a single-phase ferritic structure approached zero. The influence of temperatures in the region of austenite dissolution was further evaluated by microstructural characterization using electron backscattered diffraction of isothermally heat-treated and quenched samples. The new experimental data are compared to thermodynamic calculations, and the precision of databases is discussed.

  6. In Situ Synthesis of Uranium Carbide and its High Temperature Cubic Phase

    SciTech Connect

    Reiche, Helmut Matthias; Vogel, Sven C.

    2015-03-25

    New in situ data for the U-C system are presented, with the goal of improving knowledge of the phase diagram to enable production of new ceramic fuels. The none quenchable, cubic, δ-phase, which in turn is fundamental to computational methods, was identified. Rich datasets of the formation synthesis of uranium carbide yield kinetics data which allow the benchmarking of modeling, thermodynamic parameters etc. The order-disorder transition (carbon sublattice melting) was observed due to equal sensitivity of neutrons to both elements. This dynamic has not been accurately described in some recent simulation-based publications.

  7. Delayed in situ crosslinking of acrylamide polymers for oil recovery applications in high-temperature formations

    SciTech Connect

    Sydansk, R.D.

    1989-07-04

    This patent describes a process for plugging a region of a high-temperature hydrocarbon-bearing formation below an earthen surface with a cross-linked acrylamide polymer gel wherein the formation is penetrated by a wellbore in communication with the region. The process comprising: admixing a gelation system at the earthen surface comprising an aqueous solvent, an unhydrolyzed acrylamide polymer made up of monomeric groups, and a polyvalent metal crosslinking agent. Wherein less than about 1.0 mole percent of the monomeric groups in the unhydrolyzed acrylamide polymer contain a carboxylate constituent based on the total number of the monomeric groups in the polymer. Wherein the polyvalent metal crosslinking agent is a salt or a complex of a trivalent or quatravalent metal cation capable of crosslinking a partially hydrolyzed acrylamide polymer; injecting the gelation system into the treatment region of the formation wherein the formation has a temperature of at least about 60{sup 0}C, hydrolyzing the polymer in the region at the formation temperature such that more than about 1.0 mole percent of the monomeric groups in the polymer contain a carboxylate constituent based on the total number of the monomeric groups in the polymer; and crosslinking the gelation system in the region to substantial completion to form the continuous immobile crosslinked acrylamide polymer gel which plugs at least a portion of the treatment region.

  8. In situ Raman spectroscopic analysis of surface oxide films on Ni-base alloy/low alloy steel dissimilar metal weld interfaces in high-temperature water

    NASA Astrophysics Data System (ADS)

    Kim, Jongjin; Choi, Kyung Joon; Bahn, Chi Bum; Kim, Ji Hyun

    2014-06-01

    In situ Raman spectroscopy has been applied to analyze the surface oxide films formed on dissimilar metal weld (DMW) interfaces of nickel-base alloy/low alloy steel under hydrogenated high-temperature water condition. For the analysis of the oxide films under high temperature/pressure aqueous conditions, an in situ Raman spectroscopy system was developed by constructing a hydrothermal cell where the entire optics including the excitation laser and the Raman light collection system were located at the nearest position to the specimen by means of immersion optics. In situ Raman spectra of the DMW interfaces were collected in hydrogenated water condition at different temperatures up to 300 °C. The measured in situ Raman spectra showed peaks of Cr2O3, NiCr2O4 and Fe3O4 at the DMW interface. It is considered that differences in the oxide chemistry originated from the chemical element distribution inside of the DMW interface region.

  9. Double-wall TiO2 nanotube arrays: enhanced photocatalytic activity and in situ TEM observations at high temperature.

    PubMed

    Xue, Chaorui; Narushima, Takashi; Ishida, Yohei; Tokunaga, Tomoharu; Yonezawa, Tetsu

    2014-11-26

    By decreasing the water content in an NH4F and glycerol-water electrolyte, the transition from single-wall to double-wall TiO2 nanotube arrays was successfully achieved using an anodization method. The double-wall TiO2 nanotube structures exhibited better photocatalytic activity than the typical single-wall structures. After modification with platinum nanoparticles, the photocatalytic activity of both the single- and double-wall TiO2 nanotubes was improved further. In situ observations at the annealing temperature of the TiO2 nanotubes were performed using a transmission electron microscopy (TEM) system. A slower structural failure of the nanotubes was obtained with the introduction of oxygen gas into the TEM column compared with the structural changes observed under high-vacuum conditions without the introduction of oxygen gas. These behaviors suggest that oxygen injection is an important factor in stabilizing the TiO2 nanotubes during the in situ TEM annealing process. The high-magnification TEM images of the double-wall TiO2 nanotubes revealed that the sintering of the inner wall can draw a clear distinction between the inner and outer walls.

  10. In-situ X-ray structure measurements on aerodynamically levitated high temperature liquids

    SciTech Connect

    Weber, Richard; Benmore, Christopher; Mei Qiang; Wilding, Martin

    2009-01-29

    High energy, high flux X-ray sources enable new measurements of liquid and amorphous materials in extreme conditions. Aerodynamic levitation in combination with laser beam heating can be used to access high purity and non-equilibrium liquids at temperatures up to 3000 K. In this work, a small aerodynamic levitator was integrated with high energy beamline 11 ID-C at the Advanced Photon Source. Scattered X-rays were detected with a Mar345 image plate. The experiments investigated a series of binary in the CaO-Al{sub 2}O{sub 3}, MgO-SiO{sub 2}, SiO{sub 2}-Al{sub 2}O{sub 3} metal oxide compositions and pure SiO{sub 2}. The results show that the liquids exhibit large changes in structure when the predominant network former is diluted. Measurements on glasses with the same compositions as the liquids suggest that significant structural rearrangement consistent with a fragile-strong transition occurs in these reluctant glass forming liquids as they vitrify.

  11. In situ studies of materials for high temperature CO2 capture and storage.

    PubMed

    Dunstan, Matthew T; Maugeri, Serena A; Liu, Wen; Tucker, Matthew G; Taiwo, Oluwadamilola O; Gonzalez, Belen; Allan, Phoebe K; Gaultois, Michael W; Shearing, Paul R; Keen, David A; Phillips, Anthony E; Dove, Martin T; Scott, Stuart A; Dennis, John S; Grey, Clare P

    2016-10-20

    Carbon capture and storage (CCS) offers a possible solution to curb the CO2 emissions from stationary sources in the coming decades, considering the delays in shifting energy generation to carbon neutral sources such as wind, solar and biomass. The most mature technology for post-combustion capture uses a liquid sorbent, amine scrubbing. However, with the existing technology, a large amount of heat is required for the regeneration of the liquid sorbent, which introduces a substantial energy penalty. The use of alternative sorbents for CO2 capture, such as the CaO-CaCO3 system, has been investigated extensively in recent years. However there are significant problems associated with the use of CaO based sorbents, the most challenging one being the deactivation of the sorbent material. When sorbents such as natural limestone are used, the capture capacity of the solid sorbent can fall by as much as 90 mol% after the first 20 carbonation-regeneration cycles. In this study a variety of techniques were employed to understand better the cause of this deterioration from both a structural and morphological standpoint. X-ray and neutron PDF studies were employed to understand better the local surface and interfacial structures formed upon reaction, finding that after carbonation the surface roughness is decreased for CaO. In situ synchrotron X-ray diffraction studies showed that carbonation with added steam leads to a faster and more complete conversion of CaO than under conditions without steam, as evidenced by the phases seen at different depths within the sample. Finally, in situ X-ray tomography experiments were employed to track the morphological changes in the sorbents during carbonation, observing directly the reduction in porosity and increase in tortuosity of the pore network over multiple calcination reactions.

  12. Effect of In-Situ Cure on Measurement of Glass Transition Temperatures in High-Temperature Thermosetting Polymers (Briefing Charts)

    DTIC Science & Technology

    2015-05-20

    TEMPERATURES IN HIGH-TEMPERATURE THERMOSETTING POLYMERS 5a. CONTRACT NUMBER In-House 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) 5d...temperature thermosetting polymer via dynamic mechanical analysis alone. These difficulties result from the residual cure of samples heated beyond their... Polymers Andrew J. Guenthner,1 Josiah T. Reams,2 Michael D. Ford2, Kevin R. Lamison,2 Joseph M. Mabry1 2 Outline: The Effects of “Frozen” Chemistry

  13. In-Situ X-Ray Diffraction Observations of Low Temperature Ag-Nanoink Sintering and High Temperature Eutectic Reaction with Copper

    SciTech Connect

    Elmer, J. W.; Specht, Eliot D

    2012-01-01

    Nanoinks, which contain nm sized metallic particles suspended in an organic dispersant fluid, are finding numerous microelectronic applications. Nanoinks sinter at much lower temperatures than bulk metals due to their high surface area to volume ratio and small radius of curvature, which reduces their melting points significantly below their bulk values. The unusually low melting and sintering temperatures have unique potential for materials joining since their melting points increase dramatically after initial sintering. In this paper Ag nanoink is studied using in-situ synchrotron based x-ray diffraction to follow the kinetics of the initial sintering step by analysis of diffraction patterns, and to directly observe the high remelt temperature of sintered nanoinks. Ag nanoink is further explored as a possible eutectic bonding medium with copper by tracking phase transformations to high temperatures where melting occurs at the Ag-Cu eutectic temperature, demonstrating nanoinks as a viable eutectic bonding medium.

  14. Effects of High-Temperature Stress on Various Biomembranes of Leaf Cells In Situ and In Vitro

    PubMed Central

    Thebud, Regina; Santarius, Kurt A.

    1982-01-01

    The sensitivity of photosynthetic and respiratory functions to supraoptimal temperature stress was compared after heating of leaves, protoplasts and membrane systems of spinach (Spinacia oleracea L. cv. Monatol) and lettuce (Valerianella locusta [L.] Betcke) in situ and in vitro. After heating of whole leaves or protoplasts, endogenous respiration was not or only slightly affected at temperatures which caused a marked decrease of photosynthesis. This was manifested when mitochondria and thylakoids were isolated from heat-treated leaves. In the presence of exogenous substrates, mitochondrial electron transport and phosphorylation were even somewhat stimulated compared to the controls. Inactivation of net CO2 uptake of whole leaves following heat stress and of the photochemical activities of chloroplast membranes isolated from heat-treated leaves of the same origin occurred nearly simultaneously. In protoplasts, photosynthesis was inactivated at temperatures far below those which caused drastic changes in the integrity of the tonoplast and the plasmalemma. This indicates that damage occurring within the chloroplasts rather than alterations in the compartmentation of the cell is responsible for the high sensitivity of photosynthesis to supraoptimal temperature stress. Mitochondria and thykaloids isolated from the same preparation of intact leaves under comparable conditions and subjected to heat treatment in vitro, however, were inactivated nearly in the same temperature range. Thus, mitochondria are much more stable within their cytoplasmic environment. PMID:16662445

  15. Long-term, high frequency in situ measurements of intertidal mussel bed temperatures using biomimetic sensors.

    PubMed

    Helmuth, Brian; Choi, Francis; Matzelle, Allison; Torossian, Jessica L; Morello, Scott L; Mislan, K A S; Yamane, Lauren; Strickland, Denise; Szathmary, P Lauren; Gilman, Sarah E; Tockstein, Alyson; Hilbish, Thomas J; Burrows, Michael T; Power, Anne Marie; Gosling, Elizabeth; Mieszkowska, Nova; Harley, Christopher D G; Nishizaki, Michael; Carrington, Emily; Menge, Bruce; Petes, Laura; Foley, Melissa M; Johnson, Angela; Poole, Megan; Noble, Mae M; Richmond, Erin L; Robart, Matt; Robinson, Jonathan; Sapp, Jerod; Sones, Jackie; Broitman, Bernardo R; Denny, Mark W; Mach, Katharine J; Miller, Luke P; O'Donnell, Michael; Ross, Philip; Hofmann, Gretchen E; Zippay, Mackenzie; Blanchette, Carol; Macfarlan, J A; Carpizo-Ituarte, Eugenio; Ruttenberg, Benjamin; Peña Mejía, Carlos E; McQuaid, Christopher D; Lathlean, Justin; Monaco, Cristián J; Nicastro, Katy R; Zardi, Gerardo

    2016-10-11

    At a proximal level, the physiological impacts of global climate change on ectothermic organisms are manifest as changes in body temperatures. Especially for plants and animals exposed to direct solar radiation, body temperatures can be substantially different from air temperatures. We deployed biomimetic sensors that approximate the thermal characteristics of intertidal mussels at 71 sites worldwide, from 1998-present. Loggers recorded temperatures at 10-30 min intervals nearly continuously at multiple intertidal elevations. Comparisons against direct measurements of mussel tissue temperature indicated errors of ~2.0-2.5 °C, during daily fluctuations that often exceeded 15°-20 °C. Geographic patterns in thermal stress based on biomimetic logger measurements were generally far more complex than anticipated based only on 'habitat-level' measurements of air or sea surface temperature. This unique data set provides an opportunity to link physiological measurements with spatially- and temporally-explicit field observations of body temperature.

  16. Long-term, high frequency in situ measurements of intertidal mussel bed temperatures using biomimetic sensors

    NASA Astrophysics Data System (ADS)

    Helmuth, Brian; Choi, Francis; Matzelle, Allison; Torossian, Jessica L.; Morello, Scott L.; Mislan, K. A. S.; Yamane, Lauren; Strickland, Denise; Szathmary, P. Lauren; Gilman, Sarah E.; Tockstein, Alyson; Hilbish, Thomas J.; Burrows, Michael T.; Power, Anne Marie; Gosling, Elizabeth; Mieszkowska, Nova; Harley, Christopher D. G.; Nishizaki, Michael; Carrington, Emily; Menge, Bruce; Petes, Laura; Foley, Melissa M.; Johnson, Angela; Poole, Megan; Noble, Mae M.; Richmond, Erin L.; Robart, Matt; Robinson, Jonathan; Sapp, Jerod; Sones, Jackie; Broitman, Bernardo R.; Denny, Mark W.; Mach, Katharine J.; Miller, Luke P.; O'Donnell, Michael; Ross, Philip; Hofmann, Gretchen E.; Zippay, Mackenzie; Blanchette, Carol; Macfarlan, J. A.; Carpizo-Ituarte, Eugenio; Ruttenberg, Benjamin; Peña Mejía, Carlos E.; McQuaid, Christopher D.; Lathlean, Justin; Monaco, Cristián J.; Nicastro, Katy R.; Zardi, Gerardo

    2016-10-01

    At a proximal level, the physiological impacts of global climate change on ectothermic organisms are manifest as changes in body temperatures. Especially for plants and animals exposed to direct solar radiation, body temperatures can be substantially different from air temperatures. We deployed biomimetic sensors that approximate the thermal characteristics of intertidal mussels at 71 sites worldwide, from 1998-present. Loggers recorded temperatures at 10-30 min intervals nearly continuously at multiple intertidal elevations. Comparisons against direct measurements of mussel tissue temperature indicated errors of ~2.0-2.5 °C, during daily fluctuations that often exceeded 15°-20 °C. Geographic patterns in thermal stress based on biomimetic logger measurements were generally far more complex than anticipated based only on ‘habitat-level’ measurements of air or sea surface temperature. This unique data set provides an opportunity to link physiological measurements with spatially- and temporally-explicit field observations of body temperature.

  17. Real-time in situ probing of high-temperature quantum dots solution synthesis.

    PubMed

    Abécassis, Benjamin; Bouet, Cécile; Garnero, Cyril; Constantin, Doru; Lequeux, Nicolas; Ithurria, Sandrine; Dubertret, Benoit; Pauw, Brian Richard; Pontoni, Diego

    2015-04-08

    Understanding the formation mechanism of colloidal nanocrystals is of paramount importance in order to design new nanostructures and synthesize them in a predictive fashion. However, reliable data on the pathways leading from molecular precursors to nanocrystals are not available yet. We used synchrotron-based time-resolved in situ small and wide-angle X-ray scattering to experimentally monitor the formation of CdSe quantum dots synthesized in solution through the heating up of precursors in octadecene at 240 °C. Our experiment yields a complete movie of the structure of the solution from the self-assembly of the precursors to the formation of the quantum dots. We show that the initial cadmium precursor lamellar structure melts into small micelles at 100 °C and that the first CdSe nuclei appear at 218.7 °C. The size distributions and concentration in nanocrystals are measured in a quantitative fashion as a function of time. We show that a short nucleation burst lasting 30 s is followed by a slow decrease of nanoparticle concentration. The rate-limiting process of the quantum dot formation is found to be the thermal activation of selenium.

  18. Chromium Reaction Mechanisms for Speciation using Synchrotron in-Situ High-Temperature X-ray Diffraction.

    PubMed

    Low, Fiona; Kimpton, Justin; Wilson, Siobhan A; Zhang, Lian

    2015-07-07

    We use in situ high-temperature X-ray diffraction (HT-XRD), ex-situ XRD and synchrotron X-ray absorption near edge structure spectroscopy (XANES) to derive fundamental insights into mechanisms of chromium oxidation during combustion of solid fuels. To mimic the real combustion environment, mixtures of pure eskolaite (Cr(3+)2O3), lime (CaO) and/or kaolinite [Al2Si2O5(OH)4] have been annealed at 600-1200 °C in air versus 1% O2 diluted by N2. Our results confirm for the first time that (1) the optimum temperature for Cr(6+) formation is 800 °C for the coexistence of lime and eskolaite; (2) upon addition of kaolinite into oxide mixture, the temperature required to produce chromatite shifts to 1000 °C with a remarkable reduction in the fraction of Cr(6+). Beyond 1000 °C, transient phases are formed that bear Cr in intermediate valence states, which convert to different species other than Cr(6+) in the cooling stage; (3) of significance to Cr mobility from the waste products generated by combustion, chromatite formed at >1000 °C has a glassy disposition that prevents its water-based leaching; and (4) Increasing temperature facilitates the migration of eskolaite particles into bulk lime and enhances the extent to which Cr(3+) is oxidized, thereby completing the oxidation of Cr(3+) to Cr(6+) within 10 min.

  19. Long-term, high frequency in situ measurements of intertidal mussel bed temperatures using biomimetic sensors

    PubMed Central

    Helmuth, Brian; Choi, Francis; Matzelle, Allison; Torossian, Jessica L.; Morello, Scott L.; Mislan, K.A.S.; Yamane, Lauren; Strickland, Denise; Szathmary, P. Lauren; Gilman, Sarah E.; Tockstein, Alyson; Hilbish, Thomas J.; Burrows, Michael T.; Power, Anne Marie; Gosling, Elizabeth; Mieszkowska, Nova; Harley, Christopher D.G.; Nishizaki, Michael; Carrington, Emily; Menge, Bruce; Petes, Laura; Foley, Melissa M.; Johnson, Angela; Poole, Megan; Noble, Mae M.; Richmond, Erin L.; Robart, Matt; Robinson, Jonathan; Sapp, Jerod; Sones, Jackie; Broitman, Bernardo R.; Denny, Mark W.; Mach, Katharine J.; Miller, Luke P.; O’Donnell, Michael; Ross, Philip; Hofmann, Gretchen E.; Zippay, Mackenzie; Blanchette, Carol; Macfarlan, J.A.; Carpizo-Ituarte, Eugenio; Ruttenberg, Benjamin; Peña Mejía, Carlos E.; McQuaid, Christopher D.; Lathlean, Justin; Monaco, Cristián J.; Nicastro, Katy R.; Zardi, Gerardo

    2016-01-01

    At a proximal level, the physiological impacts of global climate change on ectothermic organisms are manifest as changes in body temperatures. Especially for plants and animals exposed to direct solar radiation, body temperatures can be substantially different from air temperatures. We deployed biomimetic sensors that approximate the thermal characteristics of intertidal mussels at 71 sites worldwide, from 1998-present. Loggers recorded temperatures at 10–30 min intervals nearly continuously at multiple intertidal elevations. Comparisons against direct measurements of mussel tissue temperature indicated errors of ~2.0–2.5 °C, during daily fluctuations that often exceeded 15°–20 °C. Geographic patterns in thermal stress based on biomimetic logger measurements were generally far more complex than anticipated based only on ‘habitat-level’ measurements of air or sea surface temperature. This unique data set provides an opportunity to link physiological measurements with spatially- and temporally-explicit field observations of body temperature. PMID:27727238

  20. High Temperature Fabrication of Nanostructured Yttria-Stabilized-Zirconia (YSZ) Scaffolds by In Situ Carbon Templating Xerogels.

    PubMed

    Muhoza, Sixbert P; Cottam, Matthew A; Gross, Michael D

    2017-04-16

    We demonstrate a method for the high temperature fabrication of porous, nanostructured yttria-stabilized-zirconia (YSZ, 8 mol% yttria - 92 mol% zirconia) scaffolds with tunable specific surface areas up to 80 m(2)·g(-1). An aqueous solution of a zirconium salt, yttrium salt, and glucose is mixed with propylene oxide (PO) to form a gel. The gel is dried under ambient conditions to form a xerogel. The xerogel is pressed into pellets and then sintered in an argon atmosphere. During sintering, a YSZ ceramic phase forms and the organic components decompose, leaving behind amorphous carbon. The carbon formed in situ serves as a hard template, preserving a high surface area YSZ nanomorphology at sintering temperature. The carbon is subsequently removed by oxidation in air at low temperature, resulting in a porous, nanostructured YSZ scaffold. The concentration of the carbon template and the final scaffold surface area can be systematically tuned by varying the glucose concentration in the gel synthesis. The carbon template concentration was quantified using thermogravimetric analysis (TGA), the surface area and pore size distribution was determined by physical adsorption measurements, and the morphology was characterized using scanning electron microscopy (SEM). Phase purity and crystallite size was determined using X-ray diffraction (XRD). This fabrication approach provides a novel, flexible platform for realizing unprecedented scaffold surface areas and nanomorphologies for ceramic-based electrochemical energy conversion applications, e.g. solid oxide fuel cell (SOFC) electrodes.

  1. Optical cell for combinatorial in situ Raman spectroscopic measurements of hydrogen storage materials at high pressures and temperatures.

    PubMed

    Hattrick-Simpers, Jason R; Hurst, Wilbur S; Srinivasan, Sesha S; Maslar, James E

    2011-03-01

    An optical cell is described for high-throughput backscattering Raman spectroscopic measurements of hydrogen storage materials at pressures up to 10 MPa and temperatures up to 823 K. High throughput is obtained by employing a 60 mm diameter × 9 mm thick sapphire window, with a corresponding 50 mm diameter unobstructed optical aperture. To reproducibly seal this relatively large window to the cell body at elevated temperatures and pressures, a gold o-ring is employed. The sample holder-to-window distance is adjustable, making this cell design compatible with optical measurement systems incorporating lenses of significantly different focal lengths, e.g., microscope objectives and single element lenses. For combinatorial investigations, up to 19 individual powder samples can be loaded into the optical cell at one time. This cell design is also compatible with thin-film samples. To demonstrate the capabilities of the cell, in situ measurements of the Ca(BH(4))(2) and nano-LiBH(4)-LiNH(2)-MgH(2) hydrogen storage systems at elevated temperatures and pressures are reported.

  2. Optical cell for combinatorial in situ Raman spectroscopic measurements of hydrogen storage materials at high pressures and temperatures

    NASA Astrophysics Data System (ADS)

    Hattrick-Simpers, Jason R.; Hurst, Wilbur S.; Srinivasan, Sesha S.; Maslar, James E.

    2011-03-01

    An optical cell is described for high-throughput backscattering Raman spectroscopic measurements of hydrogen storage materials at pressures up to 10 MPa and temperatures up to 823 K. High throughput is obtained by employing a 60 mm diameter × 9 mm thick sapphire window, with a corresponding 50 mm diameter unobstructed optical aperture. To reproducibly seal this relatively large window to the cell body at elevated temperatures and pressures, a gold o-ring is employed. The sample holder-to-window distance is adjustable, making this cell design compatible with optical measurement systems incorporating lenses of significantly different focal lengths, e.g., microscope objectives and single element lenses. For combinatorial investigations, up to 19 individual powder samples can be loaded into the optical cell at one time. This cell design is also compatible with thin-film samples. To demonstrate the capabilities of the cell, in situ measurements of the Ca(BH4)2 and nano-LiBH4-LiNH2-MgH2 hydrogen storage systems at elevated temperatures and pressures are reported.

  3. Development of a new micro-furnace for "in situ" high-temperature single crystal X-ray diffraction measurements

    NASA Astrophysics Data System (ADS)

    Alvaro, Matteo; Angel, Ross J.; Marciano, Claudio; Zaffiro, Gabriele; Scandolo, Lorenzo; Mazzucchelli, Mattia L.; Milani, Sula; Rustioni, Greta; Domeneghetti, Chiara M.; Nestola, Fabrizio

    2015-04-01

    Several experimental methods to reliably determine elastic properties of minerals at non-ambient conditions have been developed. In particular, different techniques for generating high-pressure and high-temperature have been successfully adopted for single-crystal and powder X-ray diffraction measurements. High temperature devices for "in-situ" measurements should provide the most controlled isothermal environment as possible across the entire sample. It is intuitive that in general, thermal gradients across the sample increase as the temperature increases. Even if the small isothermal volume required for single-crystal X-ray diffraction experiments makes such phenomena almost negligible, the design of a furnace should also aim to reduce thermal gradients by including a large thermal mass that encloses the sample. However this solution often leads to complex design that results in a restricted access to reciprocal space or attenuation of the incident or diffracted intensity (with consequent reduction of the accuracy and/or precision in lattice parameter determination). Here we present a newly-developed H-shaped Pt-Pt/Rh resistance microfurnace for in-situ high-temperature single-crystal X-ray diffraction measurements. The compact design of the furnace together with the long collimator-sample-detector distance allows us to perform measurements up to 2θ = 70° with no further restrictions on any other angular movement. The microfurnace is equipped with a water cooling system that allows a constant thermal gradient to be maintained that in turn guarantees thermal stability with oscillations smaller than 5°C in the whole range of operating T of room-T to 1200°C. The furnace has been built for use with a conventional 4-circle Eulerian geometry equipped with point detector and automated with the SINGLE software (Angel and Finger 2011) that allows the effects of crystal offsets and diffractometer aberrations to be eliminated from the refined peak positions by the 8

  4. In situ high pressure and temperature carbon-13 nmr for the study of carbonation reactions of carbon dioxide

    NASA Astrophysics Data System (ADS)

    Surface, James Andrew

    The aqueous reactions of carbon dioxide with various Mg-containing minerals [MgO, Mg(OH)2, and Mg2SiO4] at several different pressures (1-200 bar) and temperatures (25-150C) have been studied using a novel, elevated pressure and temperature 13C NMR probe. Critical observations about reaction rates, chemical exchange, and pH measurements throughout these reactions and the implications of the in situ measurements made during these reactions are discussed. A new method is used to elucidate pH under high pressure and temperature conditions which utilizes a calculation scheme wherein experimental data and a computational model are combined. Additionally, a 1D pH imaging method is employed to observe pH gradient effects across mineral samples during their reaction with CO2. Finally, other experimental details are discussed including ex situ analysis on carbonate products using pXRD, Raman, and MAS NMR. Detailed discussion outlines how to use 13C NMR to study CO2 mineralization reactions.

  5. Development of self-powered wireless high temperature electrochemical sensor for in situ corrosion monitoring of coal-fired power plant.

    PubMed

    Aung, Naing Naing; Crowe, Edward; Liu, Xingbo

    2015-03-01

    Reliable wireless high temperature electrochemical sensor technology is needed to provide in situ corrosion information for optimal predictive maintenance to ensure a high level of operational effectiveness under the harsh conditions present in coal-fired power generation systems. This research highlights the effectiveness of our novel high temperature electrochemical sensor for in situ coal ash hot corrosion monitoring in combination with the application of wireless communication and an energy harvesting thermoelectric generator (TEG). This self-powered sensor demonstrates the successful wireless transmission of both corrosion potential and corrosion current signals to a simulated control room environment.

  6. Novel Modified Optical Fibers for High Temperature In-Situ Miniaturized Gas Sensors in Advanced Fossil Energy Systems

    SciTech Connect

    Pickrell, Gary; Scott, Brian

    2014-06-30

    This report covers the technical progress on the program “Novel Modified Optical Fibers for High Temperature In-Situ Miniaturized Gas Sensors in Advanced Fossil Energy Systems”, funded by the National Energy Technology Laboratory of the U.S. Department of Energy, and performed by the Materials Science & Engineering and Electrical & Computer Engineering Departments at Virginia Tech, and summarizes technical progress from July 1st, 2005 –June 30th, 2014. The objective of this program was to develop novel fiber materials for high temperature gas sensors based on evanescent wave absorption in optical fibers. This project focused on two primary areas: the study of a sapphire photonic crystal fiber (SPCF) for operation at high temperature and long wavelengths, and a porous glass based fiber optic sensor for gas detection. The sapphire component of the project focused on the development of a sapphire photonic crystal fiber, modeling of the new structures, fabrication of the optimal structure, development of a long wavelength interrogation system, testing of the optical properties, and gas and temperature testing of the final sensor. The fabrication of the 6 rod SPCF gap bundle (diameter of 70μm) with a hollow core was successfully constructed with lead-in and lead-out 50μm diameter fiber along with transmission and gas detection testing. Testing of the sapphire photonic crystal fiber sensor capabilities with the developed long wavelength optical system showed the ability to detect CO2 at or below 1000ppm at temperatures up to 1000°C. Work on the porous glass sensor focused on the development of a porous clad solid core optical fiber, a hollow core waveguide, gas detection capabilities at room and high temperature, simultaneous gas species detection, suitable joining technologies for the lead-in and lead-out fibers and the porous sensor, sensor system sensitivity improvement, signal processing improvement, relationship between pore structure and fiber

  7. Synchrotron X-ray micro-tomography at the Advanced Light Source: Developments in high-temperature in-situ mechanical testing

    NASA Astrophysics Data System (ADS)

    Barnard, Harold S.; MacDowell, A. A.; Parkinson, D. Y.; Mandal, P.; Czabaj, M.; Gao, Y.; Maillet, E.; Blank, B.; Larson, N. M.; Ritchie, R. O.; Gludovatz, B.; Acevedo, C.; Liu, D.

    2017-06-01

    At the Advanced Light Source (ALS), Beamline 8.3.2 performs hard X-ray micro-tomography under conditions of high temperature, pressure, mechanical loading, and other realistic conditions using environmental test cells. With scan times of 10s-100s of seconds, the microstructural evolution of materials can be directly observed over multiple time steps spanning prescribed changes in the sample environment. This capability enables in-situ quasi-static mechanical testing of materials. We present an overview of our in-situ mechanical testing capabilities and recent hardware developments that enable flexural testing at high temperature and in combination with acoustic emission analysis.

  8. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    DOE PAGES

    Weber, J. K. R.; Tamalonis, A.; Benmore, C. J.; ...

    2016-07-01

    We integrated an aerodynamic levitator with carbon dioxide laser beam heating with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. Furthermore, the chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The samplemore » environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. Our system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.« less

  9. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    SciTech Connect

    Weber, J. K. R.; Alderman, O. L. G.; Tamalonis, A.; Sendelbach, S.; Benmore, C. J.; Hebden, A.; Williamson, M. A.

    2016-07-15

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  10. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    SciTech Connect

    Weber, J. K. R.; Tamalonis, A.; Benmore, C. J.; Alderman, O. L. G.; Sendelbach, S.; Hebden, A.; Williamson, M. A.

    2016-07-01

    We integrated an aerodynamic levitator with carbon dioxide laser beam heating with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. Furthermore, the chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. Our system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  11. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    NASA Astrophysics Data System (ADS)

    Weber, J. K. R.; Tamalonis, A.; Benmore, C. J.; Alderman, O. L. G.; Sendelbach, S.; Hebden, A.; Williamson, M. A.

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  12. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials

    SciTech Connect

    Weber, J. K. R.; Tamalonis, A.; Benmore, C. J.; Alderman, O. L. G.; Sendelbach, S.; Hebden, A.; Williamson, M. A.

    2016-07-01

    We integrated an aerodynamic levitator with carbon dioxide laser beam heating with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. Furthermore, the chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. Our system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  13. Aerodynamic levitator for in situ x-ray structure measurements on high temperature and molten nuclear fuel materials.

    PubMed

    Weber, J K R; Tamalonis, A; Benmore, C J; Alderman, O L G; Sendelbach, S; Hebden, A; Williamson, M A

    2016-07-01

    An aerodynamic levitator with carbon dioxide laser beam heating was integrated with a hermetically sealed controlled atmosphere chamber and sample handling mechanism. The system enabled containment of radioactive samples and control of the process atmosphere chemistry. The chamber was typically operated at a pressure of approximately 0.9 bars to ensure containment of the materials being processed. Samples 2.5-3 mm in diameter were levitated in flowing gas to achieve containerless conditions. Levitated samples were heated to temperatures of up to 3500 °C with a partially focused carbon dioxide laser beam. Sample temperature was measured using an optical pyrometer. The sample environment was integrated with a high energy (100 keV) x-ray synchrotron beamline to enable in situ structure measurements to be made on levitated samples as they were heated, melted, and supercooled. The system was controlled from outside the x-ray beamline hutch by using a LabVIEW program. Measurements have been made on hot solid and molten uranium dioxide and binary uranium dioxide-zirconium dioxide compositions.

  14. In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays: High Resolution Imaging at Ambient Pressure and Elevated Temperature.

    PubMed

    Baier, Sina; Damsgaard, Christian D; Scholz, Maria; Benzi, Federico; Rochet, Amélie; Hoppe, Robert; Scherer, Torsten; Shi, Junjie; Wittstock, Arne; Weinhausen, Britta; Wagner, Jakob B; Schroer, Christian G; Grunwaldt, Jan-Dierk

    2016-02-01

    A new closed cell is presented for in situ X-ray ptychography which allows studies under gas flow and at elevated temperature. In order to gain complementary information by transmission and scanning electron microscopy, the cell makes use of a Protochips E-chipTM which contains a small, thin electron transparent window and allows heating. Two gold-based systems, 50 nm gold particles and nanoporous gold as a relevant catalyst sample, were used for studying the feasibility of the cell. Measurements showing a resolution around 40 nm have been achieved under a flow of synthetic air and during heating up to temperatures of 933 K. An elevated temperature exhibited little influence on image quality and resolution. With this study, the potential of in situ hard X-ray ptychography for investigating annealing processes of real catalyst samples is demonstrated. Furthermore, the possibility to use the same sample holder for ex situ electron microscopy before and after the in situ study underlines the unique possibilities available with this combination of electron microscopy and X-ray microscopy on the same sample.

  15. High Temperature Deformation Mechanism in Hierarchical and Single Precipitate Strengthened Ferritic Alloys by In Situ Neutron Diffraction Studies

    PubMed Central

    Song, Gian; Sun, Zhiqian; Li, Lin; Clausen, Bjørn; Zhang, Shu Yan; Gao, Yanfei; Liaw, Peter K.

    2017-01-01

    The ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni2TiAl/NiAl or single-Ni2TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior between the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate. PMID:28387230

  16. High temperature deformation mechanism in hierarchical and single precipitate strengthened ferritic alloys by in situ neutron diffraction studies

    DOE PAGES

    Song, Gian; Sun, Zhiqian; Li, Lin; ...

    2017-04-07

    Here, the ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni2TiAl/NiAl or single-Ni2TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior betweenmore » the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate.« less

  17. High Temperature Deformation Mechanism in Hierarchical and Single Precipitate Strengthened Ferritic Alloys by In Situ Neutron Diffraction Studies

    NASA Astrophysics Data System (ADS)

    Song, Gian; Sun, Zhiqian; Li, Lin; Clausen, Bjørn; Zhang, Shu Yan; Gao, Yanfei; Liaw, Peter K.

    2017-04-01

    The ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni2TiAl/NiAl or single-Ni2TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior between the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate.

  18. Beamline Electrostatic Levitator (BESL) for in-situ High Energy K-Ray Diffraction Studies of Levitated Solids and Liquids at High Temperature

    NASA Technical Reports Server (NTRS)

    Gangopadhyay, A. K.; Lee, G. W.; Kelton, K. F.; Rogers, J. R.; Goldman, A. I.; Robinson, D. S.; Rathz, T. J.; Hyers, R. W.

    2005-01-01

    Determinations of the phase formation sequence, the crystal structures and the thermodynamic properties of materials at high temperatures are difficult because of contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic (EML), aerodynamic, and acoustic levitation, are most suitable these studies. An adaptation of ESL for in-situ structural studies of a wide range of materials, including metals, semiconductors, insulators using high energy (125 keV) synchrotron x-rays is described here. This beamline ESL (BESL) allows the in-situ determination of the atomic structures of equilibrium solid and liquid phases, including undercooled liquids, as well as real-time studies of solid-solid and liquid-solid phase transformations. The use of image plate (MAR345) or GE-Angio detectors enables fast (30 ms - 1s) acquisition of complete diffraction patterns over a wide q-range (4 - 140/mm). The wide temperature range (300 - 2500 K), containerless processing under high vacuum (10(exp -7) - 10(exp -8) torr), and fast data acquisition, make BESL particularly suitable for phase diagram studies of high temperature materials. An additional, critically important, feature of BESL is the ability to also make simultaneous measurement of a host of thermo-physical properties, including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension; all on the same sample and simultaneous with the structural measurements.

  19. Beamline Electrostatic Levitator (BESL) for in-situ High Energy K-Ray Diffraction Studies of Levitated Solids and Liquids at High Temperature

    NASA Technical Reports Server (NTRS)

    Gangopadhyay, A. K.; Lee, G. W.; Kelton, K. F.; Rogers, J. R.; Goldman, A. I.; Robinson, D. S.; Rathz, T. J.; Hyers, R. W.

    2005-01-01

    Determinations of the phase formation sequence, the crystal structures and the thermodynamic properties of materials at high temperatures are difficult because of contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic (EML), aerodynamic, and acoustic levitation, are most suitable these studies. An adaptation of ESL for in-situ structural studies of a wide range of materials, including metals, semiconductors, insulators using high energy (125 keV) synchrotron x-rays is described here. This beamline ESL (BESL) allows the in-situ determination of the atomic structures of equilibrium solid and liquid phases, including undercooled liquids, as well as real-time studies of solid-solid and liquid-solid phase transformations. The use of image plate (MAR345) or GE-Angio detectors enables fast (30 ms - 1s) acquisition of complete diffraction patterns over a wide q-range (4 - 140/mm). The wide temperature range (300 - 2500 K), containerless processing under high vacuum (10(exp -7) - 10(exp -8) torr), and fast data acquisition, make BESL particularly suitable for phase diagram studies of high temperature materials. An additional, critically important, feature of BESL is the ability to also make simultaneous measurement of a host of thermo-physical properties, including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension; all on the same sample and simultaneous with the structural measurements.

  20. Generation of methane in the Earth's mantle: In situ high pressure–temperature measurements of carbonate reduction

    PubMed Central

    Scott, Henry P.; Hemley, Russell J.; Mao, Ho-kwang; Herschbach, Dudley R.; Fried, Laurence E.; Howard, W. Michael; Bastea, Sorin

    2004-01-01

    We present in situ observations of hydrocarbon formation via carbonate reduction at upper mantle pressures and temperatures. Methane was formed from FeO, CaCO3-calcite, and water at pressures between 5 and 11 GPa and temperatures ranging from 500°C to 1,500°C. The results are shown to be consistent with multiphase thermodynamic calculations based on the statistical mechanics of soft particle mixtures. The study demonstrates the existence of abiogenic pathways for the formation of hydrocarbons in the Earth's interior and suggests that the hydrocarbon budget of the bulk Earth may be larger than conventionally assumed. PMID:15381767

  1. X ray attenuation measurements for high-temperature materials characterization and in situ monitoring of damage accumulation

    NASA Astrophysics Data System (ADS)

    Baaklini, George Youssef

    1991-10-01

    The development and application is examined of x ray attenuation measurement systems that are capable of (1) characterizing density variations in high temperature materials, e.g., monolithic ceramics, ceramic and intermetallic matrix composites and (2) noninvasively monitoring damage accumulation and failure sequences in ceramic matrix composites under room temperature tensile testing. Results are presented in the development of (1) a point scan digital radiography system and (2) an in-situ x ray material testing system. The former is used to characterize silicon carbide and silicon nitride specimens and the latter is used to image the failure behavior of silicon carbide fiber reinforced reaction bonded silicon nitride matrix composites. Further, state of the art x ray computed tomography is studied to determine its capabilities and limitations in characterizing density variations of subscale engine components, e.g., a silicon carbide rotor, a silicon nitride blade, and a silicon carbide fiber reinforced beta titanium matrix rod, rotor, and ring. Microfocus radiography, conventional radiography, scanning acoustic microscopy, and metallography are used to substantiate the x ray computed tomography findings. Point scan digital radiography is a viable technique for characterization density variations in monolithic ceramic specimens. But it is very limited and time consuming in characterizing ceramic matrix composities. Precise x ray attenuation measurements, reflecting minute density variations, are achieved by photon counting and by using micro collimators at the source and the detector. X ray computed tomography is found to be a unique x ray attenuation measurement technique capable of providing cross sectional spatial density information in monolithic ceramics and metal matrix composites. X ray computed tomography is proven to accelerate generic composite component development. Radiographic evaluation before, during and after loading show the effect of preexisting

  2. Molecular beam mass spectrometer equipped with a catalytic wall reactor for in situ studies in high temperature catalysis research

    SciTech Connect

    Horn, R.; Ihmann, K.; Ihmann, J.; Jentoft, F.C.; Geske, M.; Taha, A.; Pelzer, K.; Schloegl, R.

    2006-05-15

    A newly developed apparatus combining a molecular beam mass spectrometer and a catalytic wall reactor is described. The setup has been developed for in situ studies of high temperature catalytic reactions (>1000 deg. C), which involve besides surface reactions also gas phase reactions in their mechanism. The goal is to identify gas phase radicals by threshold ionization. A tubular reactor, made from the catalytic material, is positioned in a vacuum chamber. Expansion of the gas through a 100 {mu}m sampling orifice in the reactor wall into differentially pumped nozzle, skimmer, and collimator chambers leads to the formation of a molecular beam. A quadrupole mass spectrometer with electron impact ion source designed for molecular beam inlet and threshold ionization measurements is used as the analyzer. The sampling time from nozzle to detector is estimated to be less than 10 ms. A detection time resolution of up to 20 ms can be reached. The temperature of the reactor is measured by pyrometry. Besides a detailed description of the setup components and the physical background of the method, this article presents measurements showing the performance of the apparatus. After deriving the shape and width of the energy spread of the ionizing electrons from measurements on N{sub 2} and He we estimated the detection limit in threshold ionization measurements using binary mixtures of CO in N{sub 2} to be in the range of several hundreds of ppm. Mass spectra and threshold ionization measurements recorded during catalytic partial oxidation of methane at 1250 deg. C on a Pt catalyst are presented. The detection of CH{sub 3}{center_dot} radicals is successfully demonstrated.

  3. Molecular beam mass spectrometer equipped with a catalytic wall reactor for in situ studies in high temperature catalysis research

    NASA Astrophysics Data System (ADS)

    Horn, R.; Ihmann, K.; Ihmann, J.; Jentoft, F. C.; Geske, M.; Taha, A.; Pelzer, K.; Schlögl, R.

    2006-05-01

    A newly developed apparatus combining a molecular beam mass spectrometer and a catalytic wall reactor is described. The setup has been developed for in situ studies of high temperature catalytic reactions (>1000°C), which involve besides surface reactions also gas phase reactions in their mechanism. The goal is to identify gas phase radicals by threshold ionization. A tubular reactor, made from the catalytic material, is positioned in a vacuum chamber. Expansion of the gas through a 100μm sampling orifice in the reactor wall into differentially pumped nozzle, skimmer, and collimator chambers leads to the formation of a molecular beam. A quadrupole mass spectrometer with electron impact ion source designed for molecular beam inlet and threshold ionization measurements is used as the analyzer. The sampling time from nozzle to detector is estimated to be less than 10ms. A detection time resolution of up to 20ms can be reached. The temperature of the reactor is measured by pyrometry. Besides a detailed description of the setup components and the physical background of the method, this article presents measurements showing the performance of the apparatus. After deriving the shape and width of the energy spread of the ionizing electrons from measurements on N2 and He we estimated the detection limit in threshold ionization measurements using binary mixtures of CO in N2 to be in the range of several hundreds of ppm. Mass spectra and threshold ionization measurements recorded during catalytic partial oxidation of methane at 1250°C on a Pt catalyst are presented. The detection of CH3• radicals is successfully demonstrated.

  4. Development of Nano-crystalline Doped-Ceramic Enabled Fiber Sensors for High Temperature In-Situ Monitoring of Fossil Fuel Gases

    SciTech Connect

    Xiao, Hai; Dong, Junhang; Lin, Jerry; Romero, Van

    2012-03-01

    This is a final technical report for the first project year from July 1, 2005 to Jan 31, 2012 for DoE/NETL funded project DE-FC26-05NT42439: Development of Nanocrystalline Doped-Ceramic Enabled Fiber Sensors for High Temperature In-Situ Monitoring of Fossil Fuel Gases. This report summarizes the technical progresses and achievements towards the development of novel nanocrystalline doped ceramic material-enabled optical fiber sensors for in situ and real time monitoring the gas composition of flue or hot gas streams involved in fossil-fuel based power generation and hydrogen production.

  5. [In situ experimental study of phase transition of calcite by Raman spectroscopy at high temperature and high pressure].

    PubMed

    Liu, Chuan-jiang; Zheng, Hai-fei

    2012-02-01

    The phase transitions of calcite at high temperature and high pressure were investigated by using hydrothermal diamond anvil cell combined with Raman spectroscopy. The result showed that the Raman peak of 155 cm(-1) disappeared, the peak of 1 087 cm(-1) splited into 1083 and 1 090 cm(-1) peaks and the peak of 282 cm(-1) abruptly reduced to 231 cm(-1) at ambient temperature when the system pressure increased to 1 666 and 2 127 MPa respectively, which proved that calcite transformed to calcite-II and calcite-III. In the heating process at the initial pressure of 2 761 MPa and below 171 degrees C, there was no change in Raman characteristic peaks of calcite-III. As the temperature increased to 171 degrees C, the color of calcite crystal became opaque completely and the symmetric stretching vibration peak of 1 087 cm(-1), in-plane bending vibration peak of 713 cm(-1) and lattice vibration peaks of 155 and 282 cm(-1) began to mutate, showing that the calcite-III transformed to a new phase of calcium carbonate at the moment. When the temperature dropped to room temperature, this new phase remained stable all along. It also indicated that the process of phase transformation from calcite to the new phase of calcium carbonate was irreversible. The equation of phase transition between calcite-III and new phase of calcium carbonate can be determined by P(MPa) = 9.09T x (degrees C) +1 880. The slopes of the Raman peak (v1 087) of symmetrical stretching vibration depending on pressure and temperature are dv/dP = 5.1 (cm(-1) x GPa(-1)) and dv/dT = -0.055 3(cm(-1) x degrees C(-1)), respectively.

  6. Nanoparticle metamorphosis: an in situ high-temperature transmission electron microscopy study of the structural evolution of heterogeneous Au:Fe2O3 nanoparticles.

    PubMed

    Baumgardner, William J; Yu, Yingchao; Hovden, Robert; Honrao, Shreyas; Hennig, Richard G; Abruña, Héctor D; Muller, David; Hanrath, Tobias

    2014-05-27

    High-temperature in situ electron microscopy and X-ray diffraction have revealed that Au and Fe2O3 particles fuse in a fluid fashion at temperatures far below their size-reduced melting points. With increasing temperature, the fused particles undergo a sequence of complex structural transformations from surface alloy to phase segregated and ultimately core-shell structures. The combination of in situ electron microscopy and spectroscopy provides insights into fundamental thermodynamic and kinetic aspects governing the formation of heterogeneous nanostructures. The observed structural transformations present an interesting analogy to thin film growth on the curved surface of a nanoparticle. Using single-particle observations, we constructed a phase diagram illustrating the complex relationships among composition, morphology, temperature, and particle size.

  7. Direct in situ measurements of thermospheric temperature

    NASA Technical Reports Server (NTRS)

    Kayser, D. C.; Nier, A. O.; Breig, E. L.; Power, R. A.; Hanson, W. B.

    1979-01-01

    The open source neutral mass spectrometer on the Atmosphere Explorer satellites used for direct in situ measurements of the neutral gas temperature by means of the 'fly-through' mode of operation is evaluated. The derived neutral temperature (Tn) is compared with ion temperatures (T1) obtained simultaneously from the on-board retarding potential analyzer for altitudes and conditions where the two temperatures should be equal. A statistical analysis showed consistency between concurrently observed values of Tn and T1, also shown through profiles depicting their altitude distributions between 150 and 225 km. The overall magnitude of temperatures calculated from the Jacchia (1971) model results in a better representation of the observations than the higher temperatures predicted for this region by the MSIS model (Hedin, 1977), and agreement is also found between observed temperatures and neutral temperatures derived from altitude distributions of N2 particle densities.

  8. In situ analysis of proteins at high temperatures mediated by capillary-flow hydrothermal UV-vis spectrophotometer with a water-soluble chromogenic reagent.

    PubMed

    Kawamura, Kunio; Nagayoshi, Hiroki; Yao, Toshio

    2010-05-14

    In situ monitoring of quantities, interactions, and conformations of proteins is essential for the study of biochemistry under hydrothermal environments and the analysis of hyperthermophilic organisms in natural hydrothermal systems on Earth. We have investigated the potential of a capillary-flow hydrothermal UV-vis spectrophotometer (CHUS) for performing in situ measurements of proteins and determining their behavior at extremely high temperatures, in combination with a chromogenic reagents probe, which interacts with the proteins. The spectral shift obtained using a combination of water-soluble porphyrin (TPPS) and bovine serum albumin (BSA) was the best among the spectral shifts obtained using different combinations of chromogenic reagents and proteins. The association behavior of TPPS with BSA was investigated in detail using CHUS at temperatures up to 175 degrees C and the association constant (K(ass)) of TPPS with BSA was successfully determined at temperatures up to 100 degrees C. The lnK(ass) values were inversely proportional to the T(-1) values in the temperature range 50-100 degrees C. These analyses showed for the first time that the decrease of association of TPPS with BSA is due to the conformational change, fragmentation, and/or denaturing of BSA rather than the decrease of the hydrophobic association between TPPS and BSA. This study conclusively demonstrates the usability of the CHUS system with a chromogenic reagent as an in situ detection and measurement system for thermostable proteins at extremely high temperatures. Copyright 2010 Elsevier B.V. All rights reserved.

  9. Phase transition in Ba{sub 2}In{sub 2}O{sub 5} studied by in situ high temperature X-ray diffraction using synchrotron radiation

    SciTech Connect

    Rey, J. F. Q.; Ferreira, F. F.; Muccillo, E. N. S.

    2009-01-29

    The order-disorder phase transition in Ba{sub 2}In{sub 2}O{sub 5} high-temperature ionic conductor was systematically studied by in situ high-temperature X-ray diffraction using synchrotron radiation and electrical conductivity. Pure barium indate was prepared by solid state reactions at 1300 deg. C. The room-temperature structural characterization showed a high degree of phase homogeneity in the prepared material. The reduction of the order-disorder phase transition temperature was verified by electrical conductivity and high-temperature X-ray diffraction. The observed features were explained based on Fourier-transform infrared spectroscopy results that revealed the presence of hydroxyl species in the crystal lattice. The increase of the intensity of few diffraction peaks near the phase transition temperature suggests the formation of a superstructure before the orthorhombic-to-tetragonal phase transition.

  10. An Insertable Passive LC Pressure Sensor Based on an Alumina Ceramic for In Situ Pressure Sensing in High-Temperature Environments.

    PubMed

    Xiong, Jijun; Li, Chen; Jia, Pinggang; Chen, Xiaoyong; Zhang, Wendong; Liu, Jun; Xue, Chenyang; Tan, Qiulin

    2015-08-31

    Pressure measurements in high-temperature applications, including compressors, turbines, and others, have become increasingly critical. This paper proposes an implantable passive LC pressure sensor based on an alumina ceramic material for in situ pressure sensing in high-temperature environments. The inductance and capacitance elements of the sensor were designed independently and separated by a thermally insulating material, which is conducive to reducing the influence of the temperature on the inductance element and improving the quality factor of the sensor. In addition, the sensor was fabricated using thick film integrated technology from high-temperature materials that ensure stable operation of the sensor in high-temperature environments. Experimental results showed that the sensor accurately monitored pressures from 0 bar to 2 bar at temperatures up to 800 °C. The sensitivity, linearity, repeatability error, and hysteretic error of the sensor were 0.225 MHz/bar, 95.3%, 5.5%, and 6.2%, respectively.

  11. High-Temperature In situ Deformation of GaAs Micro-pillars: Lithography Versus FIB Machining

    NASA Astrophysics Data System (ADS)

    Chen, M.; Wehrs, J.; Michler, J.; Wheeler, J. M.

    2016-11-01

    The plasticity of silicon-doped GaAs was investigated between 25°C and 400°C using microcompression to prevent premature failure by cracking. Micropillars with diameters of 2.5 μm were fabricated on a < 100rangle -oriented GaAs single crystal by means of both conventional lithographic etching techniques and focused ion beam machining and then compressed in situ in the scanning electron microscope (SEM). A transition in deformation mechanisms from partial dislocations to perfect dislocations was found at around 100°C. At lower temperatures, the residual surface layer from lithographic processing was found to provide sufficient constraint to prevent crack opening, which resulted in a significant increase in ductility over FIB-machined pillars. Measured apparent activation energies were found to be significantly lower than previous bulk measurements, which is mostly attributed to the silicon dopant and to a lesser extent to the size effect.

  12. In-situ tube burst testing and high-temperature deformation behavior of candidate materials for accident tolerant fuel cladding

    SciTech Connect

    Gussev, Maxim N.; Byun, Thak Sang; Yamamoto, Yukinori; Maloy, Stuart A.; Terrani, Kurt A.

    2015-11-01

    The high resistance of cladding to plastic deformation and burst failure is one of the most essential properties of accident tolerant fuel (ATF) for maintaining structural integrity during a loss-of-coolant accident (LOCA) since the deformation and burst behavior governs the cooling efficiency of flow channels and process of fission product release. To simulate and evaluate such deformation and burst process of thin-walled cladding, an in-situ testing and evaluation method has been developed on the basis of visual imaging and image analysis techniques. The method uses a specialized optics system consisted of a high-resolution video camera, light filtering unit, and monochromatic light sources, and the in-situ testing is performed using a 50 mm long pressurized thin-walled tubular specimen set in a programmable furnace. In this study eleven (11) candidate cladding materials for ATF, i.e., 6 FeCrAl alloys and 5 nanostructured steels, were tested using the newly developed method, and the time-dependent images were analyzed to produce detailed deformation and burst data such as true hoop stress, strain (creep) rate, and failure stress. Relatively soft FeCrAl alloys deformed and burst below 800°C while negligible strain rates were measured for higher strength alloys and/or for relatively thick wall specimens.

  13. In-situ tube burst testing and high-temperature deformation behavior of candidate materials for accident tolerant fuel cladding

    DOE PAGES

    Byun, Thak Sang; Yamamoto, Yukinori; Maloy, Stuart A.; ...

    2015-08-25

    Here, one of the most essential properties of accident tolerant fuel (ATF) for maintaining structural integrity during a loss-of-coolant accident (LOCA) is high resistance of the cladding to plastic deformation and burst failure, since the deformation and burst behavior governs the cooling efficiency of flow channels and the process of fission product release. To simulate and evaluate the deformation and burst process of thin-walled cladding, an in-situ testing and evaluation method has been developed on the basis of visual imaging and image analysis techniques. The method uses a specialized optics system consisting of a high-resolution video camera, a light filteringmore » unit, and monochromatic light sources. The in-situ testing is performed using a 50 mm long pressurized thin-walled tubular specimen set in a programmable furnace. As the first application, ten (10) candidate cladding materials for ATF, i.e., five FeCrAl alloys and five nanostructured steels, were tested using the newly developed method, and the time-dependent images were analyzed to produce detailed deformation and burst data such as true hoop stress, strain (creep) rate, and failure stress. Relatively soft FeCrAl alloys deformed and burst below 800 °C, while negligible strain rates were measured for higher strength alloys.« less

  14. In-situ tube burst testing and high-temperature deformation behavior of candidate materials for accident tolerant fuel cladding

    SciTech Connect

    Byun, Thak Sang; Yamamoto, Yukinori; Maloy, Stuart A.; Gussev, M. N.; Terrani, K. A.

    2015-08-25

    Here, one of the most essential properties of accident tolerant fuel (ATF) for maintaining structural integrity during a loss-of-coolant accident (LOCA) is high resistance of the cladding to plastic deformation and burst failure, since the deformation and burst behavior governs the cooling efficiency of flow channels and the process of fission product release. To simulate and evaluate the deformation and burst process of thin-walled cladding, an in-situ testing and evaluation method has been developed on the basis of visual imaging and image analysis techniques. The method uses a specialized optics system consisting of a high-resolution video camera, a light filtering unit, and monochromatic light sources. The in-situ testing is performed using a 50 mm long pressurized thin-walled tubular specimen set in a programmable furnace. As the first application, ten (10) candidate cladding materials for ATF, i.e., five FeCrAl alloys and five nanostructured steels, were tested using the newly developed method, and the time-dependent images were analyzed to produce detailed deformation and burst data such as true hoop stress, strain (creep) rate, and failure stress. Relatively soft FeCrAl alloys deformed and burst below 800 °C, while negligible strain rates were measured for higher strength alloys.

  15. In-situ tube burst testing and high-temperature deformation behavior of candidate materials for accident tolerant fuel cladding

    NASA Astrophysics Data System (ADS)

    Gussev, M. N.; Byun, T. S.; Yamamoto, Y.; Maloy, S. A.; Terrani, K. A.

    2015-11-01

    One of the most essential properties of accident tolerant fuel (ATF) for maintaining structural integrity during a loss-of-coolant accident (LOCA) is high resistance of the cladding to plastic deformation and burst failure, since the deformation and burst behavior governs the cooling efficiency of flow channels and the process of fission product release. To simulate and evaluate the deformation and burst process of thin-walled cladding, an in-situ testing and evaluation method has been developed on the basis of visual imaging and image analysis techniques. The method uses a specialized optics system consisting of a high-resolution video camera, a light filtering unit, and monochromatic light sources. The in-situ testing is performed using a 50 mm long pressurized thin-walled tubular specimen set in a programmable furnace. As the first application, ten (10) candidate cladding materials for ATF, i.e., five FeCrAl alloys and five nanostructured steels, were tested using the newly developed method, and the time-dependent images were analyzed to produce detailed deformation and burst data such as true hoop stress, strain (creep) rate, and failure stress. Relatively soft FeCrAl alloys deformed and burst below 800 °C, while negligible strain rates were measured for higher strength alloys.

  16. InAlN high electron mobility transistor Ti/Al/Ni/Au Ohmic contact optimisation assisted by in-situ high temperature transmission electron microscopy

    SciTech Connect

    Smith, M. D.; Parbrook, P. J.; O'Mahony, D.; Conroy, M.; Schmidt, M.

    2015-09-14

    This paper correlates the micro-structural and electrical characteristics associated with annealing of metallic multi-layers typically used in the formation of Ohmic contacts to InAlN high electron mobility transistors. The multi-layers comprised Ti/Al/Ni/Au and were annealed via rapid thermal processing at temperatures up to 925 °C with electrical current-voltage analysis establishing the onset of Ohmic (linear IV) behaviour at 750–800 °C. In-situ temperature dependent transmission electron microscopy established that metallic diffusion and inter-mixing were initiated near a temperature of 500 °C. Around 800 °C, inter-diffusion of the metal and semiconductor (nitride) was observed, correlating with the onset of Ohmic electrical behaviour. The sheet resistance associated with the InAlN/AlN/GaN interface is highly sensitive to the anneal temperature, with the range depending on the Ti layer thickness. The relationship between contact resistivity and measurement temperature follow that predicted by thermionic field emission for contacts annealed below 850 °C, but deviated above this due to excessive metal-semiconductor inter-diffusion.

  17. In Situ High Temperature High Pressure MAS NMR Study on the Crystallization of AlPO 4 -5

    SciTech Connect

    Zhao, Zhenchao; Xu, Suochang; Hu, Mary Y.; Bao, Xinhe; Hu, Jian Zhi

    2016-01-28

    A damped oscillating crystallization process of AlPO4-5 at the presence of small amount of water is demonstrated by in situ high temperature high pressure multinuclear MAS NMR. Crystalline AlPO4-5 is formed from an intermediate semicrystalline phase via continuous rearrangement of the local structure of amorphous precursor gel. Activated water catalyzes the rearrangement via repeatedly hydrolysis and condensation reaction. Strong interactions between organic template and inorganic species facilitate the ordered rearrangement. During the crystallization process, excess water, phosphate, and aluminums are expelled from the precursor. The oscillating crystallization reflects mass transportation between the solid and liquid phase during the crystallization process. This crystallization process is also applicable to AlPO4-5 crystallized in the presence of a relatively large amount of water.

  18. High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source†

    NASA Astrophysics Data System (ADS)

    Toulemonde, Pierre; Goujon, Céline; Laversenne, Laetitia; Bordet, Pierre; Bruyère, Rémy; Legendre, Murielle; Leynaud, Olivier; Prat, Alain; Mezouar, Mohamed

    2014-04-01

    We have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα 1, 2≈0.56 Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7 mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2.

  19. Application of In Situ Neutron and X-Ray Measurements at High Temperatures in the Development of Co-Re-Based Alloys for Gas Turbines

    NASA Astrophysics Data System (ADS)

    Mukherji, Debashis; Rösler, Joachim; Wehrs, Juri; Strunz, Pavel; Beran, Přemysl; Gilles, Ralph; Hofmann, Michael; Hoelzel, Markus; Eckerlebe, Helmut; Szentmiklósi, Laszlo; Mácsik, Zsuzsanna

    2013-01-01

    Co-Re alloy development is prompted by the search for new materials for future gas turbines which can be used at temperatures considerably higher than the current day single crystal Ni-based superalloys. The Co-Re-based alloys have been designed to have very high melting range, and they are meant for application at +373 K (+100 °C) above Ni-superalloys. They are significantly different from the conventional Co-based alloys that are used in static components of today's gas turbines, and the Co-Re alloys have never been used for structural applications before. The Co-Re-Cr system has complex microstructure with many different phases present. Phase transformations and stabilities of fine strengthening precipitates at high temperatures remain mostly unexplored in the Co-Re alloys, and to develop basic understanding, model ternary and quaternary compositions were studied within the alloy development program. In situ neutron and synchrotron measurements at high temperatures were extensively used for this purpose, and some recent results from the in situ measurements are presented. In particular, the effect of boron doping in Co-Re alloys and the stabilities of the fine TaC precipitates at high temperatures were investigated. A fine dispersion of TaC precipitates strengthens some Co-Re alloys, and their stabilities at the application temperatures are critical. In the beginning, the alloy development strategy is very briefly discussed.

  20. High temperature exposure of in-situ thermocouple fixed-point cells: stability with up to three months of continuous use

    NASA Astrophysics Data System (ADS)

    Elliott, C. J.; Greenen, A.; Lowe, D.; Pearce, J. V.; Machin, G.

    2015-04-01

    To categorise thermocouples in batches, manufacturers state an expected operating tolerance for when the thermocouples are as-new. In use, thermocouple behaviour can rapidly change and the tolerance becomes invalid, especially when used at high temperatures (i.e. above 1000 °C) as the processes leading to de-calibration, such as oxidation and contamination, can be very fast and lead to erroneous readings. In-situ thermocouple self-validation provides a method to track the drift and correct the thermocouple reading in real-time, but it must be shown to be reliable. Two miniature temperature fixed-point cells designed at NPL for in-situ thermocouple self-validation, the first containing a Pt-C eutectic alloy and the second containing a Ru-C eutectic alloy, have been exposed to temperatures close to their melting point for 2200 h and 1570 h, respectively, and continuously, for up to three months. Recalibration after this long-term high-temperature exposure, where a tantalum-sheathed thermocouple was always in place, is used to show that no significant change of the temperature reference point (the melting temperature) has occurred in either the Pt-C ingot or the Ru-C ingot, over timescales far longer than previously demonstrated and approaching that required by industry for practical use of the device.

  1. High-Temperature Tensile and Tribological Behavior of Hybrid (ZrB2+Al3Zr)/AA5052 In Situ Composite

    NASA Astrophysics Data System (ADS)

    Gautam, G.; Kumar, N.; Mohan, A.; Gautam, R. K.; Mohan, S.

    2016-09-01

    During service life, components such as piston, cylinder blocks, brakes, and discs/drums, have to work under high-temperature conditions. In order to have appropriate material for such applications high-temperature studies are important. Hybrid (ZrB2+Al3Zr)/AA5052 in situ composite has been investigated from ambient to 523 K (250 °C) at an interval of 50 deg. (ZrB2+Al3Zr)/AA5052 in situ composite has been fabricated by the direct melt reaction of AA5052 alloy with zirconium and boron salts. Microstructure studies show refinement in the grain size of base alloy on in situ formation of reinforcement particles. Al3Zr particles are observed in rectangular and polyhedron shapes. It is observed from the tensile studies that ultimate tensile strength, yield strength, and percentage elongation decrease with increase in test temperature. Similar kind of behavior is also observed for flow curve properties. The tensile results have also been correlated with fractography. Wear and friction results indicate that the wear rate increases with increase in normal load, whereas coefficient of friction shows decreasing trend. With increasing test temperature, wear rate exhibits a typical phenomenon. After an initial increase, wear rate follows a decreasing trend up to 423 K (150 °C), and finally a rapid increase is observed, whereas coefficient of friction increases continuously with increase in test temperature. The mechanisms responsible for the variation of wear and friction with different temperatures have been discussed in detail with the help of worn surfaces studies under scanning electron microscope (SEM) & 3D-profilometer and debris analysis by XRD.

  2. In-situ high temperature X-ray diffraction study on the phase transition process of polymetallic sulfide ore

    NASA Astrophysics Data System (ADS)

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

    2017-04-01

    The phase transformation of the polymetallic sulfide ore is quite complicated, especially the variety and diversity of the roasted intermediate. The mineralogy properties of the ore particles were characterized by XRF, ICP and SEM-EDS. The thermal stability of the complex ore was investigated using TG-DSC under different atmosphere (pure N2 and 1% O2-N2). The phase changes and intermediates were revealed by the in-situ XRD in pure N2 and 1% O2-N2 atmospheres with the temperature range from 25 to 800°C. These results indicated that the crystal transformation of the pyrrhotite from monoclinic to hexagonal at 320°C, and the pentlandite and chalcopyrite were decomposed into monosulfide solid solution in pure N2. While the pentlandite and chalcopyrite were completely oxidized into M*xFe3-xO4 (M*=Fe, Ni, Cu) and Fe2O3, which is also the final product of the ore sample oxidized under 1% O2-N2 atmosphere.

  3. High-temperature tensile cell for in situ real-time investigation of carbon fibre carbonization and graphitization processes.

    PubMed

    Behr, Michael; Rix, James; Landes, Brian; Barton, Bryan; Billovits, Gerry; Hukkanen, Eric; Patton, Jasson; Wang, Weijun; Keane, Denis; Weigand, Steven

    2016-11-01

    A new high-temperature fibre tensile cell is described, developed for use at the Advanced Photon Source at Argonne National Laboratory to enable the investigation of the carbonization and graphitization processes during carbon fibre production. This cell is used to heat precursor fibre bundles to temperatures up to ∼2300°C in a controlled inert atmosphere, while applying tensile stress to facilitate formation of highly oriented graphitic microstructure; evolution of the microstructure as a function of temperature and time during the carbonization and higher-temperature graphitization processes can then be monitored by collecting real-time wide-angle X-ray diffraction (WAXD) patterns. As an example, the carbonization and graphitization behaviour of an oxidized polyacrylonitrile fibre was studied up to a temperature of ∼1750°C. Real-time WAXD revealed the gradual increase in microstructure alignment with the fibre axis with increasing temperature over the temperature range 600-1100°C. Above 1100°C, no further changes in orientation were observed. The overall magnitude of change increased with increasing applied tensile stress during carbonization. As a second example, the high-temperature graphitizability of PAN- and pitch-derived commercial carbon fibres was studied. Here, the magnitude of graphitic microstructure evolution of the pitch-derived fibre far exceeded that of the PAN-derived fibres at temperatures up to ∼2300°C, indicating its facile graphitizability.

  4. In situ high-temperature X-ray diffraction and spectroscopic study of fibroferrite, FeOH(SO4)·5H2O

    NASA Astrophysics Data System (ADS)

    Ventruti, Gennaro; Ventura, Giancarlo Della; Corriero, Nicola; Malferrari, Daniele; Gualtieri, Alessandro F.; Susta, Umberto; Lacalamita, Maria; Schingaro, Emanuela

    2016-09-01

    The thermal dehydration process of fibroferrite, FeOH(SO4)·5H2O, a secondary iron-bearing hydrous sulfate, was investigated by in situ high-temperature synchrotron X-ray powder diffraction (HT-XRPD), in situ high-temperature Fourier transform infrared spectroscopy (HT-FTIR) and thermal analysis (TGA-DTA) combined with evolved gas mass spectrometry. The data analysis allowed the determination of the stability fields and the reaction paths for this mineral as well as characterization of its high-temperature products. Five main endothermic peaks are observed in the DTA curve collected from room T up to 800 °C. Mass spectrometry of gases evolved during thermogravimetric analysis confirms that the first four mass loss steps are due to water emission, while the fifth is due to a dehydroxylation process; the final step is due to the decomposition of the remaining sulfate ion. The temperature behavior of the different phases occurring during the heating process was analyzed, and the induced structural changes are discussed. In particular, the crystal structure of a new phase, FeOH(SO4)·4H2O, appearing at about 80 °C due to release of one interstitial H2O molecule, was solved by ab initio real-space and reciprocal-space methods. This study contributes to further understanding of the dehydration mechanism and thermal stability of secondary sulfate minerals.

  5. In-situ validation of remotely sensed land surface temperatures in high-arctic land regions - implications for gap filling and trend analyses

    NASA Astrophysics Data System (ADS)

    Westermann, S.; Langer, M.; Ostby, T.; Boike, J.; Schuler, T.; Etzelmuller, B.

    2015-12-01

    We present a summary of validation efforts of MODIS land surface temperature (MOD11A1, MYD11A1) using in-situ observations from the high-arctic sites Ny-Ålesund (79 °N) and Austfonna ice cap (80 °N) on Svalbard, as well as Samoylov Island in NE Siberia (72 °N). For all three sites, multi-year time series of outgoing and incoming long-wave radiation are available from which the skin temperature can be calculated. Our analysis is focused on long-term averages of all-sky temperatures which are required to determine trends of surface temperatures. At all sites, yearly averages computed from all available MODIS LST measurements are cold-biased by up to 3 °C, which is mainly caused by a significant cold-bias during the winter period. A closer analysis using in-situ observations of cloudiness reveals two main error sources. First, winter surface temperatures are systematically warmer for cloudy skies, so that the satellite predominantly samples "cold" clear-sky conditions. Secondly, the cloud detection algorithm fails to exclude a significant number of cloudy scenes, so that colder cloud top temperatures are contained in the surface temperature record. For the Austfonna ice cap, we estimate that the fraction of such cloud top temperatures could exceed 40%, which highlights the importance of this error source. Over the N Atlantic region, the number of MODIS LST retrievals varies by up to a factor of three, with highest numbers on the Greenland ice sheet and lowest numbers on Iceland the coastal regions of Norway. When assessing trends in land surface temperatures through remote sensing, three factors must be considered: a) trends in the "true" fraction of cloudy conditions, b) trends in the surface temperature for cloudy conditions, and c) trends in misidentified cloudy scenes and cloud top temperatures. We demonstrate that a simple gap-filling procedure using downscaled air temperatures from the ERA-interim reanalysis can significantly improve the agreement with in-situ

  6. High-temperature "spectrochronopotentiometry": correlating electrochemical performance with in situ Raman spectroscopy in solid oxide fuel cells.

    PubMed

    Kirtley, John D; Halat, David M; McIntyre, Melissa D; Eigenbrodt, Bryan C; Walker, Robert A

    2012-11-20

    Carbon formation or "coking" on solid oxide fuel cell (SOFC) anodes adversely affects performance by blocking catalytic sites and reducing electrochemical activity. Quantifying these effects, however, often requires correlating changes in SOFC electrochemical efficiency measured during operation with results from ex situ measurements performed after the SOFC has been cooled and disassembled. Experiments presented in this work couple vibrational Raman spectroscopy with chronopotentiometry to observe directly the relationship between graphite deposited on nickel cermet anodes and the electrochemical performance of SOFCs operating at 725 °C. Raman spectra from Ni cermet anodes at open circuit voltage exposed to methane show a strong vibrational band at 1556 cm(-1) assigned to the "G" mode of highly ordered graphite. When polarized in the absence of a gas-phase fuel, these carbon-loaded anodes operate stably, oxidizing graphite to form CO and CO(2). Disappearance of graphite intensity measured in the Raman spectra is accompanied by a steep ∼0.8 V rise in the cell potential needed to keep the SOFC operating under constant current conditions. Continued operation leads to spectroscopically observable Ni oxidation and another steep rise in cell potential. Time-dependent spectroscopic and electrochemical measurements pass through correlated equivalence points providing unequivocal, in situ evidence that identifies how SOFC performance depends on the chemical condition of its anode. Chronopotentiometric data are used to quantify the oxide flux necessary to eliminate the carbon initially present on the SOFC anode, and data show that the oxidation mechanisms responsible for graphite removal correlate directly with the electrochemical condition of the anode as evidenced by voltammetry and impedance measurements. Electrochemically oxidizing the Ni anode damages the SOFC significantly and irreversibly. Anodes that have been reconstituted following electrochemical oxidation of

  7. Temperature-gradient epitaxy under in situ growth mode diagnostics by scanning reflection high-energy electron diffraction

    NASA Astrophysics Data System (ADS)

    Koida, T.; Komiyama, D.; Koinuma, H.; Ohtani, M.; Lippmaa, M.; Kawasaki, M.

    2002-01-01

    We have developed a parallel film growth method on a temperature-gradient substrate to quickly control and optimize the film growth mode. A continuous-wave neodymium-doped yttrium-aluminum-garnet laser heating was used to achieve a stable temperature gradient covering a 300 °C range of temperatures over a distance of 11 mm. The growth mode was determined by time-resolved scanning reflection high-energy electron diffraction. Transition from layer-by-layer to step-flow growth by the deposition temperature was observed during La0.5Sr0.5MnO3 film growth on a single SrTiO3 substrate, proving a powerful tool not only for investigating the growth dynamics but also for seeking the optimized deposition conditions in one run of experiment.

  8. Pyrosequencing reveals high-temperature cellulolytic microbial consortia in Great Boiling Spring after in situ lignocellulose enrichment.

    PubMed

    Peacock, Joseph P; Cole, Jessica K; Murugapiran, Senthil K; Dodsworth, Jeremy A; Fisher, Jenny C; Moser, Duane P; Hedlund, Brian P

    2013-01-01

    To characterize high-temperature cellulolytic microbial communities, two lignocellulosic substrates, ammonia fiber-explosion-treated corn stover and aspen shavings, were incubated at average temperatures of 77 and 85°C in the sediment and water column of Great Boiling Spring, Nevada. Comparison of 109,941 quality-filtered 16S rRNA gene pyrosequences (pyrotags) from eight enrichments to 37,057 quality-filtered pyrotags from corresponding natural samples revealed distinct enriched communities dominated by phylotypes related to cellulolytic and hemicellulolytic Thermotoga and Dictyoglomus, cellulolytic and sugar-fermenting Desulfurococcales, and sugar-fermenting and hydrogenotrophic Archaeoglobales. Minor enriched populations included close relatives of hydrogenotrophic Thermodesulfobacteria, the candidate bacterial phylum OP9, and candidate archaeal groups C2 and DHVE3. Enrichment temperature was the major factor influencing community composition, with a negative correlation between temperature and richness, followed by lignocellulosic substrate composition. This study establishes the importance of these groups in the natural degradation of lignocellulose at high temperatures and suggests that a substantial portion of the diversity of thermophiles contributing to consortial cellulolysis may be contained within lineages that have representatives in pure culture.

  9. Pyrosequencing Reveals High-Temperature Cellulolytic Microbial Consortia in Great Boiling Spring after In Situ Lignocellulose Enrichment

    PubMed Central

    Peacock, Joseph P.; Cole, Jessica K.; Murugapiran, Senthil K.; Dodsworth, Jeremy A.; Fisher, Jenny C.; Moser, Duane P.; Hedlund, Brian P.

    2013-01-01

    To characterize high-temperature cellulolytic microbial communities, two lignocellulosic substrates, ammonia fiber-explosion-treated corn stover and aspen shavings, were incubated at average temperatures of 77 and 85°C in the sediment and water column of Great Boiling Spring, Nevada. Comparison of 109,941 quality-filtered 16S rRNA gene pyrosequences (pyrotags) from eight enrichments to 37,057 quality-filtered pyrotags from corresponding natural samples revealed distinct enriched communities dominated by phylotypes related to cellulolytic and hemicellulolytic Thermotoga and Dictyoglomus, cellulolytic and sugar-fermenting Desulfurococcales, and sugar-fermenting and hydrogenotrophic Archaeoglobales. Minor enriched populations included close relatives of hydrogenotrophic Thermodesulfobacteria, the candidate bacterial phylum OP9, and candidate archaeal groups C2 and DHVE3. Enrichment temperature was the major factor influencing community composition, with a negative correlation between temperature and richness, followed by lignocellulosic substrate composition. This study establishes the importance of these groups in the natural degradation of lignocellulose at high temperatures and suggests that a substantial portion of the diversity of thermophiles contributing to consortial cellulolysis may be contained within lineages that have representatives in pure culture. PMID:23555835

  10. Argon–germane in situ plasma clean for reduced temperature Ge on Si epitaxy by high density plasma chemical vapor deposition

    DOE PAGES

    Douglas, Erica A.; Sheng, Josephine J.; Verley, Jason C.; ...

    2015-06-04

    We found that the demand for integration of near infrared optoelectronic functionality with silicon complementary metal oxide semiconductor (CMOS) technology has for many years motivated the investigation of low temperature germanium on silicon deposition processes. Our work describes the development of a high density plasma chemical vapor deposition process that uses a low temperature (<460 °C) in situ germane/argon plasma surface preparation step for epitaxial growth of germanium on silicon. It is shown that the germane/argon plasma treatment sufficiently removes SiOx and carbon at the surface to enable germanium epitaxy. Finally, the use of this surface preparation step demonstrates anmore » alternative way to produce germanium epitaxy at reduced temperatures, a key enabler for increased flexibility of integration with CMOS back-end-of-line fabrication.« less

  11. Argon–germane in situ plasma clean for reduced temperature Ge on Si epitaxy by high density plasma chemical vapor deposition

    SciTech Connect

    Douglas, Erica A.; Sheng, Josephine J.; Verley, Jason C.; Carroll, Malcolm S.

    2015-06-04

    We found that the demand for integration of near infrared optoelectronic functionality with silicon complementary metal oxide semiconductor (CMOS) technology has for many years motivated the investigation of low temperature germanium on silicon deposition processes. Our work describes the development of a high density plasma chemical vapor deposition process that uses a low temperature (<460 °C) in situ germane/argon plasma surface preparation step for epitaxial growth of germanium on silicon. It is shown that the germane/argon plasma treatment sufficiently removes SiOx and carbon at the surface to enable germanium epitaxy. Finally, the use of this surface preparation step demonstrates an alternative way to produce germanium epitaxy at reduced temperatures, a key enabler for increased flexibility of integration with CMOS back-end-of-line fabrication.

  12. Microstructure and high-temperature wear properties of in situ TiC composite coatings by plasma transferred arc surface alloying on gray cast iron

    NASA Astrophysics Data System (ADS)

    Zhao, Hang; Li, Jian-jun; Zheng, Zhi-zhen; Wang, Ai-hua; Huang, Qi-wen; Zeng, Da-wen

    2015-12-01

    In this work, an in situ synthesized TiC-reinforced metal matrix composite (MMC) coating of approximately 350-400 µm thickness was fabricated on a gray cast iron (GCI) substrate by plasma transferred arc (PTA) surface alloying of Ti-Fe alloy powder. Microhardness tests showed that the surface hardness increased approximately four-fold after the alloying treatment. The microstructure of the MMC coating was mainly composed of residual austenite, acicular martensite, and eutectic ledeburite. Scanning electron microscopy (SEM) and X-ray diffraction analyzes revealed that the in situ TiC particles, which were formed by direct reaction of Ti with carbon originally contained in the GCI, was uniformly distributed at the boundary of residual austenite in the alloying zone. Pin-on-disc high-temperature wear tests were performed on samples both with and without the MMC coating at room temperature and at elevated temperatures (473 K and 623 K), and the wear behavior and mechanism were investigated. The results showed that, after the PTA alloying treatment, the wear resistance of the samples improved significantly. On the basis of our analysis of the composite coatings by optical microscopy, SEM with energy-dispersive X-ray spectroscopy, and microhardness measurements, we attributed this improvement of wear resistance to the transformation of the microstructure and to the presence of TiC particles.

  13. Investigation of phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) by in situ synchrotron high-temperature powder diffraction

    SciTech Connect

    Ouyang, Xin; Huang, Saifang; Zhang, Weijun; Cao, Peng; Huang, Zhaohui; Gao, Wei

    2014-03-15

    In situ synchrotron X-ray powder diffraction was used to study the high-temperature phase evolution of CaCu{sub 3}Ti{sub 4}O{sub 12} (CCTO) precursors prepared via solid-state and sol–gel methods. After the precursors are heated to 1225 °C, the CCTO phase is the main phase observed in the calcined powder, with the presence of some minor impurities. Comparing the two precursors, we found that the onset temperature for the CCTO phase formation is 800 °C in the sol–gel precursor, lower than that in the solid-state precursor (875 °C). Intermediate phases were only observed in the sol–gel precursor. Both precursors are able to be calcined to sub-micrometric sized powders. Based on the synchrotron data along with differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA), the phase formation sequence and mechanism during calcination are proposed in this study. -- Graphical abstract: The in situ synchrotron HT-XRD patterns of CCTO sol–gel and solid-state precursor. Highlights: • Phase formation sequence/mechanism in two CCTO precursors has been established. • Formation temperature of CCTO via sol–gel method is lower than solid-state method. • Intermediate phases are only observed in the sol–gel precursor. • Both precursors are able to be calcined into sub-micrometric sized powders.

  14. In situ studies of oxidation of ZrB2 and ZrB2-SiC composites at high temperatures

    SciTech Connect

    Sarin, P; Driemeyer, P E; Haggerty, R P; Kim, D -K; Bell, J L; Apostolov, Z D; Kriven, W M

    2010-08-27

    High temperature oxidation of ZrB2 and the effect of SiC on controlling the oxidation of ZrB2 in ZrB2-SiC composites were studied in situ, in air, using X-ray diffraction. Oxidation was studied by quantitatively analyzing the crystalline phase changes in the samples, both non-isothermally, as a function of temperature, up to ~1650 ºC, as well as isothermally, as a function of time, at ~1300 ºC. During the non-isothermal studies, the formation and transformation of intermediate crystalline phases of ZrO2 were also observed. The change in SiC content, during isothermal oxidation studies of ZrB2-SiC composites, was similar in the examined temperature range, regardless of sample microstructure and composition. Higher SiC content, however, markedly retarded the oxidation rate of the ZrB2 phase in the composites. A novel approach to quantify the extent of oxidation by estimating the thickness of the oxidation layer formed during oxidation of ZrB2 and ZrB2-SiC composites, based on fractional conversion of ZrB2 to ZrO2 in situ, is presented.

  15. Hydrogen sensor based on Au and YSZ/HgO/Hg electrode for in situ measurement of dissolved H2 in high-temperature and -pressure fluids.

    PubMed

    Zhang, R H; Hu, S M; Zhang, X T; Wang, Y

    2008-11-15

    Gold as a hydrogen-sensing electrode for in situ measurement of dissolved H2 in aqueous solutions under extreme conditions is reported. The dissolved H2 sensor, constructed with a Au-based sensing element and coupled with a YSZ/HgO/Hg electrode, is well suited for determining dissolved H2 concentrations of aqueous fluids at elevated temperatures and pressures. The Au electrode is made of Au wire mounted in a quartz bar, which can be pressurized and heated in the high-pressure and -temperature conditions. The Au-YSZ sensor has been tested for its potential response to the concentrations of dissolved H2 in fluids by using a flow-through reactor at high temperatures up to 400 degrees C and pressures to 38 MPa. Good sensitivity and linear response between the hydrogen concentrations in the fluids and the H2 sensor potentials are reported for hydrogen gas in the concentration range of 0.1-0.001 M H2 in aqueous fluids at temperatures up to 340 degrees C and 30 MPa. Nernstian response of the cell potential to dissolved H2 in fluids was determined at 340 degrees C and 30 MPa, described as follows: DeltaE = 0.9444 + 0. 0603 log m H2 The experimental results indicate that the Au-YSZ/HgO/Hg cell can be used to measure the solubility of H2 in aqueous fluid at temperatures and pressures near to the critical state of water. Thus, this type of Au hydrogen sensor could be easily used for in situ measurement of H2 in hydrothermal fluids in a high-pressure vessel, or at midocean ridge, due to its structure of compression resistance.

  16. Highly conductive graphene by low-temperature thermal reduction and in situ preparation of conductive polymer nanocomposites.

    PubMed

    Yang, Liping; Kong, Junhua; Yee, Wu Aik; Liu, Wanshuang; Phua, Si Lei; Toh, Cher Ling; Huang, Shu; Lu, Xuehong

    2012-08-21

    Polydopamine-coated graphene oxide (DGO) films exhibit electrical conductivities of 11,000 S m(-1) and 30,000 S m(-1) upon vacuum annealing at 130 °C and 180 °C, respectively. Conductive poly(vinyl alcohol)/graphene and epoxy/graphene nanocomposites show low percolation thresholds due to the excellent dispersibility of the DGO sheets and their effective in situ reduction.

  17. Oil-Soluble Silver-Organic Molecule for in Situ Deposition of Lubricious Metallic Silver at High Temperatures.

    PubMed

    Desanker, Michael; Johnson, Blake; Seyam, Afif M; Chung, Yip-Wah; Bazzi, Hassan S; Delferro, Massimiliano; Marks, Tobin J; Wang, Q Jane

    2016-06-01

    A major challenge in lubrication technology is to enhance lubricant performance at extreme temperatures that exceed conventional engine oil thermal degradation limits. Soft noble metals such as silver have low reactivity and shear strength, which make them ideal solid lubricants for wear protection and friction reduction between contacting surfaces at high temperatures. However, achieving adequate dispersion in engine lubricants and metallic silver deposition over predetermined temperatures ranges presents a significant chemical challenge. Here we report the synthesis, characterization, and tribological implementation of the trimeric silver pyrazolate complex, [Ag(3,5-dimethyl-4-n-hexyl-pyrazolate)]3 (1). This complex is oil-soluble and undergoes clean thermolysis at ∼310 °C to deposit lubricious, protective metallic silver particles on metal/metal oxide surfaces. Temperature-controlled tribometer tests show that greater than 1 wt % loading of 1 reduces wear by 60% in PAO4, a poly-α-olefin lubricant base fluid, and by 70% in a commercial fully formulated 15W40 motor oil (FF oil). This silver-organic complex also imparts sufficient friction reduction so that the tribological transition from oil as the primary lubricant through its thermal degradation, to 1 as the primary lubricant, is experimentally undetectable.

  18. In-Situ Measurement of High-Temperature Proton Exchange Membrane Fuel Cell Stack Using Flexible Five-in-One Micro-Sensor.

    PubMed

    Lee, Chi-Yuan; Weng, Fang-Bor; Kuo, Yzu-Wei; Tsai, Chao-Hsuan; Cheng, Yen-Ting; Cheng, Chih-Kai; Lin, Jyun-Ting

    2016-10-18

    In the chemical reaction that proceeds in a high-temperature proton exchange membrane fuel cell stack (HT-PEMFC stack), the internal local temperature, voltage, pressure, flow and current nonuniformity may cause poor membrane material durability and nonuniform fuel distribution, thus influencing the performance and lifetime of the fuel cell stack. In this paper micro-electro-mechanical systems (MEMS) are utilized to develop a high-temperature electrochemical environment-resistant five-in-one micro-sensor embedded in the cathode channel plate of an HT-PEMFC stack, and materials and process parameters are appropriately selected to protect the micro-sensor against failure or destruction during long-term operation. In-situ measurement of the local temperature, voltage, pressure, flow and current distributions in the HT-PEMFC stack is carried out. This integrated micro-sensor has five functions, and is favorably characterized by small size, good acid resistance and temperature resistance, quick response, real-time measurement, and the goal is being able to be put in any place for measurement without affecting the performance of the battery.

  19. In-Situ Measurement of High-Temperature Proton Exchange Membrane Fuel Cell Stack Using Flexible Five-in-One Micro-Sensor

    PubMed Central

    Lee, Chi-Yuan; Weng, Fang-Bor; Kuo, Yzu-Wei; Tsai, Chao-Hsuan; Cheng, Yen-Ting; Cheng, Chih-Kai; Lin, Jyun-Ting

    2016-01-01

    In the chemical reaction that proceeds in a high-temperature proton exchange membrane fuel cell stack (HT-PEMFC stack), the internal local temperature, voltage, pressure, flow and current nonuniformity may cause poor membrane material durability and nonuniform fuel distribution, thus influencing the performance and lifetime of the fuel cell stack. In this paper micro-electro-mechanical systems (MEMS) are utilized to develop a high-temperature electrochemical environment-resistant five-in-one micro-sensor embedded in the cathode channel plate of an HT-PEMFC stack, and materials and process parameters are appropriately selected to protect the micro-sensor against failure or destruction during long-term operation. In-situ measurement of the local temperature, voltage, pressure, flow and current distributions in the HT-PEMFC stack is carried out. This integrated micro-sensor has five functions, and is favorably characterized by small size, good acid resistance and temperature resistance, quick response, real-time measurement, and the goal is being able to be put in any place for measurement without affecting the performance of the battery. PMID:27763559

  20. Accelerated corrosion and oxide dissolution in 316L stainless steel irradiated in situ in high temperature water

    NASA Astrophysics Data System (ADS)

    Raiman, Stephen S.; Was, Gary S.

    2017-09-01

    316L stainless steel samples were irradiated with a proton beam while simultaneously exposed to high temperature water with added hydrogen (320 °C, 3 wppm H2, neutral pH) to study the effect of radiation on stainless steel corrosion. Irradiated samples had thinner and more porous inner oxides with a lower chromium content when compared to unirradiated samples. Observations suggest that depletion of chromium from the inner oxide can be attributed to the dissolution of chromium-rich spinel oxides in irradiated water, leading to an accelerated rate of inner oxide dissolution. Sample areas which were not irradiated, but were exposed to the flow of irradiated water were also found to be porous and deficient in chromium, indicating that these phenomena can be attributed primarily to water radiolysis. A new empirical equation for oxide growth and dissolution is used to describe the observed changes in oxide thickness under irradiation. An experiment in which a stainless steel sample was exposed to high temperature water (320 °C, 3 wppm H2, neutral pH) without irradiation, and then exposed for a second time with irradiation was conducted to observe the effect of irradiation on a pre-formed protective film. After the irradiated exposure, the sample exhibited chromium loss in regions which were directly irradiated, but not on regions exposed only to irradiated water, suggesting that a pre-formed protective oxide may be effective in preventing chromium loss due to irradiated water. Additionally, this observation suggests that enhanced kinetics under irradiation may have accelerated dissolution of chromium from the inner oxide.

  1. In situ Gas Temperature Measurements by UV-Absorption Spectroscopy

    NASA Astrophysics Data System (ADS)

    Fateev, A.; Clausen, S.

    2009-02-01

    The absorption spectrum of the NO A2Σ+ ← X2Πγ-system can be used for in situ evaluation of gas temperature. Experiments were performed with a newly developed atmospheric-pressure high-temperature flow gas cell at highly uniform and stable gas temperatures over a 0.533 m path in the range from 23 °C to 1,500 °C. The gas temperature was evaluated (1) from the analysis of the structure of selected NO high-resolution γ-absorption bands and (2) from the analysis of vibrational distribution in the NO γ-absorption system in the (211-238) nm spectral range. The accuracy of both methods is discussed. Validation of the classical Lambert-Beer law has been demonstrated at NO concentrations up to 500 ppm and gas temperatures up to 1,500 °C over an optical absorption path length of 0.533 m.

  2. In situ atomic force microscope study of high-temperature untwinning surface relief in Mn-Fe-Cu antiferromagnetic shape memory alloy

    SciTech Connect

    Wang, L.; Cui, Y. G.; Wan, J. F.; Rong, Y. H.; Zhang, J. H.; Jin, X.; Cai, M. M.

    2013-05-06

    The N-type untwinning surface relief associated with the fcc {r_reversible} fct martensitic transformation (MT) was observed in the Mn{sub 81.5}Fe{sub 14.0}Cu{sub 4.5} antiferromagnetic high-temperature shape memory alloy (SMA) by in situ atomic force microscopy. The measured untwinning relief angles ({theta}{sub {alpha}} Double-Vertical-Line {theta}{sub {beta}}) at the ridge and at the valley were different, and both angles were less than the conventional values. The surface relief exhibited good reversibility during heating and cooling because of the crystallographic reversibility of thermal-elastic SMAs. Untwinning shear was proposed as the main mechanism of the N-type surface relief. The order of the reverse MT was discussed based on the experimental measurements.

  3. Catalytic behavior of metal catalysts in high-temperature RWGS reaction: In-situ FT-IR experiments and first-principles calculations

    NASA Astrophysics Data System (ADS)

    Choi, Sungjun; Sang, Byoung-In; Hong, Jongsup; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook; Kim, Hyoungchul

    2017-01-01

    High-temperature chemical reactions are ubiquitous in (electro) chemical applications designed to meet the growing demands of environmental and energy protection. However, the fundamental understanding and optimization of such reactions are great challenges because they are hampered by the spontaneous, dynamic, and high-temperature conditions. Here, we investigated the roles of metal catalysts (Pd, Ni, Cu, and Ag) in the high-temperature reverse water-gas shift (RWGS) reaction using in-situ surface analyses and density functional theory (DFT) calculations. Catalysts were prepared by the deposition-precipitation method with urea hydrolysis and freeze-drying. Most metals show a maximum catalytic activity during the RWGS reaction (reaching the thermodynamic conversion limit) with formate groups as an intermediate adsorbed species, while Ag metal has limited activity with the carbonate species on its surface. According to DFT calculations, such carbonate groups result from the suppressed dissociation and adsorption of hydrogen on the Ag surface, which is in good agreement with the experimental RWGS results.

  4. Catalytic behavior of metal catalysts in high-temperature RWGS reaction: In-situ FT-IR experiments and first-principles calculations

    PubMed Central

    Choi, Sungjun; Sang, Byoung-In; Hong, Jongsup; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook; Kim, Hyoungchul

    2017-01-01

    High-temperature chemical reactions are ubiquitous in (electro) chemical applications designed to meet the growing demands of environmental and energy protection. However, the fundamental understanding and optimization of such reactions are great challenges because they are hampered by the spontaneous, dynamic, and high-temperature conditions. Here, we investigated the roles of metal catalysts (Pd, Ni, Cu, and Ag) in the high-temperature reverse water-gas shift (RWGS) reaction using in-situ surface analyses and density functional theory (DFT) calculations. Catalysts were prepared by the deposition-precipitation method with urea hydrolysis and freeze-drying. Most metals show a maximum catalytic activity during the RWGS reaction (reaching the thermodynamic conversion limit) with formate groups as an intermediate adsorbed species, while Ag metal has limited activity with the carbonate species on its surface. According to DFT calculations, such carbonate groups result from the suppressed dissociation and adsorption of hydrogen on the Ag surface, which is in good agreement with the experimental RWGS results. PMID:28120896

  5. Catalytic behavior of metal catalysts in high-temperature RWGS reaction: In-situ FT-IR experiments and first-principles calculations.

    PubMed

    Choi, Sungjun; Sang, Byoung-In; Hong, Jongsup; Yoon, Kyung Joong; Son, Ji-Won; Lee, Jong-Ho; Kim, Byung-Kook; Kim, Hyoungchul

    2017-01-25

    High-temperature chemical reactions are ubiquitous in (electro) chemical applications designed to meet the growing demands of environmental and energy protection. However, the fundamental understanding and optimization of such reactions are great challenges because they are hampered by the spontaneous, dynamic, and high-temperature conditions. Here, we investigated the roles of metal catalysts (Pd, Ni, Cu, and Ag) in the high-temperature reverse water-gas shift (RWGS) reaction using in-situ surface analyses and density functional theory (DFT) calculations. Catalysts were prepared by the deposition-precipitation method with urea hydrolysis and freeze-drying. Most metals show a maximum catalytic activity during the RWGS reaction (reaching the thermodynamic conversion limit) with formate groups as an intermediate adsorbed species, while Ag metal has limited activity with the carbonate species on its surface. According to DFT calculations, such carbonate groups result from the suppressed dissociation and adsorption of hydrogen on the Ag surface, which is in good agreement with the experimental RWGS results.

  6. High-temperature in-situ TEM straining of the interaction with dislocations and particles for Cu-added ferritic stainless steel.

    PubMed

    Kobayashi, Shuhei; Kaneko, Kenji; Yamada, Kazuhiro; Kikuchi, Masao; Kanno, Norihiro; Hamada, Junichi

    2014-11-01

    IntroductionCu is always present in the matrix when ferritic steels were prepared from ferrous scrap. When the ferritic steels are aged thermally, Cu precipitates start appear and disperse finely and homogeneously [1], which may make the steels strengthened by precipitation hardening. In this study, the interaction between Cu precipitates and dislocations was exmined via high-temperature in-situ TEM straining. ExperimentalCu-added ferritic stainless steel (Fe-18.4%Cr-1.5%Cu) was used in the present study. Specimen was aged at1073 K for 360 ks. Samples for TEM observation were prepared by focused ion beam (FIB; Quanta 3D 200i) method. Microstructure of specimen was analyzed by JEM-3200FSK and high-temperature in-situ TEM straining was conducted using JEM-1300NEF. Results and discussionInteraction between Cu precipitates and dislocation is seen from consecutive TEM images acquired by in-situ TEM straining at 1073 K, as shown in Fig.1. The size of Cu precipitates was about 70 nm and several dislocations were present within the field of view. In particular, progressing dislocations contacted with the Cu precipitate at right angle, as indicated by arrows in Fig.1 (b) to (d). This result implies that there is an attractive interaction between dislocations and the Cu precipitate. This is attributed to the fact that Stress field of dislocations was easily relaxed in interface between the Cu precipitate and matrix because of lattice and interface diffusion as well as slip in the interface [2,3]. Furthermore, dislocations pass through the particle after contacting it, so that the interaction with dislocations and particles should be explained by Srolovitz mechanism [4].jmicro;63/suppl_1/i28/DFU083F1F1DFU083F1Fig. 1.TEM images foucused on interaction with dislocations and partticles. © The Author 2014. Published by Oxford University Press on behalf of The Japanese Society of Microscopy. All rights reserved. For permissions, please e-mail: journals.permissions@oup.com.

  7. In situ high temperature X-Ray diffraction study of the phase equilibria in the UO2-PuO2-Pu2O3 system

    NASA Astrophysics Data System (ADS)

    Belin, Renaud C.; Strach, Michal; Truphémus, Thibaut; Guéneau, Christine; Richaud, Jean-Christophe; Rogez, Jacques

    2015-10-01

    The region of the U-Pu-O phase diagram delimited by the compounds UO2-PuO2-Pu2O3 is known to exhibit a miscibility gap at low temperature. Consequently, MOX fuels with a composition entering this region could decompose into two fluorite phases and thus exhibit chemical heterogeneities. The experimental data on this domain found in the literature are scarce and usually provided using DTA that is not suitable for the investigation of such decomposition phenomena. In the present work, new experimental data, i.e. crystallographic phases, lattice parameters, phase fractions and temperature of phase separation, were measured in the composition range 0.14 < Pu/(U + Pu) < 0.62 and 1.85 < O/(U + Pu) < 2 from 298 to 1750 K using a novel in situ high temperature X-ray diffraction apparatus. A very good agreement is found between the temperature of phase separation determined from our results and using the thermodynamic model of the U-Pu-O system based on the CALPHAD method. Also, the combined use of thermodynamic calculations and XRD results refinement proved helpful in the determination of the O/M ratio of the samples during cooling. The methodology used in the current work might be useful to investigate other oxides systems exhibiting a miscibility gap.

  8. GAXRD and in situ X-ray diffraction characterizations of the yttrium implantation effect on pure iron oxidation at high temperature

    NASA Astrophysics Data System (ADS)

    Caudron, E.; Buscail, H.; Cueff, R.; Issartel, C.; Perrier, S.; Riffard, F.

    2002-07-01

    High temperature oxidation behaviours of yttrium implanted and unimplanted pure iron were analyzed at T=700^{circ}C and under oxygen partial pressure Po2=0.04 Pa for 24h by several X-ray diffraction techniques to understand the yttrium implantation effect on pure iron oxidation resistance at high temperature. Sample compositions and structures were investigated before and after yttrium implantation to determine the yttrium distributions and the main compounds induced by ion implantation. Yttrium implantation effects were characterized using analytical and structural techniques such as Rutherford Backscattering Spectrometry (RBS), Secondary Ion Mass Spectrometry (SIMS), Reflection High Energy Electron Diffraction (RHEED), X-ray Diffraction (XRD) and Glancing Angle X-ray Diffraction (GAXRD). Yttrium-implanted and unimplanted pure iron oxidation weight gains were studied by thermogravimetry and structural analyses were carried out by in-situ high temperature X-ray diffraction. The aim of this paper is to show the initial nucleation stage of the main compounds induced by pure iron oxidation at high temperature according to the surface treatment (yttrium implantation). The results obtained by Glancing angle X-ray diffraction and by in-situ high temperature X-ray diffraction allow to understand the better oxidation resistance observed in the case of yttrium implanted pure iron. Les comportements en oxydation à haute température (T=700^{circ}C - pression partielle d'oxygène Po2=0.04 Pa) du fer pur brut et implanté à l'yttrium ont été analysés pendant 24h par plusieurs techniques dc diffraction X afin de comprendre l'effet de l'yttrium sur la résistance à l'oxydation à haute température du fer pur. Les compositions et les analyses structurales ont été effectuées avant et après implantation pour déterminer les distributions en yttrium ainsi que les différents composés induits par l'implantion ionique. Les effets de l'implantation d'yttrium ont

  9. An in-situ SERS investigation of the passive film on stainless steel at high temperature in pressurized water

    NASA Astrophysics Data System (ADS)

    Kumai, Christopher Shigeki

    2000-10-01

    An in situ study of the films formed on stainless steel at 288°C was performed using Surface Enhanced Raman Spectroscopy (SERS). By monitoring changes in the structure of the film as the interface potential of the sample changed, it was possible to suggest how the surface film affects Intergranular Stress Corrosion Cracking (IGSCC). Samples included 304 stainless steel, chromium depleted alloys, iron, nickel, and chromium. Observations of the films on iron, nickel, and chromium were compared to calculated Pourbaix diagrams. All of the iron based samples were found to passivate by the formation of alpha-Fe2O3 at --400 mV SHE. Below this potential, the surface film consisted of Fe3O4. On the iron-chromium alloys, gamma-Fe2O3 was found to form at intermediate interface potentials. These results suggest a reason for the well-known observation that IGSCC only occurs at potentials above --230 mV. Namely, when the potential outside the crack is --230 mV, the potential at the tip of the intergranular stress corrosion crack is --400 mV, the value above which all iron base alloys regardless of their chromium concentration are passive. Decreased chromium concentrations decreased the ability of alpha-Fe 2O3 and Fe3O4 to protect the sample. In addition, decreased chromium concentrations increased the potential at which gamma-Fe2O3 formed. Ex situ scanning electron microscopy was used to show that the films formed on the iron based samples were a double layer film consisting of an inner layer of conformal Fe3O4 and an outer layer of ˜1um sized grains of Fe3O4. Upon passivation, the alpha-Fe 2O3 formed a thin layer over all surfaces. The transformation of Fe3O4 to alpha-Fe2O3 takes place by a solid state reaction. The majority of outer layer formation occurred before the formation of the passivating alpha-Fe2O3 layer. Growth of the outer layer is limited by the electrochemical reduction at the film/water interface and not by transport of iron cations through the inner layer of

  10. In situ transesterification of highly wet microalgae using hydrochloric acid.

    PubMed

    Kim, Bora; Im, Hanjin; Lee, Jae W

    2015-06-01

    This study addresses in situ transesterification of highly wet microalgae with hydrochloric acid (HCl) as a catalyst. In situ transesterification was performed by heating the mixture of wet algal cells, HCl, methanol, and solvent in one pot, resulting in the fatty acid methyl ester (FAME) yield over 90% at 95°C. The effects of reaction variables of temperature, amounts of catalyst, reactant, and solvent, and type of solvents on the yield were investigated. Compared with the catalytic effect of H2SO4, in situ transesterification using HCl has benefits of being less affected by moisture levels that are as high as or above 80%, and requiring less amounts of catalyst and solvent. For an equimolar amount of catalyst, HCl showed 15wt.% higher FAME yield than H2SO4. This in situ transesterification using HCl as a catalyst would help to realize a feasible way to produce biodiesel from wet microalgae. Copyright © 2015 Elsevier Ltd. All rights reserved.

  11. Temperature behavior of the AlH3 polymorph by in situ investigation using high resolution Raman scattering.

    PubMed

    Giannasi, A; Colognesi, D; Fichtner, M; Röhm, E; Ulivi, L; Ziparo, C; Zoppi, M

    2011-02-10

    A Raman investigation of the AlH(3) polymorph has been carried out at a low temperature (20 K) under helium atmosphere (2 bar). The pristine material was composed of three polymorphs, namely, the α, β, and γ phases. The β phase has been removed by warming the sample to 70 °C, while further heating at 100 °C was used to remove the γ phase. This allowed us to evidence, on a purely experimental basis, the characteristic Raman spectrum for each phase. Raman spectra, for the three phases, have been also calculated using density functional theory, and the results have been compared to the present experimental data, allowing for a univocal assignment, to each phase, of its characteristic spectral features.

  12. In-Situ Studies of Structure Transformation and Al Coordination of KAl(MoO₄)₂ during Heating by High Temperature Raman and (27)Al NMR Spectroscopies.

    PubMed

    Wang, Min; You, Jinglin; Sobol, Alexander; Lu, Liming; Wang, Jian; Xie, Yingfang

    2017-03-17

    Recent interest in optimizing composition and synthesis conditions of functional crystals, and the further exploration of new possible candidates for tunable solid-state lasers, has led to significant research on compounds in this family M(I)M(III)(M(VI)O₄)₂ (M(I) = alkali metal, M(III) = Al, In, Sc, Fe, Bi, lanthanide; M(VI) = Mo, W). The vibrational modes, structure transformation, and Al coordination of crystalline, glassy, and molten states of KAl(MoO₄)₂ have been investigated by in-situ high temperature Raman scattering and (27)Al magic angle spinning nuclear magnetic resonance (MAS NMR) spectroscopy, together with first principles density functional simulation of room temperature Raman spectrum. The results showed that, under the present fast quenching conditions, Al is present predominantly in [AlO₆] octahedra in both KAl(MoO₄)₂ glass and melt, with the tetrahedrally coordinated Al being minor at approximately 2.7%. The effect of K⁺, from ordered arrangement in the crystal to random distribution in the melt, on the local chemical environment of Al, was also revealed. The distribution and quantitative analysis of different Al coordination subspecies are final discussed and found to be dependent on the thermal history of the glass samples.

  13. Modelling of the vapour-liquid equilibrium of water and the in situ concentration of H3PO4 in a high temperature proton exchange membrane fuel cell

    NASA Astrophysics Data System (ADS)

    Kazdal, Timur J.; Lang, Sebastian; Kühl, Frank; Hampe, Manfred J.

    2014-03-01

    The fuel cell technology is a key element for the hydrogen energy economy and therefore crucial for sustainable development. High temperature proton exchange membrane (HT-PEM) fuel cells (FC) can be operated with reformate gas and thus represent an important bridging technology for the energy transition to a renewable energy based system. HT-PEM FCs based on phosphoric acid (PA) are still subject to intense research, investigating the electrolyte behaviour. By enhancing state of the art 2D FEM simulations of FCs with the vapour liquid equilibrium of water-phosphoric acid and evaporation kinetics, a model was created in which the local concentration of PA can be calculated. Knowledge of the concentration field yields the basis for calculating the locally varying ionic conductivity and other physical properties. By describing the volume expansion behaviour of PA it was possible to predict the catalyst particle deactivation due to the swelling of PA. The in situ concentration predicted by the simulation ranges from 96 to 111 wt%. The model was validated using measured data of a single cell design for different temperatures and pressures. By varying the PA content flooding of the simulated fuel cell could be observed and was linked to humidification effects.

  14. Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

    SciTech Connect

    Haboub, Abdel; Nasiatka, James R.; MacDowell, Alastair A.; Bale, Hrishikesh A.; Cox, Brian N.; Marshall, David B.; Ritchie, Robert O.

    2014-08-15

    A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C.

  15. Tensile testing of materials at high temperatures above 1700 °C with in situ synchrotron X-ray micro-tomography

    NASA Astrophysics Data System (ADS)

    Haboub, Abdel; Bale, Hrishikesh A.; Nasiatka, James R.; Cox, Brian N.; Marshall, David B.; Ritchie, Robert O.; MacDowell, Alastair A.

    2014-08-01

    A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C.

  16. In Situ Synthesis of Porous Carbons by Using Room-Temperature, Atmospheric-Pressure Dielectric Barrier Discharge Plasma as High-Performance Adsorbents for Solid-Phase Microextraction.

    PubMed

    Lin, Yao; Wu, Li; Xu, Kailai; Tian, Yunfei; Hou, Xiandeng; Zheng, Chengbin

    2015-09-21

    A one-step, template-free method is described to synthesize porous carbons (PCs) in situ on a metal surface by using a room-temperature, atmospheric-pressure dielectric barrier discharge (DBD) plasma. This method not only features high efficiency, environmentally friendliness, and low cost and simple equipment, but also can conveniently realize large-area synthesis of PCs by only changing the design of the DBD reactor. The synthesized PCs have a regulated nestlike morphology, and thus, provide a high specific surface area and high pore volume, which result in excellent adsorption properties. Its applicability was demonstrated by using a PC-coated stainless-steel fiber as a solid-phase microextraction (SPME) fiber to preconcentrate polycyclic aromatic hydrocarbons (PAHs) prior to analysis by gas chromatography with flame ionization detection (GC-FID). The results showed that the fiber exhibited excellent enrichment factors (4.1×10(4) to 3.1×10(5)) toward all tested PAHs. Thus, the PC-based SPME-GC-FID provides low limits of detection (2 to 20 ng L(-1)), good precision (<7.8%), and good recoveries (80-115%) for ultra-sensitive determination of PAHs in real water samples. In addition, the PC-coated fiber could be stable enough for more than 500 replicate extraction cycles.

  17. Diamond Nucleation from Amorphous Carbon and Graphite with COH Fluids: an in Situ High Pressure and Temperature Laser-Heated Diamond Anvil Cell Experimental Study

    NASA Astrophysics Data System (ADS)

    Zhang, J.; Prakapenka, V.; Kubo, A.; Kavner, A.; Green, H. W.; Dobrzhinetskaya, L. F.

    2007-12-01

    Microdiamonds from orogenic belts contain nanometer size fluid inclusions suggesting diamond formation from supercritical COH fluids. Previous studies have shown that diamonds synthesized from high pressure and temperature experiments with supercritical COH fluids are characterized by skeletal morphology and solid oxide inclusions. However, mechanism and kinetics of graphite/carbon-to-diamond transformation promoted by COH fluids at high pressure and high temperature conditions are not well understood. Here we report in situ observations of diamond nucleation from COH fluids in laser-heated diamond anvil cell. Our experimental starting materials were amorphous carbon (impurity < 2ppm) and graphite (99.9% pure). Oxalic acid dihydrate (COOH)2·2H2O) was added to amorphous carbon and glucose (C6H12O6) was added to both amorphous carbon and graphite. The organic compounds (3 wt.%) provide CO2- and CH4-rich fluid environments respectively during their breakdown at high pressure and temperature. The mixtures were kept at temperature of 1400-1700 °C and pressure of 8-10 GPa for 10-30 minutes. Experiments show that only nanocrystals of diamond were nucleated from amorphous carbon in CO2-rich fluid environment. The fastest rate of diamond nucleation and growth of ~15 micron size crystals was found in the mixture of amorphous carbon with glucose (CH4-rich environment), whereas only nanocrystalline nuclei were produced in the mixture of graphite with glucose. We have also established that under anhydrous conditions, no diamond nucleation occurred in pure graphite, and only nanocrystals of diamond were observed in the amorphous carbon starting material at temperatures 1700-1900 °C. Our results revealed that the kinetics of diamond nucleation depend on the ¡°precursor¡±: diamond nucleates and grows faster from amorphous carbon than from graphite in the presence of COH fluid; in our anhydrous experiments diamond nucleates only from amorphous carbon. These results

  18. In situ Growth of NixCu1-x Alloy Nanocatalysts on Redox-reversible Rutile (Nb,Ti)O4 Towards High-Temperature Carbon Dioxide Electrolysis

    PubMed Central

    Wei, Haoshan; Xie, Kui; Zhang, Jun; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Cui, Jiewu; Yan, Jian; Wu, Yucheng

    2014-01-01

    In this paper, we report the in situ growth of NixCu1-x (x = 0, 0.25, 0.50, 0.75 and 1.0) alloy catalysts to anchor and decorate a redox-reversible Nb1.33Ti0.67O4 ceramic substrate with the aim of tailoring the electrocatalytic activity of the composite materials through direct exsolution of metal particles from the crystal lattice of a ceramic oxide in a reducing atmosphere at high temperatures. Combined analysis using XRD, SEM, EDS, TGA, TEM and XPS confirmed the completely reversible exsolution/dissolution of the NixCu1-x alloy particles during the redox cycling treatments. TEM results revealed that the alloy particles were exsolved to anchor onto the surface of highly electronically conducting Nb1.33Ti0.67O4 in the form of heterojunctions. The electrical properties of the nanosized NixCu1-x/Nb1.33Ti0.67O4 were systematically investigated and correlated to the electrochemical performance of the composite electrodes. A strong dependence of the improved electrode activity on the alloy compositions was observed in reducing atmospheres at high temperatures. Direct electrolysis of CO2 at the NixCu1-x/Nb1.33Ti0.67O4 composite cathodes was investigated in solid-oxide electrolysers. The CO2 splitting rates were observed to be positively correlated with the Ni composition; however, the Ni0.75Cu0.25 combined the advantages of metallic nickel and copper and therefore maximised the current efficiencies. PMID:24889679

  19. In situ growth of Ni(x)Cu(1-x) alloy nanocatalysts on redox-reversible rutile (Nb,Ti)O₄ towards high-temperature carbon dioxide electrolysis.

    PubMed

    Wei, Haoshan; Xie, Kui; Zhang, Jun; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Cui, Jiewu; Yan, Jian; Wu, Yucheng

    2014-06-03

    In this paper, we report the in situ growth of Ni(x)Cu(1-x) (x = 0, 0.25, 0.50, 0.75 and 1.0) alloy catalysts to anchor and decorate a redox-reversible Nb1.33Ti0.67O4 ceramic substrate with the aim of tailoring the electrocatalytic activity of the composite materials through direct exsolution of metal particles from the crystal lattice of a ceramic oxide in a reducing atmosphere at high temperatures. Combined analysis using XRD, SEM, EDS, TGA, TEM and XPS confirmed the completely reversible exsolution/dissolution of the Ni(x)Cu(1-x) alloy particles during the redox cycling treatments. TEM results revealed that the alloy particles were exsolved to anchor onto the surface of highly electronically conducting Nb1.33Ti0.67O4 in the form of heterojunctions. The electrical properties of the nanosized Ni(x)Cu(1-x)/Nb1.33Ti0.67O4 were systematically investigated and correlated to the electrochemical performance of the composite electrodes. A strong dependence of the improved electrode activity on the alloy compositions was observed in reducing atmospheres at high temperatures. Direct electrolysis of CO2 at the Ni(x)Cu(1-x)/Nb1.33Ti0.67O4 composite cathodes was investigated in solid-oxide electrolysers. The CO2 splitting rates were observed to be positively correlated with the Ni composition; however, the Ni0.75Cu0.25 combined the advantages of metallic nickel and copper and therefore maximised the current efficiencies.

  20. In situ Growth of NixCu1-x Alloy Nanocatalysts on Redox-reversible Rutile (Nb,Ti)O4 Towards High-Temperature Carbon Dioxide Electrolysis

    NASA Astrophysics Data System (ADS)

    Wei, Haoshan; Xie, Kui; Zhang, Jun; Zhang, Yong; Wang, Yan; Qin, Yongqiang; Cui, Jiewu; Yan, Jian; Wu, Yucheng

    2014-06-01

    In this paper, we report the in situ growth of NixCu1-x (x = 0, 0.25, 0.50, 0.75 and 1.0) alloy catalysts to anchor and decorate a redox-reversible Nb1.33Ti0.67O4 ceramic substrate with the aim of tailoring the electrocatalytic activity of the composite materials through direct exsolution of metal particles from the crystal lattice of a ceramic oxide in a reducing atmosphere at high temperatures. Combined analysis using XRD, SEM, EDS, TGA, TEM and XPS confirmed the completely reversible exsolution/dissolution of the NixCu1-x alloy particles during the redox cycling treatments. TEM results revealed that the alloy particles were exsolved to anchor onto the surface of highly electronically conducting Nb1.33Ti0.67O4 in the form of heterojunctions. The electrical properties of the nanosized NixCu1-x/Nb1.33Ti0.67O4 were systematically investigated and correlated to the electrochemical performance of the composite electrodes. A strong dependence of the improved electrode activity on the alloy compositions was observed in reducing atmospheres at high temperatures. Direct electrolysis of CO2 at the NixCu1-x/Nb1.33Ti0.67O4 composite cathodes was investigated in solid-oxide electrolysers. The CO2 splitting rates were observed to be positively correlated with the Ni composition; however, the Ni0.75Cu0.25 combined the advantages of metallic nickel and copper and therefore maximised the current efficiencies.

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

    NASA Astrophysics Data System (ADS)

    Yan, Zilin; Martin, Christophe L.; Bouvard, Didier; Jauffrès, David; Lhuissier, Pierre; Salvo, Luc; Olmos, Luis; Villanova, Julie; Guillon, Olivier

    2017-06-01

    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.

  2. A multipurpose ultra-high vacuum-compatible chamber for in situ X-ray surface scattering studies over a wide range of temperature and pressure environment conditions

    NASA Astrophysics Data System (ADS)

    Ferrer, P.; Rubio-Zuazo, J.; Heyman, C.; Esteban-Betegón, F.; Castro, G. R.

    2013-03-01

    A low/high temperature (60-1000K) and pressure (10-10-3x103 mbar) "baby chamber", specially adapted to the grazing-incidence X-ray scattering station, has been designed, developed and installed at the Spanish CRG BM25 SpLine beamline at European Synchrotron Radiation Facility. The chamber has a cylindrical form with 100 mm of diameter, built on a 360° beryllium nipple of 150 mm height. The UHV equipment and a turbo pump are located on the upper part of the chamber to leave a wide solid angle for exploring reciprocal space. The chamber features 4 CF16 and 5 CF40 ports for electrical feed through and leak valves, ion gun, etc. The heat exchanger is a customized compact LN2 (or LHe) continuous flow cryostat. The sample is mounted on a Mo support on the heat exchanger, which has in the back side a BORALECTRIC® Heater Elements. Experiments of surfaces/interfaces/ multilayer materials, thin films or single crystals in a huge variety of environments can be performed, also in situ studies of growth or evolution of the samples. Data measurement can be collected with a punctual and a bi-dimensional detector, being possible to simultaneously use them.

  3. The use of in situ powder X-ray diffraction in the investigation of dolomite as a potential reversible high-temperature CO2 sorbent.

    PubMed

    Readman, Jennifer E; Blom, Richard

    2005-03-21

    We report the use of gas sorption experiments and in situ powder X-ray diffraction to study the use of dolomite (MgCa(CO3)2) as a potential reversible high-temperature CO2 sorbent. When dolomite is treated in inert atmosphere at 900 degrees C it decomposes into separate CaO and MgO rich phases and dolomite is never reformed pon CO2 sorption. Gas sorption studies show that the calcined dolomite can go through several cycles of CO2 sorption/desorption in a reversible manner, however, the sorption capacity diminishes with each cycle. Only calcium seems to be involved in the CO2 sorption, while MgO acts as a carrier for the calcium phase. Some evidence of magnesium contamination of the calcium phase was found. BET and SEM measurements were carried out to find differences in the surface area/particle morphology that may explain similarities in the sorption capacities of dolomite and calcite (CaCO3).

  4. Frictional properties of Zuccale Fault rocks from room temperature to in-situ conditions: results from high strain rotary shear experiments

    NASA Astrophysics Data System (ADS)

    Niemeijer, A. R.; Collettini, C.; Smith, S.; Spiers, C.

    2011-12-01

    The Zuccale fault is a regionally-important, low-angle normal fault, exposed on the Isle of Elba in Central Italy, that accommodated a total shear displacement of 6-8 km.The fault zone structure and fault rocks formed at less than 8 km crustal depth. The present-day fault structure is the final product of several deformation processes superposed during the fault history. Here, we focus on a series of highly foliated and phyllosilicate-rich fault rocks that represent the basal horizon of the detachment. Previous experimental work on foliated, intact samples, sheared in their in-situ microstructural (foliated) condition, demonstrated a markedly lower friction coefficient compared to homogeneously mixed powdered samples of the same material. We concluded from these experiments that the existence of a continuous, through-going foliation provides numerous planes of weakness on which shear deformation could be accommodated. However, these experiments were performed under room-dry and room temperature conditions. Moreover, the question remains as to how foliation is formed in these rocks in the first place. In this study, we report results from a series of preliminary rotary shear experiments performed on two fault rock types obtained from the Zuccale Fault. The tests were done under conditions ranging from room temperature to in-situ conditions (i.e. at temperatures up to 350 °C, applied normal stresses up to 200 MPa and fluid-saturated). Samples consisting of calcite, talc, chlorite and kaolinite (sample ZF01) and of calcite, tremolite, hornblende, kaolinite, chlorite and quartz (sample ZF02) were sheared at sliding velocities of 0.3-300 μm/s to displacements larger than 40 mm (i.e. γ > 40). Sample ZF01 was weaker than sample ZF02 at all conditions investigated. We attribute the lower strength to the weak talc present in this sample which is absent in sample ZF02. Both samples showed inherently stable, velocity-strengthening behaviour at room temperature, in

  5. Experimental method for in situ determination of material textures at simultaneous high pressure and high temperature by means of radial diffraction in the diamond anvil cell.

    PubMed

    Liermann, Hanns-Peter; Merkel, Sébastien; Miyagi, Lowell; Wenk, Hans-Rudolf; Shen, Guoyin; Cynn, Hyunchae; Evans, William J

    2009-10-01

    We introduce the design and capabilities of a resistive heated diamond anvil cell that can be used for side diffraction at simultaneous high pressure and high temperature. The device can be used to study lattice-preferred orientations in polycrystalline samples up to temperatures of 1100 K and pressures of 36 GPa. Capabilities of the instrument are demonstrated with preliminary results on the development of textures in the bcc, fcc, and hcp polymorphs of iron during a nonhydrostatic compression experiment at simultaneous high pressure and high temperature.

  6. High temperature and low field regime vortex phase diagram of in-situ prepared stainless steel sheathed MgB2 tapes

    NASA Astrophysics Data System (ADS)

    Rajput, Suchitra

    2017-04-01

    A magnetic field-temperature vortex phase diagram has been proposed for MgB2 on the basis of magnetoresistance studies performed on an in-situ prepared stainless steel sheathed MgB2 tapes. Thermally activated flux flow (TAFF) behavior is analyzed using Arrhenius relation. Low dissipative part of magnetoresistance with temperature is well described by vortex glass theory. Above critical region, the resistive behavior is influenced by fluctuation conductivity. In addition, a considerable vortex liquid region below HC2 is also observed but TAFF region is found to be quite narrow.

  7. Six Month In Situ High-Resolution Carbonate Chemistry and Temperature Study on a Coral Reef Flat Reveals Asynchronous pH and Temperature Anomalies

    PubMed Central

    Kline, David I.; Teneva, Lida; Hauri, Claudine; Schneider, Kenneth; Miard, Thomas; Chai, Aaron; Marker, Malcolm; Dunbar, Rob; Caldeira, Ken; Lazar, Boaz; Rivlin, Tanya; Mitchell, Brian Gregory; Dove, Sophie; Hoegh-Guldberg, Ove

    2015-01-01

    Understanding the temporal dynamics of present thermal and pH exposure on coral reefs is crucial for elucidating reef response to future global change. Diel ranges in temperature and carbonate chemistry parameters coupled with seasonal changes in the mean conditions define periods during the year when a reef habitat is exposed to anomalous thermal and/or pH exposure. Anomalous conditions are defined as values that exceed an empirically estimated threshold for each variable. We present a 200-day time series from June through December 2010 of carbonate chemistry and environmental parameters measured on the Heron Island reef flat. These data reveal that aragonite saturation state, pH, and pCO2 were primarily modulated by biologically-driven changes in dissolved organic carbon (DIC) and total alkalinity (TA), rather than salinity and temperature. The largest diel temperature ranges occurred in austral spring, in October (1.5 – 6.6°C) and lowest diel ranges (0.9 – 3.2°C) were observed in July, at the peak of winter. We observed large diel total pH variability, with a maximum range of 7.7 – 8.5 total pH units, with minimum diel average pH values occurring during spring and maximum during fall. As with many other reefs, the nighttime pH minima on the reef flat were far lower than pH values predicted for the open ocean by 2100. DIC and TA both increased from June (end of Fall) to December (end of Spring). Using this high-resolution dataset, we developed exposure metrics of pH and temperature individually for intensity, duration, and severity of low pH and high temperature events, as well as a combined metric. Periods of anomalous temperature and pH exposure were asynchronous on the Heron Island reef flat, which underlines the importance of understanding the dynamics of co-occurrence of multiple stressors on coastal ecosystems. PMID:26039687

  8. Six Month In Situ High-Resolution Carbonate Chemistry and Temperature Study on a Coral Reef Flat Reveals Asynchronous pH and Temperature Anomalies.

    PubMed

    Kline, David I; Teneva, Lida; Hauri, Claudine; Schneider, Kenneth; Miard, Thomas; Chai, Aaron; Marker, Malcolm; Dunbar, Rob; Caldeira, Ken; Lazar, Boaz; Rivlin, Tanya; Mitchell, Brian Gregory; Dove, Sophie; Hoegh-Guldberg, Ove

    2015-01-01

    Understanding the temporal dynamics of present thermal and pH exposure on coral reefs is crucial for elucidating reef response to future global change. Diel ranges in temperature and carbonate chemistry parameters coupled with seasonal changes in the mean conditions define periods during the year when a reef habitat is exposed to anomalous thermal and/or pH exposure. Anomalous conditions are defined as values that exceed an empirically estimated threshold for each variable. We present a 200-day time series from June through December 2010 of carbonate chemistry and environmental parameters measured on the Heron Island reef flat. These data reveal that aragonite saturation state, pH, and pCO2 were primarily modulated by biologically-driven changes in dissolved organic carbon (DIC) and total alkalinity (TA), rather than salinity and temperature. The largest diel temperature ranges occurred in austral spring, in October (1.5 - 6.6°C) and lowest diel ranges (0.9 - 3.2°C) were observed in July, at the peak of winter. We observed large diel total pH variability, with a maximum range of 7.7 - 8.5 total pH units, with minimum diel average pH values occurring during spring and maximum during fall. As with many other reefs, the nighttime pH minima on the reef flat were far lower than pH values predicted for the open ocean by 2100. DIC and TA both increased from June (end of Fall) to December (end of Spring). Using this high-resolution dataset, we developed exposure metrics of pH and temperature individually for intensity, duration, and severity of low pH and high temperature events, as well as a combined metric. Periods of anomalous temperature and pH exposure were asynchronous on the Heron Island reef flat, which underlines the importance of understanding the dynamics of co-occurrence of multiple stressors on coastal ecosystems.

  9. Thermal stability of the Mobil Five type metallosilicate molecular sieves-An in situ high temperature X-ray diffraction study

    SciTech Connect

    Bhange, D.S.; Ramaswamy, Veda . E-mail: v.ramaswamy@ncl.res.in

    2007-05-03

    We have carried out in situ high temperature X-ray diffraction (HTXRD) studies of silicalite-1 (S-1) and metallosilicate molecular sieves containing iron, titanium and zirconium having Mobil Five (MFI) structure (iron silicalite-1 (FeS-1), titanium silicalite-1 (TS-1) and zirconium silicalite-1 (ZrS-1), respectively) in order to study the thermal stability of these materials. Isomorphous substitution of Si{sup 4+} by metal atoms is confirmed by the expansion of unit cell volume by X-ray diffraction (XRD) and the presence of Si-O-M stretching band at {approx}960 cm{sup -1} by Fourier transform infrared (FTIR) spectroscopy. Appearance of cristobalite phase is seen at 1023 and 1173 K in S-1 and FeS-1 samples. While the samples S-1 and FeS-1 decompose completely to cristobalite at 1173 and 1323 K, respectively, the other two samples are thermally stable upto 1623 K. This transformation is irreversible. Although all materials show a negative lattice thermal expansion, their lattice thermal expansion coefficients vary. The thermal expansion behavior in all samples is anisotropic with relative strength of contraction along 'a' axes is more than along 'b' and 'c' axes in S-1, TS-1, ZrS-1 and vice versa in FeS-1. Lattice thermal expansion coefficients ({alpha} {sub v}) in the temperature range 298-1023 K were -6.75 x 10{sup -6} K{sup -1} for S-1, -12.91 x 10{sup -6} K{sup -1} for FeS-1, -16.02 x 10{sup -6} K{sup -1} for TS-1 and -17.92 x 10{sup -6} K{sup -1} for ZrS-1. The highest lattice thermal expansion coefficients ({alpha} {sub v}) obtained were -11.53 x 10{sup -6} K{sup -1} for FeS-1 in temperature range 298-1173 K, -20.86 x 10{sup -6} K{sup -1} for TS-1 and -25.54 x 10{sup -6} K{sup -1} for ZrS-1, respectively, in the temperature range 298-1623 K. Tetravalent cation substitution for Si{sup 4+} in the lattice leads to a high thermal stability as compared to substitution by trivalent cations.

  10. Frictional properties of Zuccale Fault rocks from room temperature to in-situ conditions: results from high strain rotary shear experiments

    NASA Astrophysics Data System (ADS)

    Niemeijer, A.; Collettini, C.; Smith, S. A. F.; Spiers, C. J.

    2012-04-01

    The Zuccale fault is a regionally-important, low-angle normal fault, exposed on the Isle of Elba in Central Italy, that accommodated a total shear displacement of 6-8 km.The fault zone structure and fault rocks formed at less than 8 km crustal depth. The present-day fault structure is the final product of several deformation processes superposed during the fault history. Here, we focus on a series of highly foliated and phyllosilicate-rich fault rocks that represent the basal horizon of the detachment. Previous experimental work on foliated, intact samples, sheared in their in-situ microstructural (foliated) condition, demonstrated a markedly lower friction coefficient compared to homogeneously mixed powdered samples of the same material. In this study, we report results from a series of rotary shear experiments performed on 1 mm thick powdered gouges made from several fault rock types obtained from the Zuccale Fault. The tests were done under conditions ranging from room temperature to in-situ conditions (i.e. at temperatures up to 300 °C, applied normal stresses up to 200 MPa and fluid-saturated.) The ratio of fluid pressure to effective normal stress was held constant at either λ=0.4 or λ=0.8 to simulate an over-pressurized fault. The samples were sheared at a constant sliding velocity of 10 μm/s for at least 5 mm, after which a velocity-stepping sequence from 1 to 300 μm/s was started to determine the velocity dependence of friction. This can be represented by the rate-and-state parameter (a-b), which was determined by an inversion of the data to the rate-and-state equations. Friction of the various fault rocks is between 0.3 and 0.7, similar to values obtained in a previous study, and decreases with increasing phyllosilicate content. Friction decreases mildly with temperature whereas normal stress and fluid pressure do not affect friction values systematically. All samples exhibited velocity-strengthening, inherently stable behavior under room temperature

  11. Determination of the Phase Boundary Fe3O4 - h-Fe3O4 at high Temperature and Pressure using in situ Synchroton Radiation

    NASA Astrophysics Data System (ADS)

    Schollenbruch, K.; Woodland, A. B.; Frost, D. J.; Wang, Y.; Sanehira, T.

    2009-12-01

    Magnetite is an important accessory mineral in the Earth’s mantle and its rare occurrence as inclusions in diamonds means that this phase has a direct relevance to geochemical processes in the deep earth. For this reason it is important to define its thermodynamic behaviour at high P and T. Magnetite transforms to an orthorhombic high-pressure phase (h-Fe3O4) at room T and ~25 GPa, however the reaction is very sluggish and h-Fe3O4 is unquenchable, complicating the determination of the exact position of the phase boundary at low T. For this reason the phase transition has been investigated by a combination of a multianvil press and in situ X-ray diffraction measurements performed at the Advanced Photo Source (APS) at Argonne National Laboratory, U.S.A.. With this setup, pressure can be monitored during an experiment, allowing different P-T trajectories to be employed (i.e. pressurisation at high T) compared to conventional methods. Experiments were performed up to 15 GPa and 1400°C. A series of measurements during pressurisation at different temperatures revealed, that diffraction peaks related to h-Fe3O4 appeared at the expense of magnetite peaks at about 10 GPa. At the onset of the phase transition, the pressure decreased slightly due to pressure buffering from the 7% volume reduction attending the transition. However, the strongest magnetite reflections remained even at the highest P and T, underlining the sluggishness of the reaction. Measurements made while tracking down P at high T provided reversals, where the regrowth of magnetite diffraction peaks were observed. Once formed, h-Fe3O4 remains metastable down to nearly ambient conditions. Post-experiment TEM investigation revealed extensive twinning and other microstructures, confirming the interpretation of Frost et al. (2001), that such structures formed during the reconversion to magnetite at low pressure. Our high P-T experiments indicate a nearly isobaric phase boundary over a range of 800-1400

  12. The thermal equation of state of FeTiO[subscript 3] ilmenite based on in situ X-ray diffraction at high pressures and temperatures

    SciTech Connect

    Tronche, E.J.; Van Kan Parker, M.; De Vries, J.; Wang, Y.; Sanehire, T.; Li, J.; Chen, B.; Gao, L.; Klemme, S.; McCammon, C.A.; Van Westerenen, W.

    2010-11-12

    We present in situ measurements of the unit-cell volume of a natural terrestrial ilmenite (Jagersfontein mine, South Africa) and a synthetic reduced ilmenite (FeTiO{sub 3}) at simultaneous high pressure and high temperature up to 16 GPa and 1273 K. Unit-cell volumes were determined using energy-dispersive synchrotron X-ray diffraction in a multi-anvil press. Moessbauer analyses show that the synthetic sample contained insignificant amounts of Fe{sup 3+} both before and after the experiment. Results were fit to Birch-Murnaghan thermal equations of state, which reproduce the experimental data to within 0.5 and 0.7 GPa for the synthetic and natural samples, respectively. At ambient conditions, the unit-cell volume of the natural sample [V{sub 0} = 314.75 {+-} 0.23 (1{sigma}) {angstrom}{sup 3}] is significantly smaller than that of the synthetic sample [V{sub 0} = 319.12 {+-} 0.26 {angstrom}{sup 3}]. The difference can be attributed to the presence of impurities and Fe{sup 3+} in the natural sample. The 1 bar isothermal bulk moduli K{sub T0} for the reduced ilmenite is slightly larger than for the natural ilmenite (181 {+-} 7 and 165 {+-} 6 GPa, respectively), with pressure derivatives K{prime}{sup 0} = 3 {+-} 1. Our results, combined with literature data, suggest that the unit-cell volume of reduced ilmenite is significantly larger than that of oxidized ilmenite, whereas their thermoelastic parameters are similar. Our data provide more appropriate input parameters for thermo-chemical models of lunar interior evolution, in which reduced ilmenite plays a critical role.

  13. Evidence for high-temperature in situ nifH transcription in an alkaline hot spring of Lower Geyser Basin, Yellowstone National Park.

    PubMed

    Loiacono, Sara T; Meyer-Dombard, D'Arcy R; Havig, Jeff R; Poret-Peterson, Amisha T; Hartnett, Hilairy E; Shock, Everett L

    2012-05-01

    Genes encoding nitrogenase (nifH) were amplified from sediment and photosynthetic mat samples collected in the outflow channel of Mound Spring, an alkaline thermal feature in Yellowstone National Park. Results indicate the genetic capacity for nitrogen fixation over the entire range of temperatures sampled (57.2°C to 80.2°C). Amplification of environmental nifH transcripts revealed in situ expression of nifH genes at temperatures up to 72.7°C. However, we were unable to amplify transcripts of nifH at the higher-temperature locations (> 72.7°C). These results indicate that microbes at the highest temperature sites contain the genetic capacity to fix nitrogen, yet either do not express nifH or do so only transiently. Field measurements of nitrate and ammonium show fixed nitrogen limitation as temperature decreases along the outflow channel, suggesting nifH expression in response to the downstream decrease in bioavailable nitrogen. Nitrogen stable isotope values of Mound Spring sediment communities further support geochemical and genetic data. DNA and cDNA nifH amplicons form several unique phylogenetic clades, some of which appear to represent novel nifH sequences in both photosynthetic and chemosynthetic microbial communities. This is the first report of in situ nifH expression in strictly chemosynthetic zones of terrestrial (non-marine) hydrothermal systems, and sets a new upper temperature limit (72.7°C) for nitrogen fixation in alkaline, terrestrial hydrothermal environments.

  14. In Situ Characterization of Ge Nanocrystals Near the Growth Temperature

    SciTech Connect

    Sharp, I.D.; Xu, Q.; Liao, C.Y.; Chrzan, D.C.; Haller, E.E.; Yi, D.O.; Beeman, J.W.; Liliental-Weber, Z.; Yu, K.M.; Zakharov, D.N.; Ager, J.W. III

    2005-06-30

    We present in situ electron diffraction data indicating that Ge nanocrystals embedded in a silica matrix can be solid at temperatures exceeding the bulk Ge melting point. Supercooling is observed when returning from temperatures above the melting point of the Ge nanocrystals. Since melting point hysteresis is observed, it is not clear if nanoclusters are solid or liquid during the initial growth process. Raman spectra of as-grown nanocrystals give a measure of compressive stress and in-situ Raman spectroscopy further confirms the presence of crystalline Ge above 800 deg. C.

  15. In Situ Characterization of Ge Nanocrystals Near the Growth Temperature

    NASA Astrophysics Data System (ADS)

    Sharp, I. D.; Xu, Q.; Yi, D. O.; Liao, C. Y.; Beeman, J. W.; Liliental-Weber, Z.; Yu, K. M.; Zakharov, D. N.; Ager, J. W.; Chrzan, D. C.; Haller, E. E.

    2005-06-01

    We present in situ electron diffraction data indicating that Ge nanocrystals embedded in a silica matrix can be solid at temperatures exceeding the bulk Ge melting point. Supercooling is observed when returning from temperatures above the melting point of the Ge nanocrystals. Since melting point hysteresis is observed, it is not clear if nanoclusters are solid or liquid during the initial growth process. Raman spectra of as-grown nanocrystals give a measure of compressive stress and in-situ Raman spectroscopy further confirms the presence of crystalline Ge above 800 °C.

  16. Highly efficient solid-state dye-sensitized solar cells based on hexylimidazolium iodide ionic polymer electrolyte prepared by in situ low-temperature polymerization

    NASA Astrophysics Data System (ADS)

    Wang, Guiqiang; Yan, Chao; Zhang, Juan; Hou, Shuo; Zhang, Wei

    2017-03-01

    Solid-state dye-sensitized solar cells (DSCs) are fabricated using a novel ionic polymer electrolyte containing hexylimidazolium iodide (HII) ionic polymer prepared by in situ polymerization of N,N‧-bis(imidazolyl) hexane and 1,6-diiodohexane without an initiator at low temperature (40 °C). The as-prepared HII ionic polymer has a similar structure to alkylimidazolium iodide ionic liquid, and the imidazolium cations are contained in the polymer main chain; so, it can act simultaneously as the redox mediator in the electrolyte. By incorporating an appropriate amount of 1,3-dimethylimidazolium iodide (DMII) in HII ionic polymer (DMII/HII ionic polymer = 0.7:1, weight ratio), the conductivity of the ionic polymer electrolyte is greatly improved due to the formation of Grotthuss bond exchange. In addition, in situ synthesis of ionic polymer electrolyte guarantees a good pore-filling of the electrolyte in the TiO2 photoanode. As a result, the solid-state DSC based on the ionic polymer electrolyte containing HII ionic polymer and DMII without iodine achieves a conversion efficiency of 6.55% under the illumination of 100 mW cm-2 (AM 1.5), which also exhibits a good at-rest stability at room temperature.

  17. Chemistry at high pressures and temperatures: in-situ synthesis and characterization of {beta}-Si{sub 3}N{sub 4} by DAC X-ray/laser-heating studies

    SciTech Connect

    Yoo, C.-S.; Akella, J.; Nicol, M.

    1996-01-01

    We have developed in-situ XRD technique at high pressures and temperatures by integrating the angle-resolved synchrotron XRD method, laser-heating system, and diamond anvil cell together. Using this technique, we have studied the direct elementary reactions of nitrogen with Si, yielding technologically important {beta}-Si{sub 3}N{sub 4}. These reactions do not occur at ambient temperatures at high pressures up to 50 GPa, but proceed exothermically at high temperatures at moderate pressures. It implies that the reaction is kinetically limited by a large activation barrier.

  18. Hybrid-type temperature sensor for in situ measurement

    SciTech Connect

    Iuchi, Tohru; Hiraka, Kensuke

    2006-11-15

    A hybrid-type surface temperature sensor combines the contact and noncontact methods, which allows us to overcome the shortcomings of both methods. The hybrid-type surface thermometer is composed mainly of two components: a metal film sheet that makes contact with an object and a radiometer that is used to detect the radiance of the rear surface of the metal film, which is actually a modified radiation thermometer. Temperature measurement using the hybrid-type thermometer with a several tens micrometer thick Hastelloy sheet, a highly heat and corrosion resistant alloy, is possible with a systematic error of -0.5 K and random errors of {+-}0.5 K, in the temperature range from 900 to 1000 K. This thermometer provides a useful means for calibration of in situ temperature measurement in various processes, especially in the silicon semiconductor industry. This article introduces the basic idea of the hybrid-type surface sensor, presents experimental results and discussions, and finally describes some applications.

  19. Isothermal nucleation and growth kinetics of Pd/Ag alloy phase via in-situ time-resolved high-temperature x-ray diffraction (HTXRD) analysis

    SciTech Connect

    Ayturk, Mahmut Engin; Payzant, E Andrew; Speakman, Scott A; Ma, Yi Hua

    2008-01-01

    Among several different approaches to form Pd/Ag alloys for hydrogen separation applications, ex-situ studies carried by conventional X-ray point scanning detectors might fail to reveal the key aspects of the phase transformation between Pd and Ag metals. In this respect, in-situ time-resolved high temperature X-ray diffraction (HTXRD) was employed to study the Pd/Ag alloy phase nucleation and growth kinetics. By the use of linear position sensitive detectors, advanced optics and profile fitting with the use of JADE-6.5 software, isothermal phase evolution of the Pd/Ag alloy at 500 C, 550 C and 600 C under hydrogen atmosphere were quantified to elucidate the mechanistic details of the Pd/Ag alloy phase nucleation and growth pattern. Analysis of the HTXRD data by the Avrami model indicated that the nucleation of the Pd/Ag alloy phase was instantaneous where the growth mechanism was through diffusion-controlled one-dimensional thickening of the Pd/Ag alloy layer. The value of the Avrami exponent, n, was found to increase with temperature with the values of 0.34, 0.39 and 0.67 at 500oC, 550oC and 600oC, respectively. In addition, parabolic rate law analysis suggested that the nucleation of the Pd/Ag alloy phase was through a heterogeneous nucleation mode, in which the nucleation sites were defined as the non-equilibrium defects. The cross-sectional SEI micrographs indicated that the Pd/Ag alloy phase growth was strongly dependent upon the deposition morphology of the as-synthesized Pd and Ag layers formed by the electroless plating. Based on the Avrami model and the parabolic rate law, the estimated activation energies for the phase transformation were 236.5 and 185.6 kJ/mol and in excellent agreement with the literature values (183-239.5 kJ/mol).

  20. Effects of temperature on in situ toxicity testing

    SciTech Connect

    Rowland, C.D.; Burton, G.A. Jr.

    1994-12-31

    With increasing concern over the impacts and perturbations to receiving waters as a result of storm water runoff and contaminated sediments, many investigators have turned towards in situ testing for direct response data. In situ testing has been shown to be an effective assessment tool. In order to further evaluate the limitations of this method, temperature effects were evaluated. There is concern that laboratory to stream transfer of test organisms may induce significant stress if water temperatures are too cool. This study was designed to specifically address the issue of temperature tolerance and attenuation of Hyalella azteca, Ceriodaphnia dubia and Pimephales promelas in in situ conditions. Temperature tolerance is of importance in areas where receiving waters are subject to low or fluctuating temperatures as well as areas of more temperate climates. In this study, the organisms where exposed to temperatures as low as 2 C for variable lengths of time, removed and allowed to come to ambient laboratory temperatures then monitored for acute or chronic responses. No effects on survival were observed after 48 h. at 5 C; however lower temperatures increased mortality.

  1. Determination of the phase boundary of the omega to beta transition in Zr using in situ high-pressure and high-temperature X-ray diffraction

    SciTech Connect

    Ono, Shigeaki; Kikegawa, Takumi

    2015-05-15

    The high-pressure behavior of zirconium has been examined using the synchrotron X-ray diffraction technique to a pressure of 38 GPa and a temperature of 800 K employing a hydrothermal diamond anvil cell technique. The structural transition from the ω to the β phase was observed. This transition has a negative dP/dT gradient, which is in general agreement with those reported in previous studies. The transition boundary was determined to be, P (GPa)=41.2–0.025×T (K). The negative slope of the transition, dP/dT, determined in our study using the diamond anvil cell technique was less than half that estimated by the previous study using a large press apparatus. - Graphical abstract: Experimental results and phase boundary of the ω–β transition in Zr. - Highlights: • X-ray diffraction patterns of zirconium were measured by the synchrotron experiments. • High-pressure experiments were performed by an external-heated diamond anvil cell. • Phase diagram of zirconium was determined at high pressures and high temperatures. • Phase boundary between omega and beta transition has a negative dP/dT slope.

  2. In situ determination of the spinel-post-spinel transition in Fe3O4 at high pressure and temperature by synchrotron X-ray diffraction

    SciTech Connect

    Schollenbruch, K; Woodland, A B; Frost, D J; Wang, Y; Sanehira, T; Langenhorst, F

    2011-08-10

    The position of the spinel-post-spinel phase transition in Fe3O4 has been determined in pressure-temperature space by in situ measurements using a multi-anvil press combined with white synchrotron radiation. Pressure measurement using the equation of state for MgO permitted pressure changes to be monitored at high temperature. The phase boundary was determined by the first appearance of diffraction peaks of the high-pressure polymorph (h-Fe3O4) during pressure increase and the disappearance of these peaks on pressure decrease along several isotherms. We intersected the phase boundary over the temperature interval of 700-1400 ºC. The boundary is linear and nearly isobaric, with a slightly positive slope. Post-experiment investigation by TEM confirms that the reverse reaction from h-Fe 3O4 to magnetite during decompression leads to the formation of microtwins on the (311) plane in the newly formed magnetite. Observations made during the phase transition suggest that the transition has a pseudomartensitic character, explaining in part why magnetite persists at conditions well within the stability field of h-Fe3O4, even at high temperatures. This study emphasizes the utility of studying phase transitions in situ at simultaneously high temperatures and pressures since the reaction kinetics may not be favorable at room temperature.

  3. Note: Heated sample platform for in situ temperature-programmed XPS.

    PubMed

    Samokhvalov, Alexander; Tatarchuk, Bruce J

    2011-07-01

    We present the design, fabrication, and performance of the multi-specimen heated platform for linear in situ heating during the Temperature-Programmed XPS (TPXPS). The platform is versatile, compatible with high vacuum (HV) and bakeout. The heater platform is tested under in situ linear heating of typical high surface area sorbent∕catalyst support--nanoporous TiO(2). The platform allows the TPXPS of multiple samples located on specimen disk that can be transferred in and out of the TPXPS chamber. Electric characteristics, temperature and pressure curves are provided. Heating power supply, PID temperature controller, data-logging hardware and software are described.

  4. Class H Oil Well Cement Hydration at Elevated Temperatures in the Presence of Retarding Agents: An In Situ High-Energy X-ray Diffraction Study

    SciTech Connect

    Jupe, Andrew C.; Wilkinson, Angus P.; Luke, Karen; Funkhouser, Gary P.

    2008-07-08

    In situ powder X-ray diffraction was used to examine the hydration of API Class H cement slurries, with a water-to-cement ratio of 0.394, at 66, 93, 121, and 177 C under autogenous pressure in the presence of varying amounts of the additives tartaric acid, modified lignosulfonate, and AMPS (2-acrylamido-2-methylpropanesulfonic acid) copolymer. All of these retarding agents inhibited the hydration of crystalline C{sub 3}S (Ca{sub 3}SiO{sub 5}), but other modes of action were also apparent. The formation of ettringite was suppressed when tartaric acid was used by itself or in combination with other additives. Changes in the hydration of C{sub 3}S vs time could not be correlated in a simple way with the observed pumping times for the cement slurries. The largest changes in pumping time as a function of temperature occurred in a temperature interval where ettringite/monosulfate decomposes and crystalline hydrogarnet starts to be formed.

  5. Temperature Calibration for In Situ Environmental Transmission Electron Microscopy Experiments

    PubMed Central

    Winterstein, JP; Lin, PA; Sharma, R

    2016-01-01

    In situ environmental transmission electron microscopy (ETEM) experiments require specimen heating holders to study material behavior in gaseous environments at elevated temperatures. In order to extract meaningful kinetic parameters, such as activation energies, it is essential to have a direct and accurate measurement of local sample temperature. This is particularly important if the sample temperature might fluctuate, for example when room temperature gases are introduced to the sample area. Using selected-area diffraction (SAD) in an ETEM, the lattice parameter of Ag nanoparticles was measured as a function of the temperature and pressure of hydrogen gas to provide a calibration of the local sample temperature. SAD permits measurement of temperature to an accuracy of ± 30 °C using Ag lattice expansion. Gas introduction can cause sample cooling of several hundred degrees celsius for gas pressures achievable in the ETEM. PMID:26441334

  6. Evaluation of MODIS Land Surface Temperature with In Situ Snow Surface Temperature from CREST-SAFE

    NASA Astrophysics Data System (ADS)

    Perez Diaz, C. L.; Lakhankar, T.; Romanov, P.; Munoz, J.; Khanbilvardi, R.; Yu, Y.

    2016-12-01

    This paper presents the procedure and results of a temperature-based validation approach for the Moderate Resolution Imaging Spectroradiometer (MODIS) Land Surface Temperature (LST) product provided by the National Aeronautics and Space Administration (NASA) Terra and Aqua Earth Observing System satellites using in situ LST observations recorded at the Cooperative Remote Sensing Science and Technology Center - Snow Analysis and Field Experiment (CREST-SAFE) during the years of 2013 (January-April) and 2014 (February-April). A total of 314 day and night clear-sky thermal images, acquired by the Terra and Aqua satellites, were processed and compared to ground-truth data from CREST-SAFE with a frequency of one measurement every 3 min. Additionally, this investigation incorporated supplementary analyses using meteorological CREST-SAFE in situ variables (i.e. wind speed, cloud cover, incoming solar radiation) to study their effects on in situ snow surface temperature (T-skin) and T-air. Furthermore, a single pixel (1km2) and several spatially averaged pixels were used for satellite LST validation by increasing the MODIS window size to 5x5, 9x9, and 25x25 windows for comparison. Several trends in the MODIS LST data were observed, including the underestimation of daytime values and nighttime values. Results indicate that, although all the data sets (Terra and Aqua, diurnal and nocturnal) showed high correlation with ground measurements, day values yielded slightly higher accuracy ( 1°C), both suggesting that MODIS LST retrievals are reliable for similar land cover classes and atmospheric conditions. Results from the CREST-SAFE in situ variables' analyses indicate that T-air is commonly higher than T-skin, and that a lack of cloud cover results in: lower T-skin and higher T-air minus T-skin difference (T-diff). Additionally, the study revealed that T-diff is inversely proportional to cloud cover, wind speed, and incoming solar radiation. Increasing the MODIS window size

  7. Miniature Fixed Points as Temperature Standards for In Situ Calibration of Temperature Sensors

    NASA Astrophysics Data System (ADS)

    Hao, X. P.; Sun, J. P.; Xu, C. Y.; Wen, P.; Song, J.; Xu, M.; Gong, L. Y.; Ding, L.; Liu, Z. L.

    2017-06-01

    Miniature Ga and Ga-In alloy fixed points as temperature standards are developed at National Institute of Metrology, China for the in situ calibration of temperature sensors. A quasi-adiabatic vacuum measurement system is constructed to study the phase-change plateaus of the fixed points. The system comprises a high-stability bath, a quasi-adiabatic vacuum chamber and a temperature control and measurement system. The melting plateau of the Ga fixed point is longer than 2 h at 0.008 W. The standard deviation of the melting temperature of the Ga and Ga-In alloy fixed points is better than 2 mK. The results suggest that the melting temperature of the Ga or Ga-In alloy fixed points is linearly related with the heating power.

  8. Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr(2+) high temperature irradiation.

    PubMed

    Brooks, Adam J; Yao, Zhongwen

    2017-10-01

    The data presented in this article is related to the research experiment, titled: 'Quasi in-situ energy dispersive X-ray spectroscopy observation of matrix and solute interactions on Y-Ti-O oxide particles in an austenitic stainless steel under 1 MeV Kr(2+) high temperature irradiation' (Brooks et al., 2017) [1]. Quasi in-situ analysis during 1 MeV Kr(2+) 520 °C irradiation allowed the same microstructural area to be observed using a transmission electron microscope (TEM), on an oxide dispersion strengthened (ODS) austenitic stainless steel sample. The data presented contains two sets of energy dispersive X-ray spectroscopy (EDX) data collected before and after irradiation to 1.5 displacements-per-atom (~1.25×10(-3) dpa/s with 7.5×10(14) ions cm(-2)). The vendor software used to process and output the data is the Bruker Esprit v1.9 suite. The data includes the spectral (counts vs. keV energy) of the quasi in-situ scanned region (512×512 pixels at 56k magnification), along with the EDX scanning parameters. The.raw files from the Bruker Esprit v1.9 output are additionally included along with the.rpl data information files. Furthermore included are the two quasi in-situ HAADF images for visual comparison of the regions before and after irradiation. This in-situ experiment is deemed 'quasi' due to the thin foil irradiation taking place at an external TEM facility. We present this data for critical and/or extended analysis from the scientific community, with applications applying to: experimental data correlation, confirmation of results, and as computer based modeling inputs.

  9. High-temperature tensile cell for in situ real-time investigation of carbon fibre carbonization and graphitization processes

    SciTech Connect

    Behr, Michael; Rix, James; Landes, Brian; Barton, Bryan; Billovits, Gerry; Hukkanen, Eric; Patton, Jasson; Wang, Weijun; Keane, Denis; Weigand, Steven

    2016-10-17

    A new high-temperature fibre tensile cell is described, developed for use at the Advanced Photon Source at Argonne National Laboratory to enable the investigation of the carbonization and graphitization processes during carbon fibre production. This cell is used to heat precursor fibre bundles to temperatures up to ~2300°C in a controlled inert atmosphere, while applying tensile stress to facilitate formation of highly oriented graphitic microstructure; evolution of the microstructure as a function of temperature and time during the carbonization and higher-temperature graphitization processes can then be monitored by collecting real-time wide-angle X-ray diffraction (WAXD) patterns. As an example, the carbonization and graphitization behaviour of an oxidized polyacrylonitrile fibre was studied up to a temperature of ~1750°C. Real-time WAXD revealed the gradual increase in microstructure alignment with the fibre axis with increasing temperature over the temperature range 600–1100°C. Above 1100°C, no further changes in orientation were observed. The overall magnitude of change increased with increasing applied tensile stress during carbonization. As a second example, the high-temperature graphitizability of PAN- and pitch-derived commercial carbon fibres was studied. Here, the magnitude of graphitic microstructure evolution of the pitch-derived fibre far exceeded that of the PAN-derived fibres at temperatures up to ~2300°C, indicating its facile graphitizability.

  10. Preparation of W-Ta thin-film thermocouple on diamond anvil cell for in-situ temperature measurement under high pressure

    SciTech Connect

    Yang Jie; Li Ming; Zhang Honglin; Gao Chunxiao

    2011-04-15

    In this paper, a W-Ta thin-film thermocouple has been integrated on a diamond anvil cell by thin-film deposition and photolithography methods. The thermocouple was calibrated and its thermal electromotive force was studied under high pressure. The results indicate that the thermal electromotive force of the thermocouple exhibits a linear relationship with temperature and is not associated with pressure. The resistivity measurement of ZnS powders under high pressure at different temperatures shows that the phase transition pressure decreases as the temperature increases.

  11. Preparation of W-Ta thin-film thermocouple on diamond anvil cell for in-situ temperature measurement under high pressure.

    PubMed

    Yang, Jie; Li, Ming; Zhang, Honglin; Gao, Chunxiao

    2011-04-01

    In this paper, a W-Ta thin-film thermocouple has been integrated on a diamond anvil cell by thin-film deposition and photolithography methods. The thermocouple was calibrated and its thermal electromotive force was studied under high pressure. The results indicate that the thermal electromotive force of the thermocouple exhibits a linear relationship with temperature and is not associated with pressure. The resistivity measurement of ZnS powders under high pressure at different temperatures shows that the phase transition pressure decreases as the temperature increases.

  12. New Experimental Method for In Situ Determination of Material Textures at Simultaneous High-Pressure and -Temperature by Means of Radial Diffraction in the Diamond Anvil Cell.

    SciTech Connect

    Liermann, H; Merkel, S; Miyagi, L; Wenk, H; Shen, G; Cynn, H; Evans, W J

    2009-07-15

    We introduce the design and capabilities of a new resistive heated diamond anvil cell that can be used for side diffraction at simultaneous high-pressure and -temperature. The device can be used to study lattice-preferred orientations in polycrystalline samples up to temperatures of 1100 K and pressures of 36 GPa. Capabilities of the instrument are demonstrated with preliminary results on the development of textures in the BCC, FCC and HCP polymorphs of iron during a non-hydrostatic compression experiment at simultaneous high-pressure and -temperature.

  13. Preparation of W-Ta thin-film thermocouple on diamond anvil cell for in-situ temperature measurement under high pressure

    NASA Astrophysics Data System (ADS)

    Yang, Jie; Li, Ming; Zhang, Honglin; Gao, Chunxiao

    2011-04-01

    In this paper, a W-Ta thin-film thermocouple has been integrated on a diamond anvil cell by thin-film deposition and photolithography methods. The thermocouple was calibrated and its thermal electromotive force was studied under high pressure. The results indicate that the thermal electromotive force of the thermocouple exhibits a linear relationship with temperature and is not associated with pressure. The resistivity measurement of ZnS powders under high pressure at different temperatures shows that the phase transition pressure decreases as the temperature increases.

  14. Cross-check of ex-situ and in-situ metrology of a bendable temperature stabilized KB mirror

    SciTech Connect

    Yuan, Sheng Sam; Goldberg, Kenneth A.; Yashchuk, Valeriy V.; Celestre, Richard; McKinney, Wayne R.; Morrison, Gregory; Macdougall, James; Mochi, Iacopo; Warwick, Tony

    2010-09-15

    At the Advanced Light Source (ALS), we are developing broadly applicable, high-accuracy, in-situ, at-wavelength wavefront slope measurement techniques for Kirkpatrick-Baez (KB) mirror nano-focusing. In this paper, we report an initial cross-check of ex-situ and in-situ metrology of a bendable temperature stabilized KB mirror. This cross-check provides a validation of the in-situ shearing interferometry currently under development at the ALS.

  15. A novel high-temperature furnace for combined in situ synchrotron X-ray diffraction and infrared thermal imaging to investigate the effects of thermal gradients upon the structure of ceramic materials.

    PubMed

    Robinson, James B; Brown, Leon D; Jervis, Rhodri; Taiwo, Oluwadamilola O; Millichamp, Jason; Mason, Thomas J; Neville, Tobias P; Eastwood, David S; Reinhard, Christina; Lee, Peter D; Brett, Daniel J L; Shearing, Paul R

    2014-09-01

    A new technique combining in situ X-ray diffraction using synchrotron radiation and infrared thermal imaging is reported. The technique enables the application, generation and measurement of significant thermal gradients, and furthermore allows the direct spatial correlation of thermal and crystallographic measurements. The design and implementation of a novel furnace enabling the simultaneous thermal and X-ray measurements is described. The technique is expected to have wide applicability in material science and engineering; here it has been applied to the study of solid oxide fuel cells at high temperature.

  16. In Situ Analysis of a High-Temperature Cure Reaction in Real Time Using Modulated Fiber-Optic FT-Raman Spectroscopy

    NASA Technical Reports Server (NTRS)

    Aust, Jeffrey F.; Cooper, John B.; Wise, Kent L.; Jensen, Brian J.

    1999-01-01

    The vibrational spectrum of a high-temperature (330 C) polymerization reaction was successfully monitored in real time with the use of a modulated fiber-optic Fourier transform (FT)-Raman spectrometer. A phenylethynyl-terminated monomer was cured, and spectral evidence for two different reaction products was acquired. The products are a conjugated polyene chain and a cyclized trimer. This is the first report describing the use of FT-Raman spectroscopy to monitor a high temperature (greater than 250 C) reaction in real time.

  17. In Situ Analysis of a High-Temperature Cure Reaction in Real Time Using Modulated Fiber-Optic FT-Raman Spectroscopy

    NASA Technical Reports Server (NTRS)

    Aust, Jeffrey F.; Cooper, John B.; Wise, Kent L.; Jensen, Brian J.

    1999-01-01

    The vibrational spectrum of a high-temperature (330 C) polymerization reaction was successfully monitored in real time with the use of a modulated fiber-optic Fourier transform (FT)-Raman spectrometer. A phenylethynyl-terminated monomer was cured, and spectral evidence for two different reaction products was acquired. The products are a conjugated polyene chain and a cyclized trimer. This is the first report describing the use of FT-Raman spectroscopy to monitor a high temperature (greater than 250 C) reaction in real time.

  18. High accuracy in situ radiometric mapping.

    PubMed

    Tyler, Andrew N

    2004-01-01

    In situ and airborne gamma ray spectrometry have been shown to provide rapid and spatially representative estimates of environmental radioactivity across a range of landscapes. However, one of the principal limitations of this technique has been the influence of changes in the vertical distribution of the source (e.g. 137Cs) on the observed photon fluence resulting in a significant reduction in the accuracy of the in situ activity measurement. A flexible approach for single gamma photon emitting radionuclides is presented, which relies on the quantification of forward scattering (or valley region between the full energy peak and Compton edge) within the gamma ray spectrum to compensate for changes in the 137Cs vertical activity distribution. This novel in situ method lends itself to the mapping of activity concentrations in environments that exhibit systematic changes in the vertical activity distribution. The robustness of this approach has been demonstrated in a salt marsh environment on the Solway coast, SW Scotland, with both a 7.6 cm x 7.6 cm NaI(Tl) detector and a 35% n-type HPGe detector. Application to ploughed field environments has also been demonstrated using HPGe detector, including its application to the estimation of field moist bulk density and soil erosion measurement. Ongoing research work is also outlined.

  19. High Temperature Mechanical Behavior of MgAl2O4-YAG Eutectic Ceramic In Situ Composites by Float Zone Method

    NASA Astrophysics Data System (ADS)

    Abalı, Serkan

    2017-09-01

    The directionally solidified eutectic MgAl2O4-Y3Al5O12 crystal was prepared at a pressure of 0.4 MPa of ambient nitrogen gas by the high frequency induction heated floating zone furnace. In order to determine the high temperature characteristics, directionally solidified MgAl2O4-Y3Al5O12 eutectic phase has been analyzed with creep test, tensile strength, young modulus and fracture toughness at the various temperatures and the microstructural variations have been studied according to the analysis results. It has been seen that directionally solidified with zone melting MgAl2O4-YAG eutectic ceramic which has given the value of 168 MPa below 10-6/s strain rate at 1,700 °C temperature has revealed minimum stress.

  20. Combining Remote Temperature Sensing with in-Situ Sensing to Track Marine/Freshwater Mixing Dynamics

    PubMed Central

    McCaul, Margaret; Barland, Jack; Cleary, John; Cahalane, Conor; McCarthy, Tim; Diamond, Dermot

    2016-01-01

    The ability to track the dynamics of processes in natural water bodies on a global scale, and at a resolution that enables highly localised behaviour to be visualized, is an ideal scenario for understanding how local events can influence the global environment. While advances in in-situ chem/bio-sensing continue to be reported, costs and reliability issues still inhibit the implementation of large-scale deployments. In contrast, physical parameters like surface temperature can be tracked on a global scale using satellite remote sensing, and locally at high resolution via flyovers and drones using multi-spectral imaging. In this study, we show how a much more complete picture of submarine and intertidal groundwater discharge patterns in Kinvara Bay, Galway can be achieved using a fusion of data collected from the Earth Observation satellite (Landsat 8), small aircraft and in-situ sensors. Over the course of the four-day field campaign, over 65,000 in-situ temperatures, salinity and nutrient measurements were collected in parallel with high-resolution thermal imaging from aircraft flyovers. The processed in-situ data show highly correlated patterns between temperature and salinity at the southern end of the bay where freshwater springs can be identified at low tide. Salinity values range from 1 to 2 ppt at the southern end of the bay to 30 ppt at the mouth of the bay, indicating the presence of a freshwater wedge. The data clearly show that temperature differences can be used to track the dynamics of freshwater and seawater mixing in the inner bay region. This outcome suggests that combining the tremendous spatial density and wide geographical reach of remote temperature sensing (using drones, flyovers and satellites) with ground-truthing via appropriately located in-situ sensors (temperature, salinity, chemical, and biological) can produce a much more complete and accurate picture of the water dynamics than each modality used in isolation. PMID:27589770

  1. Combining Remote Temperature Sensing with in-Situ Sensing to Track Marine/Freshwater Mixing Dynamics.

    PubMed

    McCaul, Margaret; Barland, Jack; Cleary, John; Cahalane, Conor; McCarthy, Tim; Diamond, Dermot

    2016-08-31

    The ability to track the dynamics of processes in natural water bodies on a global scale, and at a resolution that enables highly localised behaviour to be visualized, is an ideal scenario for understanding how local events can influence the global environment. While advances in in-situ chem/bio-sensing continue to be reported, costs and reliability issues still inhibit the implementation of large-scale deployments. In contrast, physical parameters like surface temperature can be tracked on a global scale using satellite remote sensing, and locally at high resolution via flyovers and drones using multi-spectral imaging. In this study, we show how a much more complete picture of submarine and intertidal groundwater discharge patterns in Kinvara Bay, Galway can be achieved using a fusion of data collected from the Earth Observation satellite (Landsat 8), small aircraft and in-situ sensors. Over the course of the four-day field campaign, over 65,000 in-situ temperatures, salinity and nutrient measurements were collected in parallel with high-resolution thermal imaging from aircraft flyovers. The processed in-situ data show highly correlated patterns between temperature and salinity at the southern end of the bay where freshwater springs can be identified at low tide. Salinity values range from 1 to 2 ppt at the southern end of the bay to 30 ppt at the mouth of the bay, indicating the presence of a freshwater wedge. The data clearly show that temperature differences can be used to track the dynamics of freshwater and seawater mixing in the inner bay region. This outcome suggests that combining the tremendous spatial density and wide geographical reach of remote temperature sensing (using drones, flyovers and satellites) with ground-truthing via appropriately located in-situ sensors (temperature, salinity, chemical, and biological) can produce a much more complete and accurate picture of the water dynamics than each modality used in isolation.

  2. In-situ changes in the elastic wave velocity of rock with increasing temperature using high-resolution coda wave interferometry

    NASA Astrophysics Data System (ADS)

    Griffiths, Luke; Heap, Michael; Lengliné, Olivier; Schmittbuhl, Jean; Baud, Patrick

    2017-04-01

    Rock undergoes fluctuations in temperature in various settings in Earth's crust, including areas of volcanic or geothermal activity, or industrial environments such as hydrocarbon or geothermal reservoirs. Changes in temperature can cause thermal stresses that can result in the formation of microcracks, which affect the mechanical, physical, and transport properties of rocks. Of the affected physical properties, the elastic wave velocity of rock is particularly sensitive to microcracking. Monitoring the evolution of elastic wave velocity during the thermal stressing of rock therefore provides valuable insight into thermal cracking processes. One monitoring technique is Coda Wave Interferometry (CWI), which infers high-resolution changes in the medium from changes in multiple-scattered elastic waves. We have designed a new experimental setup to perform CWI whilst cyclically heating and cooling samples of granite (cylinders of 20 mm diameter and 40 mm length). In our setup, the samples are held between two pistons within a tube furnace and are heated and cooled at a rate of 1 °C/min to temperatures of up to 300 °C. Two high temperature piezo-transducers are each in contact with an opposing face of the rock sample. The servo-controlled uniaxial press compensates for the thermal expansion and contraction of the pistons and the sample, keeping the coupling between the transducers and the sample, and the axial force acting on the sample, constant throughout. Our setup is designed for simultaneous acoustic emission monitoring (AE is commonly used as a proxy for microcracking), and so we can follow thermal microcracking precisely by combining the AE and CWI techniques. We find that during the first heating/cooling cycle, the onset of thermal microcracking occurs at a relatively low temperature of around 65 °C. The CWI shows that elastic wave velocity decreases with increasing temperature and increases during cooling. Upon cooling, back to room temperature, there is an

  3. Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature

    SciTech Connect

    Miyagi, Lowell; Kanitpanyacharoen, Waruntorn; Kaercher, Pamela; Wenk, Hans-Rudolf; Alarcon, Eloisa Zepeda; Raju, Selva Vennila; Knight, Jason; MacDowell, Alastair; Williams, Quentin

    2013-02-15

    To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate and optimize conditions for combined resistive and laser heating. For example, in Run1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg{sub 0.9}Fe{sub 0.1})O in Run3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.

  4. Combined resistive and laser heating technique for in situ radial X-ray diffraction in the diamond anvil cell at high pressure and temperature.

    PubMed

    Miyagi, Lowell; Kanitpanyacharoen, Waruntorn; Raju, Selva Vennila; Kaercher, Pamela; Knight, Jason; MacDowell, Alastair; Wenk, Hans-Rudolf; Williams, Quentin; Alarcon, Eloisa Zepeda

    2013-02-01

    To extend the range of high-temperature, high-pressure studies within the diamond anvil cell, a Liermann-type diamond anvil cell with radial diffraction geometry (rDAC) was redesigned and developed for synchrotron X-ray diffraction experiments at beamline 12.2.2 of the Advanced Light Source. The rDAC, equipped with graphite heating arrays, allows simultaneous resistive and laser heating while the material is subjected to high pressure. The goals are both to extend the temperature range of external (resistive) heating and to produce environments with lower temperature gradients in a simultaneously resistive- and laser-heated rDAC. Three different geomaterials were used as pilot samples to calibrate and optimize conditions for combined resistive and laser heating. For example, in Run#1, FeO was loaded in a boron-mica gasket and compressed to 11 GPa then gradually resistively heated to 1007 K (1073 K at the diamond side). The laser heating was further applied to FeO to raise temperature to 2273 K. In Run#2, Fe-Ni alloy was compressed to 18 GPa and resistively heated to 1785 K (1973 K at the diamond side). The combined resistive and laser heating was successfully performed again on (Mg0.9Fe0.1)O in Run#3. In this instance, the sample was loaded in a boron-kapton gasket, compressed to 29 GPa, resistive-heated up to 1007 K (1073 K at the diamond side), and further simultaneously laser-heated to achieve a temperature in excess of 2273 K at the sample position. Diffraction patterns obtained from the experiments were deconvoluted using the Rietveld method and quantified for lattice preferred orientation of each material under extreme conditions and during phase transformation.

  5. Determination of the effect of different additives in coking blends using a combination of in situ high-temperature {sup 1}H NMR and rheometry

    SciTech Connect

    Miguel C. Diaz; Karen M. Steel; Trevor C. Drage; John W. Patrick; Colin E. Snape

    2005-12-01

    High-temperature {sup 1}H NMR and rheometry measurements were carried out on 4:1 wt/wt blends of a medium volatile bituminous coal with two anthracites, two petroleum cokes, charcoal, wood, a low-temperature coke breeze, tyre crumb, and active carbon to determine the effects on fluidity development to identify the parameters responsible for these effects during pyrolysis and to study possible relationships among the parameters derived from these techniques. Positive, negative, and neutral effects were identified on the concentration of fluid material. Small positive effects (ca. 5-6%) were caused by blending the coal with petroleum cokes. Charcoal, wood, and active carbon all exerted negative effects on concentration (18-27% reduction) and mobility (12-25% reduction in T2) of the fluid phase, which have been associated with the inert character and high surface areas of these additives that adsorb the fluid phase of the coal. One of the anthracites and the low-temperature coke breeze caused deleterious effects to a lesser extent on the concentration (7-12%) and mobility (13-17%) of the fluid material, possibly due to the high concentration of metals in these additives (ca. 11% ash). Despite the high fluid character of tyre crumb at the temperature of maximum fluidity of the coal (73%), the mobility of the fluid phase of the blend was lower than expected. The comparison of {sup 1}H NMR and rheometry results indicated that to account for the variations in minimum complex viscosity for all the blends, both the maximum concentration of fluid phase and the maximum mobility of the fluid material had to be considered. For individual blends, two exponential relationships have been found between the complex viscosity and the concentration of solid phase in both the softening and resolidification stages but the parameters are different for each blend. 30 refs., 8 figs., 5 tabs.

  6. Low Temperature Regolith Bricks for In-Situ Structural Material

    NASA Technical Reports Server (NTRS)

    Grossman, Kevin; Sakthivel, Tamil S.; Mantovani, James; Seal, Sudipta

    2016-01-01

    Current technology for producing in-situ structural materials on future missions to Mars or the moon relies heavily on energy-intensive sintering processes to produce solid bricks from regolith. This process requires heating the material up to temperatures in excess of 1000 C and results in solid regolith pieces with compressive strengths in the range of 14000 to 28000 psi, but are heavily dependent on the porosity of the final material and are brittle. This method is currently preferred over a low temperature cementation process to prevent consumption of precious water and other non-renewable materials. A high strength structural material with low energy requirements is still needed for future colonization of other planets. To fulfill these requirements, a nano-functionalization process has been developed to produce structural bricks from regolith simulant and shows promising mechanical strength results. Functionalization of granular silicate particles into alkoxides using a simple low temperature chemical process produces a high surface area zeolite particles that are held together via inter-particle oxygen bonding. Addition of water in the resulting zeolite particles produces a sol-gel reaction called "inorganic polymerization" which gives a strong solid material after a curing process at 60 C. The aqueous solution by-product of the reaction is currently being investigated for its reusability; an essential component of any ISRU technology. For this study, two batches of regolith bricks are synthesized from JSC-1A; the first batch from fresh solvents and chemicals, the second batch made from the water solution by-product of the first batch. This is done to determine the feasibility of recycling necessary components of the synthesis process, mainly water. Characterization including BET surface area, SEM, and EDS has been done on the regolith bricks as well as the constituent particles,. The specific surface area of 17.53 sq m/g (average) of the granular regolith

  7. Isentropic advection and convective lifting of water vapor in the UT - LS as observed over Brazil (22° S) in February 2004 by in situ high-resolution measurements of H2O, CH4, O3 and temperature

    NASA Astrophysics Data System (ADS)

    Durry, G.; Huret, N.; Hauchecorne, A.; Marecal, V.; Pommereau, J.-P.; Jones, R. L.; Held, G.; Larsen, N.; Renard, J.-B.

    2006-12-01

    The micro-SDLA balloonborne diode laser spectrometer was flown twice from Bauru (22° S, Brazil) in February 2004 during HIBISCUS to yield in situ H2O measurements in the Upper Troposphere (UT) and Lower Stratosphere (LS) and in particular in the Tropical Tropopause Layer (TTL). The overall TTL was found warmer (with a subsaturated cold point near -79°C) and the LS moister compared to former measurements obtained in tropical oceanic conditions. The use of specific balloons with a slow descent, combined with the high-resolution of the laser sensor, allowed us to observe in situ in the UT, the TTL and the LS several thin layers correlated on H2O, CH4, O3, temperature and PV. A component of these layers is associated with the isentropic transport into the UT- LS of extratropical stratospheric air masses. Moreover, the examination of temperature and tracer (CH4, O3) profiles gives insights on the potential contribution of convective transport of H2O in the TTL.

  8. High resolution in situ ultrasonic corrosion monitor

    DOEpatents

    Grossman, R.J.

    1984-01-10

    An ultrasonic corrosion monitor is provided which produces an in situ measurement of the amount of corrosion of a monitoring zone or zones of an elongate probe placed in the corrosive environment. A monitoring zone is preferably formed between the end of the probe and the junction of the zone with a lead-in portion of the probe. Ultrasonic pulses are applied to the probe and a determination made of the time interval between pulses reflected from the end of the probe and the junction referred to, both when the probe is uncorroded and while it is corroding. Corresponding electrical signals are produced and a value for the normalized transit time delay derived from these time interval measurements is used to calculate the amount of corrosion.

  9. High resolution in situ ultrasonic corrosion monitor

    DOEpatents

    Grossman, Robert J.

    1985-01-01

    An ultrasonic corrosion monitor is provided which produces an in situ measurement of the amount of corrosion of a monitoring zone or zones of an elongate probe placed in the corrosive environment. A monitoring zone is preferably formed between the end of the probe and the junction of the zone with a lead-in portion of the probe. Ultrasonic pulses are applied to the probe and a determination made of the time interval between pulses reflected from the end of the probe and the junction referred to, both when the probe is uncorroded and while it is corroding. Corresponding electrical signals are produced and a value for the normalized transit time delay derived from these time interval measurements is used to calculate the amount of corrosion.

  10. Experimental issues in in-situ synchrotron x-ray diffraction at high pressure and temperature by using a laser-heated diamond-anvil cell

    SciTech Connect

    Yoo, C.S.

    1997-12-01

    An integrated technique of diamond-anvil cell, laser-heating and synchrotron x-ray diffraction technologies is capable of structural investigation of condensed matter in an extended region of high pressures and temperatures above 100 GPa and 3000 K. The feasibility of this technique to obtain reliable data, however, strongly depends on several experimental issues, including optical and x-ray setups, thermal gradients, pressure homogeneity, preferred orientation, and chemical reaction. In this paper, we discuss about these experimental issues together with future perspectives of this technique for obtaining accurate data.

  11. In situ Phase Transition Study of Nano- and Coarse-Grained TiO2 Under High Pressure/Temperature Conditions

    SciTech Connect

    Wang,Y.; Zhao, Y.; Zhang, J.; Xu, h.; Wang, L.; Luo, S.; Daemen, L.

    2008-01-01

    A comparative phase transition study of nanocrystalline and micro-TiO2 has been conducted under high pressure-temperature (P-T) conditions using energy-dispersive synchrotron x-ray diffraction (XRD). Our study reveals that on compression at room temperature, the micro-tetragonal anatase-type TiO2 started to transform to the orthorhombic columbite-type TiO2 near 1.6 GPa. In contrast, we did not observe this phase transition in nano-anatase at pressures of up to 8.5 GPa. At 8.5 GPa, by applying moderate heat, both samples were transformed completely to columbite-type TiO2 almost simultaneously, indicating that heat treatment could significantly expedite this phase transition. These columbite-type TiO2 phases were quenchable because after cooling them to room temperature and decompressing them to 2.0 GPa, the XRD patterns displayed no changes in comparison with those collected at 8.6 GPa and 1270 K. At 2 GPa, we heated the specimens again, and the rutile-type TiO2 started to emerge around 970 K. This phase was also quenchable after cooling and releasing pressure to ambient conditions. The grain size effects on the phase transition were discussed based on the kinetics mechanism. This study should be of considerable interest to the fields of materials science and condensed matter.

  12. In situ TEM observation of FCC Ti formation at elevated temperatures

    DOE PAGES

    Yu, Qian; Kacher, Josh; Gammer, Christoph; ...

    2017-07-04

    Pure Ti traditionally exhibits the hexagonal closed packed (HCP) crystallographic structure under ambient conditions and the body centered cubic (BCC) structure at elevated temperatures. In addition to these typical structures for Ti alloys, the presence of a face centered cubic (FCC) phase associated with thin films, interfaces, or high levels of plastic deformation has occasionally been reported. Here in this paper we show that small FCC precipitates form in freestanding thin foils during in situ transmission electron microscope (TEM) heating and we discuss the potential origins of the FCC phase in light of the in situ observations. This FCC phasemore » was found to be stable upon cooling and under ambient conditions, which allowed us to explore its mechanical properties and stability via nanomechanical in situ TEM testing. It was found that FCC platelets within the HCP matrix phase were stable under mechanical deformation and exhibited similar mechanical deformation behavior as the parent HCP phase.« less

  13. Correlation between structure and fluidity of coal tar pitch fractions studied by ambient {sup 13}C and high temperature in-situ {sup 1}H nuclear magnetic resonance

    SciTech Connect

    Andresen, J.M.; Schober, H.H.; Rusinko, F.J. Jr.

    1999-07-01

    The unique properties of coal tar pitches have resulted in numerous applications for carbon products, such as binders for carbon artifacts. However, as the number of by-product coke ovens is diminishing, the design of superior binders from alternative materials or processes is sought by the carbon industry. Accordingly, structural characterization of coal tar pitches and their solvent fractions, using quantitative analytical techniques is required to successfully obtain this goal. Quantitative solid state {sup 13}C NMR has previously been shown to be a powerful technique to study the overall aromatic ring-size for coal tar pitches and their toluene insoluble (TI) fractions. The TI fraction can further be separated into its quinoline soluble part (beta-resin) and insoluble fraction (QI). Both these fractions affect the overall coking yield and especially the fluidity of the pitches. The assessment of fluidity interactions between coal tar pitch solvent fractions during heating is therefore important for the future design of pitches from untraditional sources or processes. High temperature {sup 1}H NMR is a useful technique to investigate the fluid and rigid components of pitches, especially with its interaction with coal and to quantify mesophase. However, very little work has been performed to correlate the overall fluidity behavior of pitch with the mobility of its different solubility fractions and their structure. Accordingly, this paper addresses the fluidity interactions between different pitch solvent fractions (TS, beta-resin and QI) by high temperature {sup 1}H NMR. Particularly, the fluidity studies on the beta-resin alone can verify whether this fraction becomes plastic during heating.

  14. The influence of methanol on the chemical state of PtRu anodes in a high-temperature direct methanol fuel cell studied in situ by synchrotron-based near-ambient pressure x-ray photoelectron spectroscopy

    NASA Astrophysics Data System (ADS)

    Saveleva, Viktoriia A.; Daletou, Maria K.; Savinova, Elena R.

    2017-01-01

    Synchrotron radiation-based near-ambient pressure x-ray photoelectron spectroscopy (NAP-XPS) has recently become a powerful tool for the investigation of interfacial phenomena in electrochemical power sources such as batteries and fuel cells. Here we present an in situ NAP-XPS study of the anode of a high-temperature direct methanol fuel cell with a phosphoric acid-doped hydrocarbon membrane, which reveals an enhanced flooding of the Pt3Ru anode with phosphoric acid in the presence of methanol. An analysis of the electrode surface composition depending on the cell voltage and on the presence of methanol reveals the strong influence of the latter on the extent of Pt oxidation and on the transformation of Ru into Ru (IV) hydroxide.

  15. In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells

    NASA Astrophysics Data System (ADS)

    Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

    2015-11-01

    A core-shell anode consisting of nickel-gadolinium-doped-ceria (Ni-GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets. The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres. Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode. The maximum power density of the attractive anode was 97 mW cm-2, which is higher than that of a conventional NiO-GDC anode prepared by an aerosol process at 55 mW cm-2 and 600 °C, followed by sintering at 1300 °C. Furthermore, the macro- and microstructure of the Ni-GDC-nanocube anode were preserved before and after the power-generation test at 700 °C. Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully.

  16. In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells.

    PubMed

    Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

    2015-11-30

    A core-shell anode consisting of nickel-gadolinium-doped-ceria (Ni-GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets. The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres. Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode. The maximum power density of the attractive anode was 97 mW cm(-2), which is higher than that of a conventional NiO-GDC anode prepared by an aerosol process at 55 mW cm(-2) and 600 °C, followed by sintering at 1300 °C. Furthermore, the macro- and microstructure of the Ni-GDC-nanocube anode were preserved before and after the power-generation test at 700 °C. Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully.

  17. In situ fabrication of high-performance Ni-GDC-nanocube core-shell anode for low-temperature solid-oxide fuel cells

    PubMed Central

    Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

    2015-01-01

    A core–shell anode consisting of nickel–gadolinium-doped-ceria (Ni–GDC) nanocubes was directly fabricated by a chemical process in a solution containing a nickel source and GDC nanocubes covered with highly reactive {001} facets. The cermet anode effectively generated a Ni metal framework even at 500 °C with the growth of the Ni spheres. Anode fabrication at such a low temperature without any sintering could insert a finely nanostructured layer close to the interface between the electrolyte and the anode. The maximum power density of the attractive anode was 97 mW cm–2, which is higher than that of a conventional NiO–GDC anode prepared by an aerosol process at 55 mW cm–2 and 600 °C, followed by sintering at 1300 °C. Furthermore, the macro- and microstructure of the Ni–GDC-nanocube anode were preserved before and after the power-generation test at 700 °C. Especially, the reactive {001} facets were stabled even after generation test, which served to reduce the activation energy for fuel oxidation successfully. PMID:26615816

  18. Multifunctional Nanowire/film Composites based Bi-modular Sensors for In-situ and Real-time High Temperature Gas Detection

    SciTech Connect

    Gao, Pu-Xian; Lei, Yu

    2013-06-01

    This final report to the Department of Energy/National Energy Technology Laboratory for DE-FE0000870 covers the period from 2009 to June, 2013 and summarizes the main research accomplishments, which can be divided in sensing materials innovation, bimodular sensor demonstration, and new understanding and discoveries. As a matter of fact, we have successfully completed all the project tasks in June 1, 2013, and presented the final project review presentation on the 9th of July, 2013. Specifically, the major accomplishments achieved in this project include: 1) Successful development of a new class of high temperature stable gas sensor nanomaterials based on composite nano-array strategy in a 3D or 2D fashion using metal oxides and perovskite nanostructures. 2) Successful demonstration of bimodular nanosensors using 2D nanofibrous film and 3D composite nanowire arrays using electrical resistance mode and electrochemical electromotive force mode. 3) Series of new discoveries and understandings based on the new composite nanostructure platform toward enhancing nanosensor performance in terms of stability, selectivity, sensitivity and mass flux sensing. In this report, we highlight some results toward these accomplishments.

  19. Wireless device for monitoring the temperature - moisture regime in situ

    NASA Astrophysics Data System (ADS)

    Hudec, Ján; Štofanik, Vladimír; Vretenár, Viliam; Kubičár, Ľudovít

    2014-05-01

    This contribution presents the wireless device for monitoring the temperature - moisture regime in situ. For the monitoring so called moisture sensor is used. Principle of moisture sensor is based on measuring the thermal conductivity. Moisture sensor has cylindrical shape with about 20 mm diameter and 20 mm length. It is made of porous material identical to the monitored object. The thermal conductivity is measured by hot-ball method. Hot-ball method is patented invention of the Institute of Physic SAS. It utilizes a small ball, diameter up to 2 mm, in which sensing elements are incorporated. The ball produces heat spreading into surrounding material, in our case into body of the moisture sensor. Temperature of the ball is measured simultaneously. Then change of the temperature, in steady state, is inversely proportional to the thermal conductivity. Such moisture sensor is inserted into monitored wall. Thermophysical properties of porous material are function of moisture. Moisture sensors are calibrated for dry and water saturated state. Whole the system is primarily intended to do long-term monitoring. Design of a new electronic device was needed for this innovative method. It covers all needed operations for measurement. For example energizing hot-ball sensor, measuring its response, storing the measured data and wireless data transmission. The unit is able to set parameters of measurement via wireless access as well. This contribution also includes the description of construction and another features of the wireless measurement system dedicated for this task. Possibilities and functionality of the system is demonstrated by actual monitoring of the tower of St. Martin's Cathedral in Bratislava. Correlations with surrounding meteorological conditions are presented. Some of them can be also measured by our system, right in the monitoring place.

  20. In Situ Monitoring of Temperature inside Lithium-Ion Batteries by Flexible Micro Temperature Sensors

    PubMed Central

    Lee, Chi-Yuan; Lee, Shuo-Jen; Tang, Ming-Shao; Chen, Pei-Chi

    2011-01-01

    Lithium-ion secondary batteries are commonly used in electric vehicles, smart phones, personal digital assistants (PDA), notebooks and electric cars. These lithium-ion secondary batteries must charge and discharge rapidly, causing the interior temperature to rise quickly, raising a safety issue. Over-charging results in an unstable voltage and current, causing potential safety problems, such as thermal runaways and explosions. Thus, a micro flexible temperature sensor for the in in-situ monitoring of temperature inside a lithium-ion secondary battery must be developed. In this work, flexible micro temperature sensors were integrated into a lithium-ion secondary battery using the micro-electro-mechanical systems (MEMS) process for monitoring temperature in situ. PMID:22163735

  1. In situ monitoring of temperature inside lithium-ion batteries by flexible micro temperature sensors.

    PubMed

    Lee, Chi-Yuan; Lee, Shuo-Jen; Tang, Ming-Shao; Chen, Pei-Chi

    2011-01-01

    Lithium-ion secondary batteries are commonly used in electric vehicles, smart phones, personal digital assistants (PDA), notebooks and electric cars. These lithium-ion secondary batteries must charge and discharge rapidly, causing the interior temperature to rise quickly, raising a safety issue. Over-charging results in an unstable voltage and current, causing potential safety problems, such as thermal runaways and explosions. Thus, a micro flexible temperature sensor for the in in-situ monitoring of temperature inside a lithium-ion secondary battery must be developed. In this work, flexible micro temperature sensors were integrated into a lithium-ion secondary battery using the micro-electro-mechanical systems (MEMS) process for monitoring temperature in situ.

  2. Oil-Well Cement and C3S Hydration Under High Pressure as Seen by In Situ X-Ray Diffraction, Temperatures ;= 80 degrees C with No Additives

    SciTech Connect

    Jupe, Andrew C.; Wilkinson, Angus P.; Funkhouser, Garry P.

    2012-06-28

    The hydration kinetics of a white cement and batches of both Class G and H oil-well cements were examined between 0 and 60 MPa, at {le}80 C, using in situ synchrotron X-ray diffraction. This gives a continuous measure of the C{sub 3}S (Ca{sub 3}SiO{sub 5}), CH (Ca(OH){sub 2}), C{sub 4}AF (Ca{sub 2}FeAlO{sub 5}), ettringite, and other phases in the hydrating slurries. Slurries prepared from single-phase C{sub 3}S; synthetic C{sub 4}AF, and gypsum; and white cement, synthetic C{sub 4}AF and gypsum were also examined. An increasing pressure enhanced the rate of hydration for all slurries. Analysis of the data, using a kinetic model, provided rate constants that were used to obtain activation volumes for C{sub 3}S hydration. For all the cement and C{sub 3}S slurries studied, similar activation volumes were obtained (average {Delta}V{double_dagger}{sup -}-35 cm{sup 3}/mol), indicating that the presence of cement phases other than C{sub 3}S has a modest influence on the pressure dependence of C{sub 3}S hydration. An alternative analysis, using the time at which 90% of the initial C{sub 3}S remained, gave similar activation volumes. Pressure accelerated the formation of ettringite from synthetic C{sub 4}AF in the presence of gypsum. However, in slurries containing cement, the pressure dependence of C{sub 3}S hydration plays a major role in determining the pressure dependence of ettringite formation.

  3. Development of Self-Powered Wireless-Ready High Temperature Electrochemical Sensors for In-Situ Corrosion Monitoring for Boiler Tubes in Next Generation Coal-based Power Systems

    SciTech Connect

    Liu, Xingbo

    2015-06-30

    The key innovation of this project is the synergy of the high temperature sensor technology based on the science of electrochemical measurement and state-of-the-art wireless communication technology. A novel self-powered wireless high temperature electrochemical sensor system has been developed for coal-fired boilers used for power generation. An initial prototype of the in-situ sensor demonstrated the capability of the wireless communication system in the laboratory and in a pilot plant (Industrial USC Boiler Setting) environment to acquire electrochemical potential and current signals during the corrosion process. Uniform and localized under-coal ash deposit corrosion behavior of Inconel 740 superalloy has been studied at different simulated coal ash hot corrosion environments using the developed sensor. Two typical potential noise patterns were found to correlate with the oxidation and sulfidation stages in the hot coal ash corrosion process. Two characteristic current noise patterns indicate the extent of the corrosion. There was a good correlation between the responses of electrochemical test data and the results from corroded surface analysis. Wireless electrochemical potential and current noise signals from a simulated coal ash hot corrosion process were concurrently transmitted and recorded. The results from the performance evaluation of the sensor confirm a high accuracy in the thermodynamic and kinetic response represented by the electrochemical noise and impedance test data.

  4. Simultaneous in-situ measurements of mesospheric temperature inversion layers and turbulence

    NASA Astrophysics Data System (ADS)

    Strelnikov, Boris; Rapp, Markus

    For several decades rocket borne ionization gauges have been used to obtain observations of mesospheric turbulence and temperature-profiles. The main advantage of these in-situ turbu-lence measurements is that they are made at very high spatial resolution and cover a wide range of spatial scales. This makes it possible to study the spectral content of the turbulent eddies in the range of spatial scales from tens of centimeters to some kilometers. Spectral analysis of these data yields turbulent energy dissipation rates at a spatial resolution of about 100 m. This reveals the highly patchy structure of MLT turbulence. Our measurements of-ten show adjacent regions with very strong turbulence and non-turbulent layers on vertical scales as short as some kilometers. Some observations even show turbulence layers which are only some hundreds of meters thick. Most of these turbulence measurements were accompa-nied by simultaneous common volume temperature measurements. Among those simultaneous measurements temperature inversion layers were often observed. In the present paper we analyze simultaneous in-situ measurements of mesospheric temperature inversion layers and turbulence measurements. This study includes about 30 sounding rocket flights launched at high northern latitudes. We compare morphology of the turbulence field with temperature profiles to gain a deeper insight how temperature inversions are related to local turbulence activity.

  5. In situ and glancing angle X-ray diffraction of the structure change during and after the high temperature oxidation at 1000 ^{circ}C in air of an yttrium-implanted 304 steel

    NASA Astrophysics Data System (ADS)

    Riffard, F.; Buscail, H.; Caudron, E.; Cueff, R.; Rabaste, F.; Issartel, C.

    2002-07-01

    A study has been made of the initial stages of oxidation of yttrium ion implanted 304 steel in an attempt to shed some light on the so-called `reactive element effect' observed on chromia forming alloys. In situ XRD was used in order to observe the initial local structural changes during the high temperature oxidation process, while glancing angle XRD was used to monitor the longer range structural transformations taking place near the surface after cooling of oxidised samples. The treatment by ion implantation promotes the intensive establishment of the chromic layer, which leads to the inhibition of the formation of iron rich oxides, by preventing the diffusion of iron through the more compact and more uniform layer initially formed than it would be in the absence of yttrium. However, the identification of yttried phases could not be established. L'effet bénéfique d'un traitement par implantation ionique d'yttrium sur un acier 304 a été mis en évidence par le suivi d'analyses in situ développées par diffraction des rayons X au cours de son oxydation isotherme à 1000^{circ}C sous air. Malgré l'altération superficielle du substrat, le traitement par implantation ionique favorise l'établissement accéléré de la couche de chromine et inhibe la formation au cours du processus d'oxydation des oxydes contenant du fer, réputés peu protecteurs, car faiblement adhérents. Des analyses conduites après refroidissement des échantillons oxydés par diffraction des rayons X sous incidence rasante révèlent la localisation de la structure spinelle au manganèse à l'interface le plus externe. L'identification de phases yttriées n'a cependant pu être établie.

  6. [In situ temperature measurement by absorption spectroscopy based on time division multiplexing technology].

    PubMed

    Lou, Nan-zheng; Li, Ning; Weng, Chun-sheng

    2012-05-01

    Tunable diode laser absorption spectroscopy (TDLAS) technology is a kind of high sensitivity, high selectivity of non contacting gas in situ measurement technique. In the present paper, in situ gas temperature measurement of an open environment was achieved by means of direct scanning multiple characteristic lines of H2O and combined with least-squares algorithm. Through the use of HITRAN spectral database, the boundary effect on the gas temperature and concentration measurements was discussed in detail, and results showed that the combination of scanning multiple characteristic lines and least-squares algorithm can effectively reduce the boundary effect on the gas temperature measurements under the open environment. Experiments using time division multiplexing technology to simultaneously scan 7444.36, 7185.60, 7182.95 and 7447.48 cm(-1), the four characteristic H2O lines, the gas temperature of tubular furnace in the range of 573-973 K was measured under different conditions. The maximum temperature difference between absorption spectrum measurement and thermocouple signal was less than 52.4 K, and the maximum relative error of temperature measurement was 6.8%.

  7. In-situ Observation and Differential Thermal Analysis of MnBi in High Magnetic Fields

    NASA Astrophysics Data System (ADS)

    Miyazaki, Daiki; Mitsui, Yoshifuru; Abematsu, Ken-ichi; Takahashi, Kohki; Watanabe, Kazuo; Uda, Satoshi; Koyama, Keiichi

    For investigating in-field process of melting and solidification visually and quantitatively, in-situ observation system with differential thermal analysis (DTA) utilized in high temperature and in high magnetic field was developed. Decomposition processes of the bulk sample of ferromagnetic MnBi were directly observed with collecting DTA data under high magnetic field of 10 T for the 290-770 K temperature range. When the temperature was over decomposition point (ferromagnetic MnBi → paramagnetic Mn1.08Bi + liquid), liquid phase appeared on the sample surface. Furthermore, when the temperature was over peritectic temperature (∼ 700 K: paramagnetic Mn1.08Bi → Mn + liquid), the sample surface was broken and a large quantity of the liquid phase appeared from the sample. The in-situ observation also suggested that the decomposition temperature increased from 620 K for a zero field to 638 K for a magnetic field of 10 T.

  8. In situ high-frequency observations of mycorrhizas.

    PubMed

    Allen, Michael F; Kitajima, Kuni

    2013-10-01

    Understanding the temporal variation of soil and root dynamics is a major step towards determining net carbon in ecosystems. We describe the installation and structure of an in situ soil observatory and sensing network consisting of an automated minirhizotron with associated soil and atmospheric sensors. Ectomycorrhizal hyphae were digitized daily during 2011 in a Mediterranean climate, high-elevation coniferous forest. Hyphal length was high, but stable during winter in moist and cold soil. As soil began to warm and dry, simultaneous mortality and production indicating turnover followed precipitation events. Mortality continued through the dry season, although some hyphae persisted through the extremes. With autumn monsoons, rapid hyphal re-growth occurred following each event. Relative hyphal length is dependent upon soil temperature and moisture. Soil respiration is related to the daily change in hyphal production, but not hyphal mortality. Continuous sensor and observation systems can provide more accurate assessments of soil carbon dynamics. © 2013 The Authors. New Phytologist © 2013 New Phytologist Trust.

  9. In situ visualisation of electromigration in Pt nanobridges at elevated temperatures.

    PubMed

    Kozlova, Tatiana; Zandbergen, Henny W

    2015-11-01

    We used a combination of in situ TEM, a MEMS-based heater as a substrate and a dedicated biasing sample holder to study the temperature dependence of electromigration in Pt nanobridges (500 nm wide, 15 nm high and 1000 nm long). We visualised changes in the nanobridges under both dynamic conditions, i.e. heating (substrate temperatures up to 660 K) and current passage. Our electromigration experiments at various substrate temperatures (100, 300, 420 and 660 K) show the same tendency: material transport occurs from the cathode to the anode side, which can be explained by the electron-wind force. In all cases the bridge breaks due to the formation of a neck closer to the cathode side. At 300, 420 and 660 K, voids and the neck form at the cathode contact pad simultaneously. The higher the temperature, the bigger the voids size. As expected, at higher temperatures a lower power is needed to break the nanobridge.

  10. In situ strain and temperature measurement and modelling during arc welding

    SciTech Connect

    Chen, Jian; Yu, Xinghua; Miller, Roger G.; Feng, Zhili

    2014-12-26

    In this study, experiments and numerical models were applied to investigate the thermal and mechanical behaviours of materials adjacent to the weld pool during arc welding. In the experiment, a new high temperature strain measurement technique based on digital image correlation (DIC) was developed and applied to measure the in situ strain evolution. In contrast to the conventional DIC method that is vulnerable to the high temperature and intense arc light involved in fusion welding processes, the new technique utilised a special surface preparation method to produce high temperature sustaining speckle patterns required by the DIC algorithm as well as a unique optical illumination and filtering system to suppress the influence of the intense arc light. These efforts made it possible for the first time to measure in situ the strain field 1 mm away from the fusion line. The temperature evolution in the weld and the adjacent regions was simultaneously monitored by an infrared camera. Finally and additionally, a thermal–mechanical finite element model was applied to substantiate the experimental measurement.

  11. In situ strain and temperature measurement and modelling during arc welding

    DOE PAGES

    Chen, Jian; Yu, Xinghua; Miller, Roger G.; ...

    2014-12-26

    In this study, experiments and numerical models were applied to investigate the thermal and mechanical behaviours of materials adjacent to the weld pool during arc welding. In the experiment, a new high temperature strain measurement technique based on digital image correlation (DIC) was developed and applied to measure the in situ strain evolution. In contrast to the conventional DIC method that is vulnerable to the high temperature and intense arc light involved in fusion welding processes, the new technique utilised a special surface preparation method to produce high temperature sustaining speckle patterns required by the DIC algorithm as well asmore » a unique optical illumination and filtering system to suppress the influence of the intense arc light. These efforts made it possible for the first time to measure in situ the strain field 1 mm away from the fusion line. The temperature evolution in the weld and the adjacent regions was simultaneously monitored by an infrared camera. Finally and additionally, a thermal–mechanical finite element model was applied to substantiate the experimental measurement.« less

  12. Manipulation of Samples at Extreme Temperatures for Fast in-situ Synchrotron Measurements

    SciTech Connect

    Weber, Richard

    2016-04-22

    An aerodynamic sample levitation system with laser beam heating was integrated with the APS beamlines 6 ID-D, 11 ID-C and 20 BM-B. The new capability enables in-situ measurements of structure and XANES at extreme temperatures (300-3500 °C) and in conditions that completely avoid contact with container surfaces. In addition to maintaining a high degree of sample purity, the use of aerodynamic levitation enables deep supercooling and greatly enhanced glass formation from a wide variety of melts and liquids. Development and integration of controlled extreme sample environments and new measurement techniques is an important aspect of beamline operations and user support. Processing and solidifying liquids is a critical value-adding step in manufacturing semiconductors, optical materials, metals and in the operation of many energy conversion devices. Understanding structural evolution is of fundamental importance in condensed materials, geology, and biology. The new capability provides unique possibilities for materials research and helps to develop and maintain a competitive materials manufacturing and energy utilization industry. Test samples were used to demonstrate key features of the capability including experiments on hot crystalline materials, liquids at temperatures from about 500 to 3500 °C. The use of controlled atmospheres using redox gas mixtures enabled in-situ changes in the oxidation states of cations in melts. Significant innovations in this work were: (i) Use of redox gas mixtures to adjust the oxidation state of cations in-situ (ii) Operation with a fully enclosed system suitable for work with nuclear fuel materials (iii) Making high quality high energy in-situ x-ray diffraction measurements (iv) Making high quality in-situ XANES measurements (v) Publishing high impact results (vi) Developing independent funding for the research on nuclear materials This SBIR project work led to a commercial instrument product for the niche market of processing and

  13. A Low-Cost, In Situ Resistivity and Temperature Monitoring System

    EPA Science Inventory

    We present a low-cost, reliable method for long-term in situ autonomous monitoring of subsurface resistivity and temperature in a shallow, moderately heterogeneous subsurface. Probes, to be left in situ, were constructed at relatively low cost with close electrode spacing. Once i...

  14. A Low-Cost, In Situ Resistivity and Temperature Monitoring System

    EPA Science Inventory

    We present a low-cost, reliable method for long-term in situ autonomous monitoring of subsurface resistivity and temperature in a shallow, moderately heterogeneous subsurface. Probes, to be left in situ, were constructed at relatively low cost with close electrode spacing. Once i...

  15. In Situ Thermal Ion Temperature Measurements in the E Region Ionosphere: Techniques, Results, and Limitations

    NASA Astrophysics Data System (ADS)

    Burchill, J. K.; Archer, W. E.; Clemmons, J. H.; Knudsen, D. J.; Nicolls, M. J.

    2011-12-01

    In situ measurements of thermal ion temperature are rare at E region altitudes, which are too low for satellites. Here we present ion temperature measurements from a Thermal Ion Imager (TII) that flew on NASA sounding rocket 36.234 (the "Joule-2" mission) into the nightside E region ionosphere on 19 January 2007 from Poker Flat, AK. The TII is an electrostatic ion energy/angle imager that provides 2D ion distributions at 8 ms resolution. Ion temperatures are derived at altitudes between 100 km and 190 km by modelling the detector total count rate versus ion bulk flow angle with respect to the plane of the imager's field of view. Modelling this count rate spin profile shows that the analysis technique is robust against a number of error sources, including variability in payload floating potential, ion upflow, and aperture widening due to reflections from electrode surfaces. A significant uncertainty is associated with the average mass of the ions, which is not measured independently. Using the International Reference Ionosphere model to estimate ion mass, we obtain an ion temperature of 1300 K at 125 km, increasing to more than 3000 K at 180 km. These temperatures are much larger than neutral temperatures obtained from an ionization gauge on the same rocket (Tn˜500 K at 125 km, ˜600 K at 180 km), and do not agree with incoherent scatter radar observations in the vicinity of the rocket. These anomalous ion temperatures are, however, consistent with results from an independent analysis of the shape of the ion distribution images from a similar instrument on a separate payload flown 10 minutes earlier [Archer, MSc Thesis, University of Calgary, 2009]. We conclude that the high ion temperature readings are an artifact related to the environment in the vicinity of the probe, and investigate mechanisms for the cause. We discuss the implications of this effect for future in situ attempts to measure ion temperature in the E region ionosphere.

  16. Comparing Temperature and Precipitation Extremes Across Multiple Reanalyses and Gridded in Situ Observational Datasets

    NASA Astrophysics Data System (ADS)

    Donat, M.; Alexander, L. V.; Sillmann, J.; Wild, S.; Zwiers, F. W.; Lippmann, T.

    2014-12-01

    Changes in climate extremes are often monitored using global gridded datasets of climate extremes based on in situ observations or reanalysis data. This study assesses the consistency of temperature and precipitation extremes between these datasets. We compare temporal evolution and spatial patterns of annual climate extremes indices across multiple global gridded datasets of in situ observations and reanalyses to make inferences on the robustness of the obtained results. While there are distinct differences in the actual values of extremes, normalized time series generally compare well and temporal correlations are high for temperature extremes, in particular for the most recent three decades when satellite data are available for assimilation. Extreme precipitation is characterized by higher temporal and spatial variability than extreme temperatures, and there is less agreement between different datasets than for temperature. However, reasonable agreement between gridded precipitation extremes from the different datasets remains. While there is general agreement between the different reanalyses and gridded observational data in regions with dense observational coverage, different reanalyses show trends of partly opposing signs in areas where in situ observations are sparse, e.g. over parts of Africa and tropical South America. However, in the absence of reliable observations it is difficult to assess which reanalyses are more realistic here than others. Using data from the 20th Century reanalysis and a novel century-long gridded dataset of extremes we also investigate consistency of extremes from these two datasets back to the beginning of the 20th Century. Global average time series of different extremes indices compare generally well over the past 70 years but show larger differences before around 1940. However, in areas with good observational coverage, including North America, Europe and Australia, agreement remains strong also throughout the earlier decades

  17. In-situ temperature measurement in lithium ion battery by transferable flexible thin film thermocouples

    NASA Astrophysics Data System (ADS)

    Mutyala, Madhu Santosh K.; Zhao, Jingzhou; Li, Jianyang; Pan, Hongen; Yuan, Chris; Li, Xiaochun

    2014-08-01

    Temperature monitoring is important for improving the safety and performance of Lithium Ion Batteries (LIB). This paper presents the feasibility study to insert flexible polymer embedded thin film thermocouples (TFTCs) in a lithium ion battery pouch cell for in-situ temperature monitoring. A technique to fabricate polyimide embedded TFTC sensors on glass substrates and later transfer it onto thin copper foils is presented. The sensor transfer process can be easily integrated into the assembly process of a pouch cell, thus holding promise in implementing in Battery Management Systems (BMS). Internal temperature of the LIB pouch cell was measured in-situ when the sensor embedded battery was operated at high rate charge-discharge cycles. The polyimide embedded TFTCs survived the battery assembly process and the battery electrolyte environment. It is observed that the heat generation inside the battery is dominant during the high-rate of discharges. The developed technique can serve to improve the battery safety and performance when implemented in battery management systems and enhance the understanding of heat generation and its effects.

  18. Mid-crust fluid and water-rock interaction kinetic experiments and their geophysical significance: 3. in situ measurements of electric conductance of the water-rock interaction system at high temperatures

    NASA Astrophysics Data System (ADS)

    Hu, S.; Zhang, R.; Zhang, X.

    2013-12-01

    Recently, we designed a new experimental apparatus, which was used to measure dissolution rates as water-rock interactions, and simultaneously in situ measure the electric conductance of the multi phase (rock - fluid) system. At first, a tubular reactor is put in horizontally. The rock sample was crushed and sieved to 20-40 mesh, and cleaned, then put in a titanium network bag inside of the vessel. The electric conductivity detectors were connected to the two ends of the vessel. Fluid inlet and outlet were also fabricated in the two ends of the vessel. And the furnace, temperature controller, liquid pump, back pressure regulator etc. are involved in the whole experimental system. High temperature (T) and pressure (P) electric conductivity measuring system consists of an electric conductivity detector (ECD limit.), which was reformed by us and connected to the vessel; and a transfer: T23-CDH-UM: 5.67(L)×3.50(W)×5.67(H) (inch).The distance between the two electrode of the sensor is 10cm. The electrode is 5cm of length and its diameter is 5/16 inch. Water-rock interaction experiments were performed using this apparatus. The volume inside of vessel is 10.81 ml, l= 170mm, d=4.5mm and 7.246g rock sample put in the vessel. The fluid velocity was changed from 1.5 to 3.5 ml/min, allowing the water through the sample. As in situ to measure the electric conductance of the rock-fluids in the vessel, continuously record the electric conductance, each record in 5 seconds. Water-basalt interaction experiments were carried out and in situ measured electric conductance at high T up to 450°C and at 22 to 36MPa. Basalt sample was collected from natural outcrop (volcanic area in Yangtze valley, China, which is K-rich trachy-basalt. Rock sample was crushed and sieved to 20-40 mesh, and cleaned. 8.0097g sample was put in the vessel (surface area: 1.37m2/g ). Experiments found dissolution rates (dis.r.) for different metals of the rock vary with T. Usually, dis.r., rSi increase with T

  19. In situ soil temperature and heat flux measurements during controlled surface burns at a southern Colorado forest site

    Treesearch

    W. J. Massman; J. M. Frank; W. D. Shepperd; M. J. Platten

    2003-01-01

    This study presents in situ soil temperature measurements at 5-6 depths and heat flux measurements at 2-5 depths obtained during the fall/winter of 2001/ 2002 at seven controlled (surface) fires within a ponderosa pine forest site at the Manitou Experimental Forest in central Colorado. Six of these burns included three different (low, medium, and high) fuel loadings...

  20. High quality protein microarray using in situ protein purification

    PubMed Central

    Kwon, Keehwan; Grose, Carissa; Pieper, Rembert; Pandya, Gagan A; Fleischmann, Robert D; Peterson, Scott N

    2009-01-01

    Background In the postgenomic era, high throughput protein expression and protein microarray technologies have progressed markedly permitting screening of therapeutic reagents and discovery of novel protein functions. Hexa-histidine is one of the most commonly used fusion tags for protein expression due to its small size and convenient purification via immobilized metal ion affinity chromatography (IMAC). This purification process has been adapted to the protein microarray format, but the quality of in situ His-tagged protein purification on slides has not been systematically evaluated. We established methods to determine the level of purification of such proteins on metal chelate-modified slide surfaces. Optimized in situ purification of His-tagged recombinant proteins has the potential to become the new gold standard for cost-effective generation of high-quality and high-density protein microarrays. Results Two slide surfaces were examined, chelated Cu2+ slides suspended on a polyethylene glycol (PEG) coating and chelated Ni2+ slides immobilized on a support without PEG coating. Using PEG-coated chelated Cu2+ slides, consistently higher purities of recombinant proteins were measured. An optimized wash buffer (PBST) composed of 10 mM phosphate buffer, 2.7 mM KCl, 140 mM NaCl and 0.05% Tween 20, pH 7.4, further improved protein purity levels. Using Escherichia coli cell lysates expressing 90 recombinant Streptococcus pneumoniae proteins, 73 proteins were successfully immobilized, and 66 proteins were in situ purified with greater than 90% purity. We identified several antigens among the in situ-purified proteins via assays with anti-S. pneumoniae rabbit antibodies and a human patient antiserum, as a demonstration project of large scale microarray-based immunoproteomics profiling. The methodology is compatible with higher throughput formats of in vivo protein expression, eliminates the need for resin-based purification and circumvents protein solubility and

  1. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability

    NASA Astrophysics Data System (ADS)

    Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang

    2015-09-01

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  2. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability

    SciTech Connect

    Kim, Jungdae; Nam, Hyoungdo; Schroeder, Allan; Shih, Chih-Kang; Qin, Shengyong; Kim, Sang-ui; Eom, Daejin

    2015-09-15

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  3. Compact low temperature scanning tunneling microscope with in-situ sample preparation capability.

    PubMed

    Kim, Jungdae; Nam, Hyoungdo; Qin, Shengyong; Kim, Sang-ui; Schroeder, Allan; Eom, Daejin; Shih, Chih-Kang

    2015-09-01

    We report on the design of a compact low temperature scanning tunneling microscope (STM) having in-situ sample preparation capability. The in-situ sample preparation chamber was designed to be compact allowing quick transfer of samples to the STM stage, which is ideal for preparing temperature sensitive samples such as ultra-thin metal films on semiconductor substrates. Conventional spring suspensions on the STM head often cause mechanical issues. To address this problem, we developed a simple vibration damper consisting of welded metal bellows and rubber pads. In addition, we developed a novel technique to ensure an ultra-high-vacuum (UHV) seal between the copper and stainless steel, which provides excellent reliability for cryostats operating in UHV. The performance of the STM was tested from 2 K to 77 K by using epitaxial thin Pb films on Si. Very high mechanical stability was achieved with clear atomic resolution even when using cryostats operating at 77 K. At 2 K, a clean superconducting gap was observed, and the spectrum was easily fit using the BCS density of states with negligible broadening.

  4. Validation of Land Surface Temperature products in arid climate regions with permanent in-situ measurements

    NASA Astrophysics Data System (ADS)

    Goettsche, F.; Olesen, F.; Trigo, I.; Hulley, G. C.

    2013-12-01

    Land Surface Temperature (LST) is operationally obtained from several space-borne sensors, e.g. from the Spinning Enhanced Visible and Infrared Imager (SEVIRI) onboard Meteosat Second Generation (MSG) by the Land Surface Analysis - Satellite Application Facility (LSA-SAF) and from the Moderate Resolution Imaging Spectroradiometer (MODIS) on EOS-Terra by the MODIS Land Team. The relative accuracy of LST products can be assessed by cross-validating different products. Alternatively, the so-called 'radiance based validation' can be used to compare satellite-retrieved LST with results from radiative transfer models: however, this requires precise a priori knowledge of land surface emissivity (LSE) and atmospheric conditions. Ultimately, in-situ measurements (';ground truth') are needed for validating satellite LST&E products. Therefore, the LST product derived by LSA-SAF is validated with independent in-situ measurements (';temperature based validation') at permanent validation stations located in different climate regions on the SEVIRI disk. In-situ validation is largely complicated by the spatial scale mismatch between satellite sensors and ground based sensors, i.e. areas observed by ground radiometers usually cover about 10 m2, whereas satellite measurements in the thermal infrared typically cover between 1 km2 and 100 km2. Furthermore, an accurate characterization of the surface is critical for all validation approaches, but particularly over arid regions, as shown by in-situ measurements revealing that LSE products can be wrong by more than 3% [1]. The permanent stations near Gobabeb (Namibia; hyper-arid desert climate) and Dahra (Senegal; hot-arid steppe-prairie climate) are two of KIT's four dedicated LST validation stations. Gobabeb station is located on vast and flat gravel plains (several 100 km2), which are mainly covered by coarse gravel, sand, and desiccated grass. The gravel plains are highly homogeneous in space and time, which makes them ideal for

  5. In-situ studies on the micro-structure evolution of A2W2O7 (A = Li, Na, K) during melting by high temperature Raman spectroscopy and density functional theory

    NASA Astrophysics Data System (ADS)

    Wang, Jian; You, Jinglin; Wang, Min; Lu, Liming; Wan, Songming; Sobol, A. A.

    2017-10-01

    In-situ high temperature Raman spectroscopic (HTRS) technique in combination with density functional theory (DFT) analysis has been adopted to investigate the micro-structure of solid and molten A2W2O7 (A = Li, Na, K). The [WO6] octahedra were found to be connected to each other by corner and edge sharing in the crystalline Li2W2O7 and K2W2O7 compounds. In the crystal lattice of Na2W2O7, on the other hand, the [WO4] tetrahedra and [WO6] octahedra were found to coexist and paired by corner sharing. Although the structural diversity has clearly led to distinct Raman spectra of the crystalline A2W2O7 compounds, the spectra of their melts tended to be analogous, showing the typical vibration modes of (W2O7)2 - dimer. A mechanism was then proposed to explain the structure evolution occurring during the melting process of A2W2O7. The effect of A+ cation on the Raman bands of (W2O7)2 - dimer in molten A2W2O7 has also been investigated. Both the wavenumber and full width at half-height (FWHH) of the characteristic band assigned to the symmetrical stretching vibration mode of Wsbnd Onb (non-bridging oxygen) in (W2O7)2 - were found to decrease in the sequence of Li+, Na+ and K+, indicating the cation effect on the mean bond length and its distribution range of Wsbnd Onb. In addition, the relative intensity of this band was also influenced by the cation and it was increased in the order of Li2W2O7, Na2W2O7 and K2W2O7, which has been explained by the charge transfer process and confirmed by Mulliken overlap population analysis.

  6. In-situ studies on the micro-structure evolution of A2W2O7 (A=Li, Na, K) during melting by high temperature Raman spectroscopy and density functional theory.

    PubMed

    Wang, Jian; You, Jinglin; Wang, Min; Lu, Liming; Wan, Songming; Sobol, A A

    2017-10-05

    In-situ high temperature Raman spectroscopic (HTRS) technique in combination with density functional theory (DFT) analysis has been adopted to investigate the micro-structure of solid and molten A2W2O7 (A=Li, Na, K). The [WO6] octahedra were found to be connected to each other by corner and edge sharing in the crystalline Li2W2O7 and K2W2O7 compounds. In the crystal lattice of Na2W2O7, on the other hand, the [WO4] tetrahedra and [WO6] octahedra were found to coexist and paired by corner sharing. Although the structural diversity has clearly led to distinct Raman spectra of the crystalline A2W2O7 compounds, the spectra of their melts tended to be analogous, showing the typical vibration modes of (W2O7)(2-) dimer. A mechanism was then proposed to explain the structure evolution occurring during the melting process of A2W2O7. The effect of A(+) cation on the Raman bands of (W2O7)(2-) dimer in molten A2W2O7 has also been investigated. Both the wavenumber and full width at half-height (FWHH) of the characteristic band assigned to the symmetrical stretching vibration mode of WOnb (non-bridging oxygen) in (W2O7)(2-) were found to decrease in the sequence of Li(+), Na(+) and K(+), indicating the cation effect on the mean bond length and its distribution range of WOnb. In addition, the relative intensity of this band was also influenced by the cation and it was increased in the order of Li2W2O7, Na2W2O7 and K2W2O7, which has been explained by the charge transfer process and confirmed by Mulliken overlap population analysis. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. In situ tryptophan-like fluorometers: assessing turbidity and temperature effects for freshwater applications.

    PubMed

    Khamis, K; Sorensen, J P R; Bradley, C; Hannah, D M; Lapworth, D J; Stevens, R

    2015-04-01

    Tryptophan-like fluorescence (TLF) is an indicator of human influence on water quality as TLF peaks are associated with the input of labile organic carbon (e.g. sewage or farm waste) and its microbial breakdown. Hence, real-time measurement of TLF could be particularly useful for monitoring water quality at a higher temporal resolution than available hitherto. However, current understanding of TLF quenching/interference is limited for field deployable sensors. We present results from a rigorous test of two commercially available submersible tryptophan fluorometers (ex ∼ 285, em ∼ 350). Temperature quenching and turbidity interference were quantified in the laboratory and compensation algorithms developed. Field trials were then undertaken involving: (i) an extended deployment (28 days) in a small urban stream; and, (ii) depth profiling of an urban multi-level borehole. TLF was inversely related to water temperature (regression slope range: -1.57 to -2.50). Sediment particle size was identified as an important control on the turbidity specific TLF response, with signal amplification apparent <150 NTU for clay particles and <650 NTU for silt particles. Signal attenuation was only observed >200 NTU for clay particles. Compensation algorithms significantly improved agreement between in situ and laboratory readings for baseflow and storm conditions in the stream. For the groundwater trial, there was an excellent agreement between laboratory and raw in situ TLF; temperature compensation provided only a marginal improvement, and turbidity corrections were unnecessary. These findings highlight the potential utility of real time TLF monitoring for a range of environmental applications (e.g. tracing polluting sources and monitoring groundwater contamination). However, in situations where high/variable suspended sediment loads or rapid changes in temperature are anticipated concurrent monitoring of turbidity and temperature is required and site specific calibration is

  8. Bedrock temperature as a potential method for monitoring change in crustal stress: Theory, in situ measurement, and a case history

    NASA Astrophysics Data System (ADS)

    Chen, Shunyun; Liu, Peixun; Liu, Liqiang; Ma, Jin

    2016-06-01

    Experimental studies have confirmed that temperature is notably affected by rock deformation; therefore, change in crustal stress should be indicated by measurable changes in bedrock temperature. In this work, we investigated the possibility that the bedrock temperature might be used to explore the state of crustal stress. In situ measurement of bedrock temperature at three stations from 2011 to 2013 was used as the basis for the theoretical analysis of this approach. We began with theoretical analyses of temperature response to change in crustal stress, and of the effect of heat conduction. This allowed distinction between temperature changes produced by crustal stress (stress temperature) from temperature changes caused by conduction from the land surface (conduction temperature). Stress temperature has two properties (synchronous response and a high-frequency feature) that allow it to be distinguished from conduction temperature. The in situ measurements confirmed that apparently synchronous changes in the stress temperature of the bedrock occur and that there exist obvious short-term components of the in situ bedrock temperature, which agrees with theory. On 20 April 2013, an earthquake occurred 95 km away from the stations, fortuitously providing a case study by which to verify our method for obtaining the state of crustal stress using temperature. The results indicated that the level of local or regional seismic activity, representing the level of stress adjustment, largely accords with the stress temperature. This means that the bedrock temperature is a tool that might be applied to understand the state of stress during seismogenic tectonics. Therefore, it is possible to record changes in the state of crustal stress in a typical tectonic position by long-term observation of bedrock temperature. Hereby, the measurement of bedrock temperature has become a new tool for gaining insight into changes in the status of shallow crustal stress.

  9. In situ characterisation of nanostructured multiphase thermoelectric materials at elevated temperatures.

    PubMed

    Aminorroaya Yamini, S; Mitchell, D R G; Avdeev, M

    2016-12-07

    Multiphase thermoelectric materials have recently attracted considerable attention due to the high thermoelectric efficiencies which can be achieved in these compounds compared to their single-phase counterparts. However, there is very little known on the structural evolution of these phases as a function of temperature. In this work we performed an in situ high temperature structural characterisation of recently reported high efficiency p-type multiphase (PbTe)0.65(PbS)0.25(PbSe)0.1 compounds by hot stage transmission electron microscopy and high-resolution neutron powder diffraction. We observed the microstructural evolution of precipitates and determined the lattice parameters of phases as a function of temperature for materials, which have been heavily and lightly doped with sodium. The role of the sodium is to optimize the concentration of charge carriers. It has been shown to distribute heterogeneously between the phases in multiphase compounds. The dissolution of secondary phases is found to occur at elevated temperatures. Although sodium concentration produces no significant differences between the lattice constants of the phases and the dissolution sequence of precipitates, it affects quite significantly the kinetics of precipitation. The heavily doped samples reach structural thermodynamic equilibrium more quickly than the lightly doped compound. These results are a step forward in designing high performance multiphase thermoelectric materials.

  10. Low temperature barriers for use with in situ processes

    SciTech Connect

    Kim, Dong Sub; Vinegar, Harold J

    2009-06-16

    A method of forming and maintaining a low temperature zone around at least a portion of a subsurface treatment area is described. The method includes reducing a temperature of heat transfer fluid with a refrigeration system. The heat transfer fluid is circulated through freeze well canisters and placed in a formation around at least a portion of the subsurface treatment area. An initial temperature of the heat transfer fluid supplied to a first freeze well canister is in a range from about -35 .degree. C. to about -55 .degree. C. At least one of the well canisters includes carbon steel. The heat transfer fluid is returned to the refrigeration system.

  11. In situ temperature tunable pores of shape memory polyurethane membranes

    NASA Astrophysics Data System (ADS)

    Ahn, Joon-Sung; Yu, Woong-Ryeol; Youk, Ji Ho; Youk Ryu, Hee

    2011-10-01

    Conventional shape memory polymers, such as shape memory polyurethanes (SMPU), can exhibit net two-way shape memory behavior (2WSM), i.e., upon heating and subsequent cooling, their macroscopic shapes change reversibly under an applied bias load. This paper is aimed at reporting similar 2WSM behavior, especially by focusing on the size of nanopores/micropores in SMPU membranes, i.e., the size of the pores can be reversibly changed by up to about 300 nm upon repeated heating and cooling. The SMPU membranes were prepared by electrospinning and elongated at temperatures higher than the transition temperature of the SMPU. Under the constant stress, the size change of the pores in the membranes was measured by applying cyclic temperature change. It was observed that the pore size changed from 150 to 440 nm according to the temperature change, demonstrating that the SMPU membrane can be utilized as a smart membrane to selectively separate substances according to their sizes by just controlling temperature.

  12. The validation of ATSR measurements with in situ sea temperatures

    SciTech Connect

    Minnett, P.J.; Stansfield, K.L.

    1993-10-08

    The largest source of uncertainty in the retrieval of SST (sea-surface) temperature from space-borne infrared radiometric measurements is in the correction for the effects of the intervening atmosphere. During a research cruise of the R/V Alliance measurements of sea surface temperature, surface meteorological variables and surface infrared radiances were taken. SST fields were generated from the ATSR data using pre-launch algorithims derived by the ATSR Instrument Team (A.M. Zavody, personal communication), and the initial comparison between ATSR measurements and SST taken along the ship`s track indicate that the dual-angle atmospheric correction is accurate in mid-latitude conditions.

  13. RNA fluorescence in situ hybridization for high-content screening.

    PubMed

    Querido, Emmanuelle; Dekakra-Bellili, Lynda; Chartrand, Pascal

    2017-08-15

    Single molecule RNA imaging using fluorescent in situ hybridization (FISH) can provide quantitative information on mRNA abundance and localization in a single cell. There is now a growing interest in screening for modifiers of RNA abundance and/or localization. For instance, microsatellite expansion within RNA can lead to toxic gain-of-function via mislocalization of these transcripts into RNA aggregate and sequestration of RNA-binding proteins. Screening for inhibitors of these RNA aggregate can be performed by high-throughput RNA FISH. Here we describe detailed methods to perform single molecule RNA FISH in multiwell plates for high-content screening (HCS) microscopy. We include protocols adapted for HCS with either standard RNA FISH with fluorescent oligonucleotide probes or the recent single molecule inexpensive FISH (smiFISH). Recommendations for success in HCS microscopy with high magnification objectives are discussed. Copyright © 2017 Elsevier Inc. All rights reserved.

  14. Plastic deformation of quartz at room temperature by SEM in situ micropillar compression

    NASA Astrophysics Data System (ADS)

    Maeder, X.; Ghisleni, R.; Michler, J.

    2010-12-01

    Rock material deformation behavior has been studied for many decades using experimental deformation apparatus, usually at high confining pressure and temperature, in order to simulate geological deformation conditions and to reach ductile deformation behavior. Such experiments are usually time consuming, the sample preparation is delicate and only the final deformed product can be analyzed. Additionally, only centimeter to millimeter sized samples can be analyzed. It has been recently discovered that the mechanical behavior of a crystalline material can change as the size of the system in question approaches any characteristic length scale associated with the dislocation processes of the material (Michler et al. 2007). Several proprieties are affected by a material’s internal and in some cases external length scales, such as the yield stress, the hardness, the brittle-to-ductile transition temperature and the fracture toughness. Length-scale dependent values of the mechanical proprieties of rocks materials and minerals have never been tested so far. They are however fundamental for the understanding of the rheology of rocks, as they may constrain for instance the deformation behavior of mylonite or ultramylonite where the grain size reaches micro- to nano- values. In order to address this issue, SEM in situ micropillar compression of natural quartz has been performed. Two sets of samples have been tested with the compression axis perpendicular to respectively the c- and the z-planes. The pillar have been fabricated by a focus ion beam from a bulk single crystal and deformed by a SEM in situ microindenter equipped with a flat diamond punch. The results show that ductile deformation occurs at room temperature with pillars of 1 micron diameter for both orientations, with yield stress of about 8.3 and 6.9 GPa for the pillars oriented parallel to respectively the c- and z-axis. Pillars oriented parallel to the c-axis show rhomb {r} slip planes and the ones

  15. In Situ Irradiation and Measurement of Triple Junction Solar Cells at Low Intensity, Low Temperature (LILT) Conditions

    NASA Technical Reports Server (NTRS)

    Harris, R.D.; Imaizumi, M.; Walters, R.J.; Lorentzen, J.R.; Messenger, S.R.; Tischler, J.G.; Ohshima, T.; Sato, S.; Sharps, P.R.; Fatemi, N.S.

    2008-01-01

    The performance of triple junction InGaP/(In)GaAs/Ge space solar cells was studied following high energy electron irradiation at low temperature. Cell characterization was carried out in situ at the irradiation temperature while using low intensity illumination, and, as such, these conditions reflect those found for deep space, solar powered missions that are far from the sun. Cell characterization consisted of I-V measurements and quantum efficiency measurements. The low temperature irradiations caused substantial degradation that differs in some ways from that seen after room temperature irradiations. The short circuit current degrades more at low temperature while the open circuit voltage degrades more at room temperature. A room temperature anneal after the low temperature irradiation produced a substantial recovery in the degradation. Following irradiation at both temperatures and an extended room temperature anneal, quantum efficiency measurement suggests that the bulk of the remaining damage is in the (In)GaAs sub-cell

  16. In Situ Irradiation and Measurement of Triple Junction Solar Cells at Low Intensity, Low Temperature (LILT) Conditions

    NASA Technical Reports Server (NTRS)

    Harris, R.D.; Imaizumi, M.; Walters, R.J.; Lorentzen, J.R.; Messenger, S.R.; Tischler, J.G.; Ohshima, T.; Sato, S.; Sharps, P.R.; Fatemi, N.S.

    2008-01-01

    The performance of triple junction InGaP/(In)GaAs/Ge space solar cells was studied following high energy electron irradiation at low temperature. Cell characterization was carried out in situ at the irradiation temperature while using low intensity illumination, and, as such, these conditions reflect those found for deep space, solar powered missions that are far from the sun. Cell characterization consisted of I-V measurements and quantum efficiency measurements. The low temperature irradiations caused substantial degradation that differs in some ways from that seen after room temperature irradiations. The short circuit current degrades more at low temperature while the open circuit voltage degrades more at room temperature. A room temperature anneal after the low temperature irradiation produced a substantial recovery in the degradation. Following irradiation at both temperatures and an extended room temperature anneal, quantum efficiency measurement suggests that the bulk of the remaining damage is in the (In)GaAs sub-cell

  17. Investigation of the high-temperature redox chemistry of Sr2Fe1.5Mo0.5O6-δ via in situ neutron diffraction

    SciTech Connect

    Bugaris, Daniel E.; Hodges, Jason P.; Huq, Ashfia; Chance, W. Michael; Heyden, Andreas; Chen, Fanglin; Loye, Hans-Conrad zur

    2014-02-07

    We investigated crystallographic structural changes for Sr2Fe1.5Mo0.5O6-δ, an electrode material for symmetric solid oxide fuel cells. These samples were heated and cooled in wet hydrogen and wet oxygen atmospheres, to simulate the reducing and oxidizing conditions experienced under actual fuel cell operating conditions, and their structures and oxygen contents were determined using in situ powder neutron diffraction. The existence of a reversible tetragonal to cubic phase transition was established to occur between room temperature and 400 °C, both on heating and cooling in either oxygen or hydrogen. Furthermore, the oxygen content reaches a low value of 5.50(2) at 850 °C in wet hydrogen. Excellent correlations are observed between the oxygen content of the structure and the conductivities reported in the literature.

  18. Development of a temperature gradient focusing method for in situ extraterrestrial biomarker analysis.

    PubMed

    Danger, Grégoire; Ross, David

    2008-08-01

    Scanning temperature gradient focusing (TGF) is a recently described technique for the simultaneous concentration and separation of charged analytes. It allows for high analyte peak capacities and low LODs in microcolumn electrophoretic separations. In this paper, we present the application of scanning TGF for chiral separations of amino acids. Using a mixture of seven carboxyfluorescein succinimidyl ester-labeled amino acids (including five chiral amino acids) which constitute the Mars7 standard, we show that scanning TGF is a very simple and efficient method for chiral separations. The modulation of TGF separation parameters (temperature window, pressure scan rate, temperature range, and chiral selector concentration) allows optimization of peak efficiencies and analyte resolutions. The use of hydroxypropyl-beta-CD at low concentration (1-5 mmol/L) as a chiral selector, with an appropriate pressure scan rate ( -0.25 Pa/s) and with a low temperature range (3-25 degrees C over 1 cm) provided high resolution between enantiomers (Rs >1.5 for each pair of enantiomers) using a short, 4 cm long capillary. With these new results, the scanning TGF method appears to be a viable method for in situ trace biomarker analysis for future missions to Mars or other solar system bodies.

  19. Temperature-responsive compounds as in situ gelling biomedical materials.

    PubMed

    Moon, Hyo Jung; Ko, Du Young; Park, Min Hee; Joo, Min Kyung; Jeong, Byeongmoon

    2012-07-21

    Aqueous solutions that undergo sol-to-gel transition as the temperature increases have been extensively studied during the last decade. The material can be designed by controlling the hydrophilic and hydrophobic balance of the material. Basically, the molecular weight of the hydrophilic block and hydrophobic block of a compound should be fine-tuned from the synthetic point of view. In addition, stereochemistry, microsequence, topology, and nanostructures of the compound also affect the transition temperature, gel window, phase diagram, and modulus of the gel. From a practical point of view, biodegradability, biocompatibility, and interactions between the material and drug or cell should be considered in designing a thermogelling material. The interactions are particularly important in that they control drug release profile and initial burst release of the drug in the drug delivery system, and affect cell proliferation, differentiation, and biomarker expression in three-dimensional cell culture and tissue engineering application. This review provides an in-depth summary of the recent progress of thermogelling systems including polymers, low molecular compounds, and nanoemulsions. Their biomedical applications were also comparatively discussed. In addition, perspectives on future material design of a new thermogelling material and its application are suggested.

  20. Calibrating IR cameras for in-situ temperature measurement during the electron beam melt processing of Inconel 718 and Ti-Al6-V4

    NASA Astrophysics Data System (ADS)

    Dinwiddie, R. B.; Kirka, M. M.; Lloyd, P. D.; Dehoff, R. R.; Lowe, L. E.; Marlow, G. S.

    2016-05-01

    High performance mid-wave infrared (IR) cameras are used for in-situ electron beam melt process monitoring and temperature measurements. Since standard factory calibrations are insufficient due to very low transmissions of the leaded glass window required for X-ray absorption, two techniques for temperature calibrations are compared. In-situ measurement of emittance will also be discussed. Ultimately, these imaging systems have the potential for routine use for online quality assurance and feedback control.

  1. Room-temperature in situ nuclear spin hyperpolarization from optically pumped nitrogen vacancy centres in diamond

    SciTech Connect

    King, Jonathan P.; Jeong, Keunhong; Vassiliou, Christophoros C.; Shin, Chang S.; Page, Ralph H.; Avalos, Claudia E.; Wang, Hai-Jing; Pines, Alexander

    2015-12-07

    Low detection sensitivity stemming from the weak polarization of nuclear spins is a primary limitation of magnetic resonance spectroscopy and imaging. Methods have been developed to enhance nuclear spin polarization but they typically require high magnetic fields, cryogenic temperatures or sample transfer between magnets. Here we report bulk, room-temperature hyperpolarization of 13C nuclear spins observed via high-field magnetic resonance. The technique harnesses the high optically induced spin polarization of diamond nitrogen vacancy centres at room temperature in combination with dynamic nuclear polarization. We observe bulk nuclear spin polarization of 6%, an enhancement of ~170,000 over thermal equilibrium. The signal of the hyperpolarized spins was detected in situ with a standard nuclear magnetic resonance probe without the need for sample shuttling or precise crystal orientation. In conclusion, hyperpolarization via optical pumping/dynamic nuclear polarization should function at arbitrary magnetic fields enabling orders of magnitude sensitivity enhancement for nuclear magnetic resonance of solids and liquids under ambient conditions.

  2. Room-temperature in situ nuclear spin hyperpolarization from optically pumped nitrogen vacancy centres in diamond

    DOE PAGES

    King, Jonathan P.; Jeong, Keunhong; Vassiliou, Christophoros C.; ...

    2015-12-07

    Low detection sensitivity stemming from the weak polarization of nuclear spins is a primary limitation of magnetic resonance spectroscopy and imaging. Methods have been developed to enhance nuclear spin polarization but they typically require high magnetic fields, cryogenic temperatures or sample transfer between magnets. Here we report bulk, room-temperature hyperpolarization of 13C nuclear spins observed via high-field magnetic resonance. The technique harnesses the high optically induced spin polarization of diamond nitrogen vacancy centres at room temperature in combination with dynamic nuclear polarization. We observe bulk nuclear spin polarization of 6%, an enhancement of ~170,000 over thermal equilibrium. The signal ofmore » the hyperpolarized spins was detected in situ with a standard nuclear magnetic resonance probe without the need for sample shuttling or precise crystal orientation. In conclusion, hyperpolarization via optical pumping/dynamic nuclear polarization should function at arbitrary magnetic fields enabling orders of magnitude sensitivity enhancement for nuclear magnetic resonance of solids and liquids under ambient conditions.« less

  3. In situ studies of microbial inactivation during high pressure processing

    NASA Astrophysics Data System (ADS)

    Maldonado, Jose Antonio; Schaffner, Donald W.; Cuitiño, Alberto M.; Karwe, Mukund V.

    2016-01-01

    High pressure processing (HPP) has been shown to reduce microbial concentration in foods. The mechanisms of microbial inactivation by HPP have been associated with damage to cell membranes. The real-time response of bacteria to HPP was measured to elucidate the mechanisms of inactivation, which can aid in designing more effective processes. Different pressure cycling conditions were used to expose Enterobacter aerogenes cells to HPP. Propidium iodide (PI) was used as a probe, which fluoresces after penetrating cells with damaged membranes and binding with nucleic acids. A HPP vessel with sapphire windows was used for measuring fluorescence in situ. Membrane damage was detected during pressurization and hold time, but not during depressurization. The drop in fluorescence was larger than expected after pressure cycles at higher pressure and longer times. This indicated possible reversible disassociation of ribosomes resulting in additional binding of PI to exposed RNA under pressure and its release after depressurization.

  4. Surface Temperature Trends in the Arctic and the Antarctic from AVHRR and In Situ Data

    NASA Astrophysics Data System (ADS)

    Perez, G. J. P.; Comiso, J. C.

    2015-12-01

    The earliest signals of a climate change are expected to be observed in the polar regions in part because of the high reflectively of snow and ice. Because of general inaccessibility, there is a paucity of in situ data and hence the need to use satellite data to observe the large-scale variability and trends in surface temperature in the two regions. The sensor with the longest satellite record on temperature has been the NOAA/Advanced Very High Resolution Radiometer (AVHRR) that has provided continuous thermal infrared data for more than 33 years. The results of analysis of the data show that there is indeed a strong signal coming from the Arctic with the trend in surface temperature (for the region > 64°N) being 0.6°C per decade which is about 3 times the global trend of 0.2°C per decade for the same period. It appeared surprising when the results from a similar region (> 64 °S) in the Antarctic show a much lower trend and comparable to the global trend. The primary source of error in the temperature data is cloud masking associated with the similar signatures of clouds and snow/ice covered surfaces. However, the derived AVHRR data show good consistency with in situ data with standard deviation less than 1°C. The AVHRR time series has also been compared and showed compatibility with data from the Aqua/Moderate Resolution Imaging Spectroradiometer (MODIS) which have been available from 2000 to the present. Some differences in the trends from the two hemispheres are expected because of very different geographical environments in the two regions. The relationships of the trend with the atmospheric global circulation in the north, as defined by the Northern Annular Mode (NAM), and that in the south, as defined by the Southern Annular Mode (SAM), have been observed to be generally weak. The occurrences of the Antarctic Circumpolar Wave (ACW) and ENSO were also studied and not considered a significant factor. It is intriguing that the observed variability in

  5. High Temperature Piezoelectric Drill

    NASA Technical Reports Server (NTRS)

    Bao, Xiaoqi; Scott, James; Boudreau, Kate; Bar-Cohen, Yoseph; Sherrit, Stewart; Badescu, Mircea; Shrout, Tom; Zhang, Shujun

    2009-01-01

    The current NASA Decadal mission planning effort has identified Venus as a significant scientific target for a surface in-situ sampling/analyzing mission. The Venus environment represents several extremes including high temperature (460 deg C), high pressure (9 MPa), and potentially corrosive (condensed sulfuric acid droplets that adhere to surfaces during entry) environments. This technology challenge requires new rock sampling tools for these extreme conditions. Piezoelectric materials can potentially operate over a wide temperature range. Single crystals, like LiNbO3, have a Curie temperature that is higher than 1000 deg C and the piezoelectric ceramics Bismuth Titanate higher than 600 deg C. A study of the feasibility of producing piezoelectric drills that can operate in the temperature range up to 500 deg C was conducted. The study includes the high temperature properties investigations of engineering materials and piezoelectric ceramics with different formulas and doping. The drilling performances of a prototype Ultrasonic/Sonic Drill/Corer (USDC) using high temperate piezoelectric ceramics and single crystal were tested at temperature up to 500 deg C. The detailed results of our study and a discussion of the future work on performance improvements are presented in this paper.

  6. High Temperature Piezoelectric Drill

    NASA Technical Reports Server (NTRS)

    Bao, Xiaoqi; Scott, James; Boudreau, Kate; Bar-Cohen, Yoseph; Sherrit, Stewart; Badescu, Mircea; Shrout, Tom; Zhang, Shujun

    2009-01-01

    The current NASA Decadal mission planning effort has identified Venus as a significant scientific target for a surface in-situ sampling/analyzing mission. The Venus environment represents several extremes including high temperature (460 deg C), high pressure (9 MPa), and potentially corrosive (condensed sulfuric acid droplets that adhere to surfaces during entry) environments. This technology challenge requires new rock sampling tools for these extreme conditions. Piezoelectric materials can potentially operate over a wide temperature range. Single crystals, like LiNbO3, have a Curie temperature that is higher than 1000 deg C and the piezoelectric ceramics Bismuth Titanate higher than 600 deg C. A study of the feasibility of producing piezoelectric drills that can operate in the temperature range up to 500 deg C was conducted. The study includes the high temperature properties investigations of engineering materials and piezoelectric ceramics with different formulas and doping. The drilling performances of a prototype Ultrasonic/Sonic Drill/Corer (USDC) using high temperate piezoelectric ceramics and single crystal were tested at temperature up to 500 deg C. The detailed results of our study and a discussion of the future work on performance improvements are presented in this paper.

  7. Winter frost resistance of Pinus cembra measured in situ at the alpine timberline as affected by temperature conditions.

    PubMed

    Buchner, Othmar; Neuner, Gilbert

    2011-11-01

    Winter frost resistance (WFR), midwinter frost hardening and frost dehardening potential of Pinus cembra L. were determined in situ by means of a novel low-temperature freezing system at the alpine timberline ecotone (1950 m a.s.l., Mt Patscherkofel, Innsbruck, Austria). In situ liquid nitrogen (LN₂)-quenching experiments should check whether maximum WFR of P. cembra belonging to the frost hardiest conifer group, being classified in US Department of Agriculture climatic zone 1, suffices to survive dipping into LN₂ (-196 °C). Viability was assessed in a field re-growth test. Maximum in situ WFR (LT₅₀) of leaves was <- 75 °C and that of buds was less (-70.3 °C), matching the lowest water contents. In midwinter, in situ freezing exotherms of leaves, buds and the xylem were often not detectable. Ice formed in the xylem at a mean of -2.8 °C and in leaves at -3.3 °C. In situ WFR of P. cembra was higher than that obtained on detached twigs, as reported earlier. In situ LN₂-quenching experiments were lethal in all cases even when twigs of P. cembra were exposed to an in situ frost hardening treatment (12 days at -20 °C followed by 3 days at -50 °C) to induce maximum WFR. Temperature treatments applied in the field significantly affected the actual WFR. In January a frost hardening treatment (21 days at -20 °C) led to a significant increase of WFR (buds: -62 °C to <- 70 °C; leaves: -59.6 °C to -65.2 °C), showing that P. cembra was not at its specific maximum WFR. In contrast, simulated warm spells in late winter led to premature frost dehardening (buds: -32.6 °C to -10.2 °C; leaves: -32.7 to -16.4 °C) followed by significantly earlier bud swelling and burst in late winter. Strikingly, both temperature treatments, either increased air temperature (+10.1 °C) or increased soil temperature (+6.5 °C), were similarly effective. This high readiness to frost harden and deharden in winter in the field must be considered to be of great significance for

  8. Low temperature selective epitaxy of in situ doped silicon and applications in nanoscale CMOS

    NASA Astrophysics Data System (ADS)

    Ban, Ibrahim

    Continuous scaling of the Complementary Metal-Oxide-Semiconductor (CMOS) devices places stringent requirements on conventional doping technologies such as ion implantation. To keep the short channel effects under control while obtaining acceptable device characteristics, super-retrograde channel profiles and ultra-shallow source-drain junctions will be required in the sub 0.1 mum regime. In this study, in-situ doped selective silicon films grown at 800°C in an Ultra-High Vacuum Rapid Thermal Chemical Vapor Deposition (UHV-RTCVD) reactor were investigated to form highly non-uniform doping profiles for channel engineering as well as ultra-shallow p+-n junctions. In-situ boron incorporation in the low-to-heavy doping range (10 16 cm--3-1019 cm--3 ) was studied and modeled with respect to silicon growth rate, diborane (B2H6), chlorine (Cl2), and hydrogen partial pressures. Multi-layer ultra-thin (100 A-500 A) in-situ boron doped films were characterized. Effects of interface contamination (oxygen and carbon), which takes place during multi-layer growth with temperature switching, on impurity (boron, carbon, and oxygen) diffusion were investigated. Using this process, very short channel lightly-doped (Leff = 0.12 mum) and moderately-doped (Leff = 0.25 mum) NMOSFETs were fabricated with respectable device characteristics. The investigations were then extended to phosphorus incorporation using phosphine (PH3) as a source gas. In the second part of our work, a heavily boron-doped silicon deposition process was developed. Growth kinetics, surface morphology, selectivity, and out-diffusion behavior were studied. We demonstrated ultra-shallow (Xj ≤ 400 A) p+-n junctions by diffusion from these films with a high interface concentration (2 x 1020 cm--3 ) achieving the lowest sheet resistance values (Rs ≤ 50 O/Sq.) reported by any technique to date. We also demonstrated, for the first time, Zero-Depth p+-n junctions using as-deposited unannealed heavily-boron-doped silicon

  9. Stream temperature estimated in situ from thermal-infrared images: best estimate and uncertainty

    NASA Astrophysics Data System (ADS)

    Iezzi, F.; Todisco, M. T.

    2015-11-01

    The paper aims to show a technique to estimate in situ the stream temperature from thermal-infrared images deepening its best estimate and uncertainty. Stream temperature is an important indicator of water quality and nowadays its assessment is important particularly for thermal pollution monitoring in water bodies. Stream temperature changes are especially due to the anthropogenic heat input from urban wastewater and from water used as a coolant by power plants and industrial manufacturers. The stream temperatures assessment using ordinary techniques (e.g. appropriate thermometers) is limited by sparse sampling in space due to a spatial discretization necessarily punctual. Latest and most advanced techniques assess the stream temperature using thermal-infrared remote sensing based on thermal imagers placed usually on aircrafts or using satellite images. These techniques assess only the surface water temperature and they are suitable to detect the temperature of vast water bodies but do not allow a detailed and precise surface water temperature assessment in limited areas of the water body. The technique shown in this research is based on the assessment of thermal-infrared images obtained in situ via portable thermal imager. As in all thermographic techniques, also in this technique, it is possible to estimate only the surface water temperature. A stream with the presence of a discharge of urban wastewater is proposed as case study to validate the technique and to show its application limits. Since the technique analyzes limited areas in extension of the water body, it allows a detailed and precise assessment of the water temperature. In general, the punctual and average stream temperatures are respectively uncorrected and corrected. An appropriate statistical method that minimizes the errors in the average stream temperature is proposed. The correct measurement of this temperature through the assessment of thermal- infrared images obtained in situ via portable

  10. In situ fabrication of a temperature- and ethanol-responsive smart membrane in a microchip.

    PubMed

    Sun, Yi-Meng; Wang, Wei; Wei, Yun-Yan; Deng, Nan-Nan; Liu, Zhuang; Ju, Xiao-Jie; Xie, Rui; Chu, Liang-Yin

    2014-07-21

    Here we report a simple and versatile strategy for the in situ fabrication of nanogel-containing smart membranes in microchannels of microchips. The fabrication approach is demonstrated by the in situ formation of a chitosan membrane containing poly(N-isopropylacrylamide) (PNIPAM) nanogels in a microchannel of a microchip. The PNIPAM nanogels, that allow temperature- and ethanol-responsive swelling-shrinking volume transitions, serve as smart nanovalves for controlling the diffusional permeability of solutes across the membrane. Such self-regulation of the membrane permeability is investigated by using fluorescein isothiocyanate (FITC) as a tracer molecule. This approach provides a promising strategy for the in situ fabrication of versatile nanogel-containing smart membranes within microchips via simply changing the functional nanogels for developing micro-scale detectors, sensors, separators and controlled release systems.

  11. Acoustic travel time gauges for in-situ determination of pressure and temperature in multi-anvil apparatus

    SciTech Connect

    Wang, Xuebing; Chen, Ting; Qi, Xintong; Zou, Yongtao; Liebermann, Robert C.; Li, Baosheng; Kung, Jennifer; Yu, Tony; Wang, Yanbin

    2015-08-14

    In this study, we developed a new method for in-situ pressure determination in multi-anvil, high-pressure apparatus using an acoustic travel time approach within the framework of acoustoelasticity. The ultrasonic travel times of polycrystalline Al{sub 2}O{sub 3} were calibrated against NaCl pressure scale up to 15 GPa and 900 °C in a Kawai-type double-stage multi-anvil apparatus in conjunction with synchrotron X-radiation, thereby providing a convenient and reliable gauge for pressure determination at ambient and high temperatures. The pressures derived from this new travel time method are in excellent agreement with those from the fixed-point methods. Application of this new pressure gauge in an offline experiment revealed a remarkable agreement of the densities of coesite with those from the previous single crystal compression studies under hydrostatic conditions, thus providing strong validation for the current travel time pressure scale. The travel time approach not only can be used for continuous in-situ pressure determination at room temperature, high temperatures, during compression and decompression, but also bears a unique capability that none of the previous scales can deliver, i.e., simultaneous pressure and temperature determination with a high accuracy (±0.16 GPa in pressure and ±17 °C in temperature). Therefore, the new in-situ Al{sub 2}O{sub 3} pressure gauge is expected to enable new and expanded opportunities for offline laboratory studies of solid and liquid materials under high pressure and high temperature in multi-anvil apparatus.

  12. High Speed Method for in Situ Multispectral Image Registration

    SciTech Connect

    Perrine, Kenneth A.; Lamarche, Brian L.; Hopkins, Derek F.; Budge, Scott E.; Opresko, Lee; Wiley, H. S.; Sowa, Marianne B.

    2007-01-29

    Multispectral confocal spinning disk microscopy provides a high resolution method for real-time live cell imaging. However, optical distortions and the physical misalignments introduced by the use of multiple acquisition cameras can obscure spatial information contained in the captured images. In this manuscript, we describe a multispectral method for real-time image registration whereby the image from one camera is warped onto the image from a second camera via a polynomial correction. This method provides a real-time pixel-for-pixel match between images obtained over physically distinct optical paths. Using an in situ calibration method, the polynomial is characterized by a set of coefficients using a least squares solver. Error analysis demonstrates optimal performance results from the use of cubic polynomials. High-speed evaluation of the warp is then performed through forward differencing with fixed-point data types. Image reconstruction errors are reduced through bilinear interpolation. The registration techniques described here allow for successful registration of multispectral images in real-time (exceeding 15 frame/sec) and have a broad applicability to imaging methods requiring pixel matching over multiple data channels.

  13. Structure determination of an integral membrane protein at room temperature from crystals in situ.

    PubMed

    Axford, Danny; Foadi, James; Hu, Nien Jen; Choudhury, Hassanul Ghani; Iwata, So; Beis, Konstantinos; Evans, Gwyndaf; Alguel, Yilmaz

    2015-06-01

    The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samples and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines.

  14. Structure determination of an integral membrane protein at room temperature from crystals in situ

    PubMed Central

    Axford, Danny; Foadi, James; Hu, Nien-Jen; Choudhury, Hassanul Ghani; Iwata, So; Beis, Konstantinos; Evans, Gwyndaf; Alguel, Yilmaz

    2015-01-01

    The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samples and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines. PMID:26057664

  15. Loading rate and test temperature effects on fracture of In Situ niobium silicide-niobium composites

    NASA Astrophysics Data System (ADS)

    Rigney, Joseph D.; Lewandowski, John J.

    1996-10-01

    Arc cast, extruded, and heat-treated in situ composites of niobium suicide (Nb5Si3) intermetallic with niobium phases (primary—Nbp and secondary—Nbs) exhibited high fracture resistance in comparison to monolithic Nb5Si3. In toughness tests conducted at 298 K and slow applied loading rates, the fracture process proceeded by the microcracking of the Nb5Si3 and plastic deformation of the Nbp and Nbs phases, producing resistance-curve behavior and toughnesses of 28 MPa√m with damage zone lengths less than 500 μm. The effects of changes in the Nbp yield strength and fracture behavior on the measured toughnesses were investigated by varying the loading rates during fracture tests at both 77 and 298 K. Quantitative fractography was utilized to completely characterize each fracture surface created at 298 K in order to determine the type of fracture mode ( i.e., dimpled, cleavage) exhibited by the Nbp. Specimens tested at either higher loading rates or lower test temperatures consistently exhibited a greater amount of cleavage fracture in the Nbp, while the Nbs, always remained ductile. However, the fracture toughness values determined from experiments spanning six orders of magnitude in loading rate at 298 and 77 K exhibited little variation, even under conditions when the majority of Nbp phases failed by cleavage at 77 K. The changes in fracture mode with increasing loading rate and/or decreasing test temperature and their effects on fracture toughness are rationalized by comparison to existing theoretical models.

  16. Structure determination of an integral membrane protein at room temperature from crystals in situ

    SciTech Connect

    Axford, Danny; Foadi, James; Hu, Nien-Jen; Choudhury, Hassanul Ghani; Iwata, So; Beis, Konstantinos; Evans, Gwyndaf; Alguel, Yilmaz

    2015-05-14

    The X-ray structure determination of an integral membrane protein using synchrotron diffraction data measured in situ at room temperature is demonstrated. The structure determination of an integral membrane protein using synchrotron X-ray diffraction data collected at room temperature directly in vapour-diffusion crystallization plates (in situ) is demonstrated. Exposing the crystals in situ eliminates manual sample handling and, since it is performed at room temperature, removes the complication of cryoprotection and potential structural anomalies induced by sample cryocooling. Essential to the method is the ability to limit radiation damage by recording a small amount of data per sample from many samples and subsequently assembling the resulting data sets using specialized software. The validity of this procedure is established by the structure determination of Haemophilus influenza TehA at 2.3 Å resolution. The method presented offers an effective protocol for the fast and efficient determination of membrane-protein structures at room temperature using third-generation synchrotron beamlines.

  17. In-situ temperature calibration procedure for temperature and strain fibre Bragg grating sensors for monitoring pre-stressing strands

    NASA Astrophysics Data System (ADS)

    Mckeeman, I.; Fusiek, G.; Perry, M.; Niewczas, P.; Johnston, M.

    2015-09-01

    In this work, we demonstrate active and passive methods for in-situ temperature calibration of fibre Bragg grating strain and temperature sensors. The method is suitable for characterising sensors which are already attached to the steel reinforcements of civil structures. The proposed method, which involves the use of active induction heating or passive room temperature fluctuations, can be implemented using portable equipment, is time efficient, and can be used to calibrate attached sensors on-site, rather than in lab conditions. Preliminary results of the induction heating calibration show good agreement with pre-calibrated temperature sensors. In-situ calibration of fibre strain sensors, attached to a prestressing strand is also successfully carried out.

  18. Ice surface temperatures: seasonal cycle and daily variability from in-situ and satellite observations

    NASA Astrophysics Data System (ADS)

    Madsen, Kristine S.; Dybkjær, Gorm; Høyer, Jacob L.; Nielsen-Englyst, Pia; Rasmussen, Till A. S.; Tonboe, Rasmus T.

    2016-04-01

    Surface temperature is an important parameter for understanding the climate system, including the Polar Regions. Yet, in-situ temperature measurements over ice- and snow covered regions are sparse and unevenly distributed, and atmospheric circulation models estimating surface temperature may have large biases. To change this picture, we will analyse the seasonal cycle and daily variability of in-situ and satellite observations, and give an example of how to utilize the data in a sea ice model. We have compiled a data set of in-situ surface and 2 m air temperature observations over land ice, snow, sea ice, and from the marginal ice zone. 2523 time series of varying length from 14 data providers, with a total of more than 13 million observations, have been quality controlled and gathered in a uniform format. An overview of this data set will be presented. In addition, IST satellite observations have been processed from the Metop/AVHRR sensor and a merged analysis product has been constructed based upon the Metop/AVHRR, IASI and Modis IST observations. The satellite and in-situ observations of IST are analysed in parallel, to characterize the IST variability on diurnal and seasonal scales and its spatial patterns. The in-situ data are used to estimate sampling effects within the satellite observations and the good coverage of the satellite observations are used to complete the geographical variability. As an example of the application of satellite IST data, results will be shown from a coupled HYCOM-CICE ocean and sea ice model run, where the IST products have been ingested. The impact of using IST in models will be assessed. This work is a part of the EUSTACE project under Horizon 2020, where the ice surface temperatures form an important piece of the puzzle of creating an observationally based record of surface temperatures for all corners of the Earth, and of the ESA GlobTemperature project which aims at applying surface temperatures in models in order to

  19. Short communication on "In-situ TEM ion irradiation investigations on U3Si2 at LWR temperatures"

    DOE PAGES

    Miao, Yinbin; Harp, Jason; Mo, Kun; ...

    2016-11-21

    Here, 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  1. Ultrahigh vacuum holder-positioner for in situ studies of conductive nanostructures in a wide temperature range

    NASA Astrophysics Data System (ADS)

    Shevtsov, D. V.; Lyaschenko, S. A.; Varnakov, S. N.

    2016-11-01

    A holder-positioner was developed in order to be used in high vacuum systems designed for synthesis and in situ samples investigation by optical methods in 77÷1171 K temperature range. During tests of holder- positioner the designed system demonstrated independence from other process chamber components, compactness, a large number of the sample degrees of freedom and the stability of maintaining temperatures in the range from 77 to 1171 K with a maximum sample cooling rate about 0.1 K/s.

  2. Comparison of MTI Satellite-Derived Surface Water Temperatures and In-Situ Measurements

    SciTech Connect

    Kurzeja, R.

    2001-07-26

    Temperatures of the water surface of a cold, mid-latitude lake and the tropical Pacific Ocean were determined from MTI images and from in situ concurrent measurements. In situ measurements were obtained at the time of the MTI image with a floating, anchored platform, which measured the surface and bulk water temperatures and relevant meteorological variables, and also from a boat moving across the target area. Atmospheric profiles were obtained from concurrent radiosonde soundings. Radiances at the satellite were calculated with the Modtran radiative transfer model. The MTI infrared radiances were within 1 percent of the calculated values at the Pacific Ocean site but were 1-2 percent different over the mid-latitude lake.

  3. In situ electrical resistance and activation energy of solid C60 under high pressure

    NASA Astrophysics Data System (ADS)

    Yang, Jie; Liu, Cai-Long; Gao, Chun-Xiao

    2013-09-01

    The in situ electrical resistance and transport activation energies of solid C60 fullerene have been measured under high pressure up to 25 GPa in the temperature range of 300-423 K by using a designed diamond anvil cell. In the experiment, four parts of boron-doped diamond films fabricated on one anvil were used as electrical measurement probes and a W—Ta thin film thermocouple which was integrated on the other diamond anvil was used to measure the temperature. The current results indicate that the measured high-pressure resistances are bigger than those reported before at the same pressure and there is no pressure-independent resistance increase before 8 GPa. From the temperature dependence of the resistivity, the C60 behaviors as a semiconductor and the activation energies of the cubic C60 fullerene are 0.49, 0.43, and 0.36 eV at 13, 15, and 19 GPa, respectively.

  4. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    NASA Astrophysics Data System (ADS)

    Chakraborty, R.; Serdy, J.; West, B.; Stuckelberger, M.; Lai, B.; Maser, J.; Bertoni, M. I.; Culpepper, M. L.; Buonassisi, T.

    2015-11-01

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H2Se and H2S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuInxGa1-xSe2 (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25-400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  5. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy

    SciTech Connect

    Chakraborty, R. E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T. E-mail: buonassisi@mit.edu; West, B.; Stuckelberger, M.; Bertoni, M. I.; Lai, B.; Maser, J.

    2015-11-15

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H{sub 2}Se and H{sub 2}S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn{sub x}Ga{sub 1−x}Se{sub 2} (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25–400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  6. Development of an in situ temperature stage for synchrotron X-ray spectromicroscopy.

    PubMed

    Chakraborty, R; Serdy, J; West, B; Stuckelberger, M; Lai, B; Maser, J; Bertoni, M I; Culpepper, M L; Buonassisi, T

    2015-11-01

    In situ characterization of micro- and nanoscale defects in polycrystalline thin-film materials is required to elucidate the physics governing defect formation and evolution during photovoltaic device fabrication and operation. X-ray fluorescence spectromicroscopy is particularly well-suited to study defects in compound semiconductors, as it has a large information depth appropriate to study thick and complex materials, is sensitive to trace amounts of atomic species, and provides quantitative elemental information, non-destructively. Current in situ methods using this technique typically require extensive sample preparation. In this work, we design and build an in situ temperature stage to study defect kinetics in thin-film solar cells under actual processing conditions, requiring minimal sample preparation. Careful selection of construction materials also enables controlled non-oxidizing atmospheres inside the sample chamber such as H2Se and H2S. Temperature ramp rates of up to 300 °C/min are achieved, with a maximum sample temperature of 600 °C. As a case study, we use the stage for synchrotron X-ray fluorescence spectromicroscopy of CuIn(x)Ga(1-x)Se2 (CIGS) thin-films and demonstrate predictable sample thermal drift for temperatures 25-400 °C, allowing features on the order of the resolution of the measurement technique (125 nm) to be tracked while heating. The stage enables previously unattainable in situ studies of nanoscale defect kinetics under industrially relevant processing conditions, allowing a deeper understanding of the relationship between material processing parameters, materials properties, and device performance.

  7. In situ-forming hydrogels--review of temperature-sensitive systems.

    PubMed

    Ruel-Gariépy, Eve; Leroux, Jean-Christophe

    2004-09-01

    In the past few years, an increasing number of in situ-forming systems have been reported in the literature for various biomedical applications, including drug delivery, cell encapsulation, and tissue repair. There are several possible mechanisms that lead to in situ gel formation: solvent exchange, UV-irradiation, ionic cross-linkage, pH change, and temperature modulation. The thermosensitive approach can be advantageous for particular applications as it does not require organic solvents, co-polymerization agents, or an externally applied trigger for gelation. In the last 2 decades, several thermosensitive formulations have been proposed. This manuscript focuses on aqueous polymeric solutions that form implants in situ in response to temperature change, generally from ambient to body temperature. It mainly reviews the characterization and use of polysaccharides, N-isopropylacrylamide copolymers, poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) (poloxamer) and its copolymers, poly(ethylene oxide)/(D,L-lactic acid-co-glycolic acid) copolymers, and thermosensitive liposome-based systems.

  8. In-situ calibration and certification of high dc voltage

    SciTech Connect

    Wickoff, B.

    1982-01-01

    A technical calibration service developed by an electrical standards laboratory to support a production facility in the calibration and certification of electron beam welder is described. The in-situ certification process utilizing standards traceable to NBS, documented procedures, applicable error analyses, and certified tolerances assigned to the calibration results are discussed.

  9. Temperature calibration of lacustrine alkenones using in-situ sampling and growth cultures

    NASA Astrophysics Data System (ADS)

    Huang, Y.; Toney, J. L.; Andersen, R.; Fritz, S. C.; Baker, P. A.; Grimm, E. C.; Theroux, S.; Amaral Zettler, L.; Nyren, P. E.

    2010-12-01

    Sedimentary alkenones have been found in an increasing number of lakes around the globe. Studies using molecular biological tools, however, indicate that haptophyte species that produce lacustrine alkenones differ from the oceanic species. In order to convert alkenone unsaturation ratios measured in sediments into temperature, it is necessary to obtain an accurate calibration for individual lakes. Using Lake George, North Dakota, U.S. as an example, we have carried out temperature calibrations by both in-situ water column sampling and culture growth experiments. In-situ measured lake water temperatures in the lake show a strong correlation with the alkenone unsaturation indices (r-squared = 0.82), indicating a rapid equilibrium of alkenone distributions with the lake water temperature in the water column. We applied the in-situ calibration to down-core measurements for Lake George and generated realistic temperature estimates for the past 8 kyr. Algal isolation and culture growth, on the other hand, reveal the presence of two different types of alkenone producing haptophytes. The species making a predominant C37:4 alkenone (species A) produced much greater concentrations of alkenones per unit volume than the species that produced a predominant C37:3 alkenone (species B). It is the first time that a haptophyte species (species A) making a predominant C37:4 alkenone is cultured successfully and now replicated at four different growth temperatures. The distribution of alkeones in Lake George sediments matches extremely well with the alkenones produced by species A, indicating species A is likely the producer for the alkenones in the sediments. The alkenone unsaturation ratio of alkenones produced by species A haptophyte shows a primary dependence on growth temperature as expected, but the slope of change appears to vary depending on the growth stages. The implications of our findings for paleoclimate reconstructions using lacustrine alkenones will be discussed.

  10. High temperature superconducting compounds

    NASA Astrophysics Data System (ADS)

    Goldman, Allen M.

    1992-11-01

    The major accomplishment of this grant has been to develop techniques for the in situ preparation of high-Tc superconducting films involving the use of ozone-assisted molecular beam epitaxy. The techniques are generalizable to the growth of trilayer and multilayer structures. Films of both the DyBa2Cu3O(7-x) and YBa2Cu3O(7-x) compounds as well as the La(2-x)Sr(x)CuO4 compound have been grown on the usual substrates, SrTiO3, YSZ, MgO, and LaAlO3, as well as on Si substrates without any buffer layer. A bolometer has been fabricated on a thermally isolated SiN substrate coated with YSZ, an effort carried out in collaboration with Honeywell Inc. The deposition process facilitates the fabrication of very thin and transparent films creating new opportunities for the study of superconductor-insulator transitions and the investigation of photo-doping with carriers of high temperature superconductors. In addition to a thin film technology, a patterning technology has been developed. Trilayer structures have been developed for FET devices and tunneling junctions. Other work includes the measurement of the magnetic properties of bulk single crystal high temperature superconductors, and in collaboration with Argonne National Laboratory, measurement of electric transport properties of T1-based high-Tc films.

  11. In Situ Determination of BCC-, FCC- and HPC-Iron Textures at Simultaneous High- Pressure and -Temperature by Means of the Resistive Heated Radial Diffraction Diamond Anvil Cell (RH-RD-DAC): Implications for the iron core.

    NASA Astrophysics Data System (ADS)

    Liermann, H.; Merkel, S.; Miyagi, L.; Wenk, H.; Shen, G.; Cynn, H.; Evans, W. J.

    2008-12-01

    Radial diffraction in the diamond anvil cell (DAC) has long been used to determine the stress state of materials under non-hydrostatic compression. This technique is also a major tool to investigate textures and infer deformation mechanisms in the earth mantle and core. However, most of these experiments have been conducted at ambient temperatures and therefore the results of these measurements may be difficult to extrapolate to the deep Earth. Here, we present texture data collected at HPCAT sector 16 BMD of the Advanced Photon Source during the plastic deformation of BCC-, FCC- and HPC-iron at simultaneous high-pressure and temperature in the new Resistive Heated Radial Diffraction Diamond Anvil Cell (RH-RD-DAC). Initial results from Rietveld refinements in MAUD indicate that BCC- iron develops a mixed {100} and {111} texture that remains active during heating. Latter is compatible with previous observations on BCC-iron and interpreted as slip along {110}<111>. Texture obtained after formation of FCC-iron at simultaneous high- pressure and temperatures show a pronounced maximum at {110} with minima at {100} and {111}. This texture is typical for FCC metals in compression with slip on {111}<110>. Processing of the HCP-iron textures at high-pressure and -temperature are under way. We will discuss the implications that the experimental results have for the deformation mechanisms of iron at pressure temperature conditions of the inner core.

  12. Low-temperature plasticity of olivine revisited with in situ TEM nanomechanical testing

    PubMed Central

    Idrissi, Hosni; Bollinger, Caroline; Boioli, Francesca; Schryvers, Dominique; Cordier, Patrick

    2016-01-01

    The rheology of the lithospheric mantle is fundamental to understanding how mantle convection couples with plate tectonics. However, olivine rheology at lithospheric conditions is still poorly understood because experiments are difficult in this temperature range where rocks and mineral become very brittle. We combine techniques of quantitative in situ tensile testing in a transmission electron microscope and numerical modeling of dislocation dynamics to constrain the low-temperature rheology of olivine. We find that the intrinsic ductility of olivine at low temperature is significantly lower than previously reported values, which were obtained under strain-hardened conditions. Using this method, we can anchor rheological laws determined at higher temperature and can provide a better constraint on intermediate temperatures relevant for the lithosphere. More generally, we demonstrate the possibility of characterizing the mechanical properties of specimens, which can be available in the form of submillimeter-sized particles only. PMID:26998522

  13. Low-temperature plasticity of olivine revisited with in situ TEM nanomechanical testing.

    PubMed

    Idrissi, Hosni; Bollinger, Caroline; Boioli, Francesca; Schryvers, Dominique; Cordier, Patrick

    2016-03-01

    The rheology of the lithospheric mantle is fundamental to understanding how mantle convection couples with plate tectonics. However, olivine rheology at lithospheric conditions is still poorly understood because experiments are difficult in this temperature range where rocks and mineral become very brittle. We combine techniques of quantitative in situ tensile testing in a transmission electron microscope and numerical modeling of dislocation dynamics to constrain the low-temperature rheology of olivine. We find that the intrinsic ductility of olivine at low temperature is significantly lower than previously reported values, which were obtained under strain-hardened conditions. Using this method, we can anchor rheological laws determined at higher temperature and can provide a better constraint on intermediate temperatures relevant for the lithosphere. More generally, we demonstrate the possibility of characterizing the mechanical properties of specimens, which can be available in the form of submillimeter-sized particles only.

  14. In Situ Elevated Temperature Testing of Fly Ash Based Geopolymer Composites

    PubMed Central

    Vickers, Les; Pan, Zhu; Tao, Zhong; van Riessen, Arie

    2016-01-01

    In situ elevated temperature investigations using fly ash based geopolymers filled with alumina aggregate were undertaken. Compressive strength and short term creep tests were carried out to determine the onset temperature of viscous flow. Fire testing using the standard cellulose curve was performed. Applying a load to the specimen as the temperature increased reduced the temperature at which viscous flow occurred (compared to test methods with no applied stress). Compressive strength increased at the elevated temperature and is attributed to viscous flow and sintering forming a more compact microstructure. The addition of alumina aggregate and reduction of water content reduced the thermal conductivity. This led to the earlier onset and shorter dehydration plateau duration times. However, crack formation was reduced and is attributed to smaller thermal gradients across the fire test specimen. PMID:28773568

  15. Fractured rock stress-permeability relationships from in situ data and effects of temperature and chemical-mechanical couplings

    DOE PAGES

    Rutqvist, J.

    2014-09-19

    The purpose of this paper is to (i) review field data on stress-induced permeability changes in fractured rock; (ii) describe estimation of fractured rock stress-permeability relationships through model calibration against such field data; and (iii) discuss observations of temperature and chemically mediated fracture closure and its effect on fractured rock permeability. The field data that are reviewed include in situ block experiments, excavation-induced changes in permeability around tunnels, borehole injection experiments, depth (and stress) dependent permeability, and permeability changes associated with a large-scale rock-mass heating experiment. Data show how the stress-permeability relationship of fractured rock very much depends on localmore » in situ conditions, such as fracture shear offset and fracture infilling by mineral precipitation. Field and laboratory experiments involving temperature have shown significant temperature-driven fracture closure even under constant stress. Such temperature-driven fracture closure has been described as thermal overclosure and relates to better fitting of opposing fracture surfaces at high temperatures, or is attributed to chemically mediated fracture closure related to pressure solution (and compaction) of stressed fracture surface asperities. Back-calculated stress-permeability relationships from field data may implicitly account for such effects, but the relative contribution of purely thermal-mechanical and chemically mediated changes is difficult to isolate. Therefore, it is concluded that further laboratory and in situ experiments are needed to increase the knowledge of the true mechanisms behind thermally driven fracture closure, and to further assess the importance of chemical-mechanical coupling for the long-term evolution of fractured rock permeability.« less

  16. High-resistive layers obtained through periodic growth and in situ annealing of InGaN by metalorganic chemical vapor deposition

    SciTech Connect

    Zhang, Shuo; Ma, Ping Liu, Boting; Wu, Dongxue; Li, Jinmin; Huang, Yuliang; Wang, Junxi

    2016-06-15

    High-resistive layers were obtained by periodic growth and in situ annealing of InGaN. The effect of the annealing temperature of InGaN on the indium content and the material sheet resistive was investigated. The indium content decreased as the increase of in situ annealing temperature. Additionally, the material sheet resistance increased with the increase of the in situ annealing temperature for the annealed samples and reached 2 × 10{sup 10}Ω/sq in the light and 2 × 10{sup 11}Ω/sq in the dark when the in situ annealing temperature reached 970{sup ∘}C. The acquirement of high-resistive layers is attributed to the generation of indium vacancy-related defects. Introducing indium vacancy-related defects to compensate background carriers can be an effective method to grow high-resistance material.

  17. Rapid thermal processing of high-efficiency silicon solar cells with controlled in-situ annealing

    SciTech Connect

    Doshi, P.; Rohatgi, A.; Ropp, M.; Chen, Z.; Ruby, D.; Meier, D.L.

    1995-01-01

    Silicon solar cell efficiencies of 17.1%, 16.4%, 14.8%, and 14.9% have been achieved on FZ, Cz, multicrystalline (mc-Si), and dendritic web (DW) silicon, respectively, using simplified, cost-effective rapid thermal processing (RTP). These represent the highest reported efficiencies for solar cells processed with simultaneous front and back diffusion with no conventional high-temperature furnace steps. Appropriate diffusion temperature coupled with the added in-situ anneal resulted in suitable minority-carrier lifetime and diffusion profiles for high-efficiency cells. The cooling rate associated with the in-situ anneal can improve the lifetime and lower the reverse saturation current density (J{sub 0}), however, this effect is material and base resistivity specific. PECVD antireflection (AR) coatings provided low reflectance and efficient front surface and bulk defect passivation. Conventional cells fabricated on FZ silicon by furnace diffusions and oxidations gave an efficiency of 18.8% due to greater short wavelength response and lower J{sub 0}.

  18. In-situ Stress Measurement of MOVPE Growth of High Efficiency Lattice-Mismatched Solar Cells

    SciTech Connect

    Geisz, J. F.; Levander, A. X.; Norman, A. G.; Jones, K. M.; Romero, M. J.

    2007-04-01

    We have recently reported high efficiencies in a monolithic III-V triple-junction solar cell design that is grown inverted with a metamorphic 1.0 eV bottom In{sub .27}Ga{sub .73}As junction. The biaxial stress and strain grown into this highly lattice-mismatched junction can be controlled by varying the design of a step-graded Ga{sub x}In{sub 1-x}P buffer layer, in which most, but not all, of the 1.9% misfit strain is relieved. A multi-beam optical stress sensor (MOSS) is a convenient tool for in situ measurement of stress during metal-organic vapor phase epitaxy (MOVPE) for the optimization of solar cell performance. The analysis of stress from curvature data is complicated by significant temperature effects due to relatively small thermal gradients in our atmospheric-pressure MOVPE reactor. These temperature effects are discussed and approximations made to allow practical analysis of the data. The results show excellent performance of inverted In{sub .27}Ga{sub .73}. As solar cells grown with slight compressive stress, but degradation under tensile stress. The best devices had a V{sub oc} of 0.54 V and a dislocation density in the low 10{sup 6} cm{sup -2}. The in situ stress data is also compared with ex situ strain data derived from X-ray diffraction measurements.

  19. Seasonal variation in phosphorus concentration-discharge hysteresis inferred from high-frequency in situ monitoring

    NASA Astrophysics Data System (ADS)

    Bieroza, M. Z.; Heathwaite, A. L.

    2015-05-01

    High-resolution in situ total phosphorus (TP), total reactive phosphorus (TRP) and turbidity (TURB) time series are presented for a groundwater-dominated agricultural catchment. Meta-analysis of concentration-discharge (c-q) intra-storm signatures for 61 storm events revealed dominant hysteretic patterns with similar frequency of anti-clockwise and clockwise responses; different determinands (TP, TRP, TURB) behaved similarly. We found that the c-q loop direction is controlled by seasonally variable flow discharge and temperature whereas the magnitude is controlled by antecedent rainfall. Anti-clockwise storm events showed lower flow discharge and higher temperature compared to clockwise events. Hydrological controls were more important for clockwise events and TP and TURB responses, whereas in-stream biogeochemical controls were important for anti-clockwise storm events and TRP responses. Based on the best predictors of the direction of the hysteresis loops, we calibrated and validated a simple fuzzy logic inference model (FIS) to determine likely direction of the c-q responses. We show that seasonal and inter-storm succession in clockwise and anti-clockwise responses corroborates the transition in P transport from a chemostatic to an episodic regime. Our work delivers new insights for the evidence base on the complexity of phosphorus dynamics. We show the critical value of high-frequency in situ observations in advancing understanding of freshwater biogeochemical processes.

  20. High voltage-power frequency electrical heating in-situ conversion technology of oil shale

    NASA Astrophysics Data System (ADS)

    Sun, Youhong; Yang, Yang; Lopatin, Vladimir; Guo, Wei; Liu, Baochang; Yu, Ping; Gao, Ke; Ma, Yinlong

    2014-05-01

    With the depletion of conventional energy sources,oil shale has got much attention as a new type of energy resource,which is rich and widespread in the world.The conventional utilization of oil shale is mainly focused on resorting to produce shale oil and fuel gas with low extraction efficiency about one in a million due to many shortcomings and limitations.And the in-situ conversion of oil shale,more environmentally friendly,is still in the experimental stage.High voltage-power frequency electrical heating in-situ conversion of oil shale is a new type of in-situ pyrolysis technology.The main equipment includes a high voltage-power frequency generator and interior reactor. The high voltage-power frequency generator can provide a voltage between 220-8000 V which can be adjusted in real time according to the actual situation.Firstly,high voltage is used to breakdown the oil shale to form a dendritic crack between two electrodes providing a conductive channel inside the oil shale rock.And then the power frequency(220V) is used to generate the electric current for heating the internal surface of conductive channel,so that the energy can be transmitted to the surrounding oil shale.When the temperature reaches 350 degree,the oil shale begins to pyrolysis.In addition,the temperature in the conductive channel can be extremely high with high voltage,which makes the internal surface of conductive channel graphitization and improves its heat conduction performance.This technology can successfully make the oil shale pyrolysis, based on a lot of lab experiments,and also produce the combustible shale oil and fuel gas.Compared to other in-situ conversion technology,this method has the following advantages: high speed of heating oil shale,the equipment underground is simple,and easy to operate;it can proceed without the limitation of shale thickness, and can be used especially in the thin oil shale reservoir;the heating channel is parallel to the oil shale layers,which has more

  1. Development of an Expanded, High Reliability Cost and Performance Database for In Situ Remediation Technologies

    DTIC Science & Technology

    2016-03-01

    ER-201120) Development of an Expanded, High- Reliability Cost and Performance Database for In-Situ...10 4.1 Overview of the Database ...Concentrations for Four Active In-Situ Remediation Technologies vs. MNA Table 5.1 OoM Reduction in Parent Compound at 235 Databases Sites vs. 3 “Remediation

  2. Temperature and layer thickness dependent in situ investigations on epindolidione organic thin-film transistors.

    PubMed

    Lassnig, R; Striedinger, B; Jones, A O F; Scherwitzl, B; Fian, A; Głowacl, E D; Stadlober, B; Winkler, A

    2016-08-01

    We report on in situ performance evaluations as a function of layer thickness and substrate temperature for bottom-gate, bottom-gold contact epindolidione organic thin-film transistors on various gate dielectrics. Experiments were carried out under ultra-high vacuum conditions, enabling quasi-simultaneous electrical and surface analysis. Auger electron spectroscopy and thermal desorption spectroscopy (TDS) were applied to characterize the quality of the substrate surface and the thermal stability of the organic films. Ex situ atomic force microscopy (AFM) was used to gain additional information on the layer formation and surface morphology of the hydrogen-bonded organic pigment. The examined gate dielectrics included SiO2, in its untreated and sputtered forms, as well as the spin-coated organic capping layers poly(vinyl-cinnamate) (PVCi) and poly((±)endo,exo-bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid, diphenylester) (PNDPE, from the class of polynorbornenes). TDS and AFM revealed Volmer-Weber island growth dominated film formation with no evidence of a subjacent wetting layer. This growth mode is responsible for the comparably high coverage required for transistor behavior at 90-95% of a monolayer composed of standing molecules. Surface sputtering and an increased sample temperature during epindolidione deposition augmented the surface diffusion of adsorbing molecules and therefore led to a lower number of better-ordered islands. Consequently, while the onset of charge transport was delayed, higher saturation mobility was obtained. The highest, bottom-contact configuration, mobilities of approximately 2.5 × 10(-3)cm(2)/Vs were found for high coverages (50 nm) on sputtered samples. The coverage dependence of the mobility showed very different characteristics for the different gate dielectrics, while the change of the threshold voltage with coverage was approximately the same for all systems. An apparent decrease of the mobility with increasing coverage on the

  3. Temperature and layer thickness dependent in situ investigations on epindolidione organic thin-film transistors

    PubMed Central

    Lassnig, R.; Striedinger, B.; Jones, A.O.F.; Scherwitzl, B.; Fian, A.; Głowacl, E.D.; Stadlober, B.; Winkler, A.

    2016-01-01

    We report on in situ performance evaluations as a function of layer thickness and substrate temperature for bottom-gate, bottom-gold contact epindolidione organic thin-film transistors on various gate dielectrics. Experiments were carried out under ultra-high vacuum conditions, enabling quasi-simultaneous electrical and surface analysis. Auger electron spectroscopy and thermal desorption spectroscopy (TDS) were applied to characterize the quality of the substrate surface and the thermal stability of the organic films. Ex situ atomic force microscopy (AFM) was used to gain additional information on the layer formation and surface morphology of the hydrogen-bonded organic pigment. The examined gate dielectrics included SiO2, in its untreated and sputtered forms, as well as the spin-coated organic capping layers poly(vinyl-cinnamate) (PVCi) and poly((±)endo,exo-bicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid, diphenylester) (PNDPE, from the class of polynorbornenes). TDS and AFM revealed Volmer-Weber island growth dominated film formation with no evidence of a subjacent wetting layer. This growth mode is responsible for the comparably high coverage required for transistor behavior at 90–95% of a monolayer composed of standing molecules. Surface sputtering and an increased sample temperature during epindolidione deposition augmented the surface diffusion of adsorbing molecules and therefore led to a lower number of better-ordered islands. Consequently, while the onset of charge transport was delayed, higher saturation mobility was obtained. The highest, bottom-contact configuration, mobilities of approximately 2.5 × 10−3cm2/Vs were found for high coverages (50 nm) on sputtered samples. The coverage dependence of the mobility showed very different characteristics for the different gate dielectrics, while the change of the threshold voltage with coverage was approximately the same for all systems. An apparent decrease of the mobility with increasing coverage on the

  4. Temperature-dependent conduction mechanism of vertically aligned graphene nanoflakes incorporated with nitrogen in situ

    NASA Astrophysics Data System (ADS)

    Kumar, Pawan

    2017-07-01

    Carbon nanostructured materials have been widely investigated and explored all over the world. However, the frontiers of applications and basic examinations related to these materials have yet to be opened in terms of their stability and robustness in the required environment. I report the temperature-dependent transport properties of vertically aligned graphene nanoflakes (GNFs) at room temperature to 800 K. Investigation of GNFs incorporated with nitrogen (N2) of varying concentration in situ and their possible conduction mechanism has been carried out over the entire range of temperatures mentioned above. N-type conductivity, carrier concentration, mobility and modulation at various temperatures are observed by means of Hall-effect measurements. The film of GNFs incorporated with nitrogen in situ persists in a linear trend, satisfying conduction behaviour expectations for all measured transport parameters with only a small discrete-point anomaly. Supporting evidence of N2 incorporation and structural modifications is studied by scanning electron microscopy, Raman spectroscopy and x-ray photoemission spectroscopy. The observation findings also provide the thermal stability of N2 incorporated into two-dimensional vertically standing GNFs.

  5. The first in situ electron temperature and density measurements of the Martian nightside ionosphere

    NASA Astrophysics Data System (ADS)

    Fowler, C. M.; Andersson, L.; Ergun, R. E.; Morooka, M.; Delory, G.; Andrews, D. J.; Lillis, Robert J.; McEnulty, T.; Weber, T. D.; Chamandy, T. M.; Eriksson, A. I.; Mitchell, D. L.; Mazelle, C.; Jakosky, B. M.

    2015-11-01

    The first in situ nightside electron density and temperature profiles at Mars are presented as functions of altitude and local time (LT) from the Langmuir Probe and Waves (LPW) instrument on board the Mars Atmosphere and Volatile EvolutioN (MAVEN) mission spacecraft. LPW is able to measure densities as low as ˜100 cm-3, a factor of up to 10 or greater improvement over previous measurements. Above 200 km, near-vertical density profiles of a few hundred cubic centimeters were observed for almost all nightside LT, with the lowest densities and highest temperatures observed postmidnight. Density peaks of a few thousand cubic centimeters were observed below 200 km at all nightside LT. The lowest temperatures were observed below 180 km and approach the neutral atmospheric temperature. One-dimensional modeling demonstrates that precipitating electrons were able to sustain the observed nightside ionospheric densities below 200 km.

  6. Simultaneous in-situ measurements of neutral temperature and oxygen in the mesosphere during the WADIS sounding rocket project

    NASA Astrophysics Data System (ADS)

    Strelnikov, Boris; Lübken, Franz-Josef; Rapp, Markus; Grygalashvyly, Mykhaylo; Löhle, Stefan; Eberhart, Martin; Fasoulas, Stefanos; Hedin, Jonas; Gumbel, Jörg; Khaplanov, Mikhail; Stegman, Jacek; Friedrich, Martin

    2016-04-01

    The WADIS project (Wave propagation and dissipation in the middle atmosphere: energy budget and distribution of trace constituents) aimed at studying waves, their dissipation, and effects on trace constituents. The project comprised two sounding rocket campaigns conducted at the Andøya Space Center (69 °N, 16 °E). One sounding rocket was launched in summer 2013 and one in winter 2015. In-situ measurements delivered high resolution altitude-profiles of neutral temperature and density, as well as plasma and oxygen densities. Atomic oxygen was measured by two different techniques. Airglow photometers operated by MISU measured emissions from excited molecular oxygen at 1.27 um (daytime summer launch) and 762 nm (night-time winter launch), both of which can be used to infer altitude profiles of atomic oxygen. This is a well-proven technique and has been applied to sounding rocket and satellite measurements in the past. Solid electrolyte sensors (FIPEX) operated by IRS is a new technique for sounding rockets, which yielded atomic oxygen density profiles with a height resolution better than 10 m. The neutral air density and temperature was measured by the CONE instrument also with very heigh altitude resolution and precision. All these instruments were mounted on the same deck of the sounding rocket and, therefore delivered real common volume measurements. In this paper we present simultaneous in-situ temperature and oxygen density measurements and discuss how variability of these quantities may influence temperature derivations from OH airglow observations at mesopause heights.

  7. Room-Temperature Large and Reversible Modulation of Photoluminescence by in Situ Electric Field in Ergodic Relaxor Ferroelectrics.

    PubMed

    Sun, Hailing; Wu, Xiao; Peng, Deng Feng; Kwok, K W

    2017-10-04

    Ferroelectric oxides with luminescent ions hold great promise in future optoelectronic devices because of their unique photoluminescence and inherent ferroelectric properties. Intriguingly, the photoluminescence performance of ferroelectric ceramics could be modulated by an external electric field. However, researchers face a current challenge of the diminutive extent and degree of reversibility of the field-driven modification that hinder their use in room-temperature practical applications. Within the scope of current contribution in rare-earth-doped bismuth sodium titanate relaxors, the most important information to be noted is the shifting of the depolarization temperature toward room temperature and the resulting considerable enhancement in ergodicity, as evidenced by the dielectric properties, polarization, and strain hysteresis, as well as the in situ Raman/X-ray diffraction studies. After the introduction of 1 mol % Eu, the induced composition and charge disorders disrupt the original long-range ferroelectric macrodomains into randomly dynamic and weakly correlated polar nanoregions, which facilitates a reversible transformation between polar nanoregions and unstable ferroelectric state under an electric field, engendering a large strain. By virtue of this, both the extent and degree of reversibility of photoluminescence modulation are enhanced (∼60%) considerably, and room-temperature in situ tunable photoluminescence response is then achieved under electric field. These should be helpful for the realization of regulating the physical couplings (photoluminescent-ferroelectrics) in multifunctional inorganic ferroelectrics with a high ergodic state by reversibly tuning the structural symmetry.

  8. High-pressure geomicrobial experimentation: narrowing the in situ-in vitro gap (Invited)

    NASA Astrophysics Data System (ADS)

    Thomas, B.; Rosenbauer, R. J.

    2010-12-01

    Geobiological investigations are biased toward observations and experimentation at the surface of the geosphere. However, the interactions between life and the geochemical components of the earth extend to great depth in sediments. Methodological and sampling difficulties obviously limit our ability to study these important deep processes at in situ temperature and pressure . These high-pressure conditions are particularly important for two reasons: 1) The free energy drive that sustains microbial communities in nature is strongly dependent upon entropy differences between the substrates and products, particularly when reactants and products are dissolved gases which can accumulate. 2) The physical properties and composition of fluids can differ dramatically at high pressures. For example, when CO2 exists in excess of its solubility and at a temperature > 31 Celsius it is considered a supercritical fluid. Above this temperature, and at elevated pressure (density), CO2 is an effective organic solvent. In short, the in situ chemical environment of deep organisms may not be reproducible with traditional in vitro methods. To explore hypotheses related to microbial activity at high pressure, we have adapted the flexible-gold reaction-cell technology used in hydrothermal experiments for the aseptic inoculation, growth, and sterilization of microbial cultures at pressures up to several hundred bars. These experimental facilities allow for serial sub-sampling of microbial culture fluids and the coexistence of separate CO2, hydrocarbon, and aqueous fluids. As a result of our experiments, we hypothesize that in nature, porewaters may reach a critical threshold whereby a separate CO2 rich fluid phase becomes an effective sterilizing barrier. This may help explain observations of the depth and temperature limit of microbial activity in sediments.

  9. Prokaryotic degradation of high molecular weight dissolved organic matter in the deep-sea waters of NW Mediterranean Sea under in situ temperature and pressure conditions during contrasted hydrological conditions

    NASA Astrophysics Data System (ADS)

    Tamburini, C.; Boutrif, M.; Garel, M.; Sempéré, R.; Repeta, D.; Charriere, B.; Nerini, D.; Panagiotopoulos, C.

    2016-02-01

    The contribution of the semi-labile dissolved organic carbon (DOC) to the global prokaryotic production has been assessed in very few previous studies. Some experiments show rapid utilization of semi-reactive DOC by prokaryotes, while other experiments show almost no utilization at all. However, all these studies did not take into account the role of hydrostatic pressure for the degradation of organic matter. In this study, we investigate (1) the degradation of "natural" high molecular weight DOM HMW-DOM (obtained after ultrafiltration) and (2) the uptake of labeled extracellular polymeric substances (3H-EPS) incubated with deep-sea water samples (2000 m-depth, NW Mediterranean Sea) under in situ pressure conditions (HP) and under atmospheric compression after decompression of the deep samples (ATM) during stratified and mixed water conditions (deep sea convection). Our results indicated that during HP incubations DOC exhibited the highest degradation rates (kHP DOC = 0.82 d-1) compared to the ATM conditions were no or few degradation was observed (kATM DOC= 0.007 d-1). An opposite trend was observed for the HP incubations from mixed deep water masses. HP incubation measurements displayed the lowest DOC degradation (kHP DOC=0.031 d-1) compared to the ATM conditions (kATM DOC=0.62 d-1). These results imply the presence of allochthonous prokaryotic cells in deep-sea samples after a winter water mass convection. Same trends were found using 3H-EPS uptake rates which were higher at HP than at ATM conditions during stratified period conditions whereas the opposite patterns were observed during deep-sea convection event. Moreover, we found than Euryarchaea were the main contributors to 3H-EPS assimilation at 2000m-depth, representing 58% of the total cells actively assimilating 3H-EPS. This study demonstrates that remineralization rates of semi-labile DOC in deep NW Med. Sea are controlled by the prokaryotic communities, which are influenced by the hydrological

  10. High pressure optical cell for synthesis and in situ Raman spectroscopy of hydrogen clathrate hydrates

    NASA Astrophysics Data System (ADS)

    Celli, Milva; Zoppi, Marco; Zaghloul, Mohamed A. S.; Ulivi, Lorenzo

    2012-11-01

    We report the design, realization, and test of a high-pressure optical cell that we have used to measure the Raman spectra of hydrogen clathrate hydrates, synthesized in situ by the application of 200-300 MPa of gas pressure on solid water. The optical apparatus is mounted on a cryogenic system so to allow measurements and sample treatment at any temperature between 300 and 20 K. A capillary pipe is connected to the inside of the cell to allow the gas flow into and out of the cell, and to regulate the internal pressure at any value from 0 to 300 MPa. In the experimental test described in this paper, the cell has been partly filled, at room temperature, with a small amount of water, then frozen at 263 K before injecting hydrogen gas, at pressure of 150 MPa, into the cell. This procedure has permitted to study hydrogen clathrate formation, by measuring Raman spectra as a function of time.

  11. Regulatory Pathway Analysis by High-Throughput In Situ Hybridization

    PubMed Central

    Visel, Axel; Carson, James; Oldekamp, Judit; Warnecke, Marei; Jakubcakova, Vladimira; Zhou, Xunlei; Shaw, Chad A; Alvarez-Bolado, Gonzalo; Eichele, Gregor

    2007-01-01

    Automated in situ hybridization enables the construction of comprehensive atlases of gene expression patterns in mammals. Such atlases can become Web-searchable digital expression maps of individual genes and thus offer an entryway to elucidate genetic interactions and signaling pathways. Towards this end, an atlas housing ∼1,000 spatial gene expression patterns of the midgestation mouse embryo was generated. Patterns were textually annotated using a controlled vocabulary comprising >90 anatomical features. Hierarchical clustering of annotations was carried out using distance scores calculated from the similarity between pairs of patterns across all anatomical structures. This process ordered hundreds of complex expression patterns into a matrix that reflects the embryonic architecture and the relatedness of patterns of expression. Clustering yielded 12 distinct groups of expression patterns. Because of the similarity of expression patterns within a group, members of each group may be components of regulatory cascades. We focused on the group containing Pax6, an evolutionary conserved transcriptional master mediator of development. Seventeen of the 82 genes in this group showed a change of expression in the developing neocortex of Pax6-deficient embryos. Electromobility shift assays were used to test for the presence of Pax6-paired domain binding sites. This led to the identification of 12 genes not previously known as potential targets of Pax6 regulation. These findings suggest that cluster analysis of annotated gene expression patterns obtained by automated in situ hybridization is a novel approach for identifying components of signaling cascades. PMID:17953485

  12. In situ stylus profilometer for a high frequency reciprocating tribometer

    NASA Astrophysics Data System (ADS)

    Kamps, T. J.; Walker, J. C.; Plint, A. G.

    2017-09-01

    Measuring the friction and wear characteristics of a tribological contact is essential to gaining a detailed understanding of its performance and predicted life. Wear rate and friction coefficient measurements are obtained from instrumented benchtop tribometers designed to replicate specific tribological contacts. Due to the difficulty of measuring wear in situ, measurements are typically made before and after an experiment. The wear rate must be assumed to be linear for it to be used to predict product life, however this is assumption can hide changes occurring during an experiment which indicate wear transitions. This paper details the design and validation of an in situ stylus profilometer for a reciprocating sliding tribometer to provide an insight into the wear transitions occurring during dry sliding of 52100 bearing steel against graphitic flake cast iron. The profilometer’s performance was validated using ground roughness standards and the accuracy found to be approximately 110 nm. Incubation, run-in and steady state wear regimes were identified by the profilometer and corroborated with friction coefficient data, providing an enhanced understanding of the tribological contact behaviour.

  13. Charge collection in Si detectors irradiated in situ at superfluid helium temperature

    NASA Astrophysics Data System (ADS)

    Verbitskaya, Elena; Eremin, Vladimir; Zabrodskii, Andrei; Dehning, Bernd; Kurfürst, Christoph; Sapinski, Mariusz; Bartosik, Marcin R.; Egorov, Nicolai; Härkönen, Jaakko

    2015-10-01

    Silicon and diamond detectors operated in a superfluid helium bath are currently being considered for the upgrade of the LHC beam loss monitoring system. The detectors would be installed in immediate proximity of the superconducting coils of the triplet magnets. We present here the results of the in situ irradiation test for silicon detectors using 23 GeV protons while keeping the detectors at a temperature of 1.9 K. Red laser (630 nm) Transient Current Technique and DC current measurements were used to study the pulse response and collected charge for silicon detectors irradiated to a maximum radiation fluence of 1×1016 p/cm2. The dependence between collected charge and irradiation fluence was parameterized using the Hecht equation and assumption of a uniform electric field distribution. The collected charge was found to degrade with particle fluence for both bias polarities. We observed that the main factor responsible for this degradation was related to trapping of holes on the donor-type radiation-induced defects. In contrast to expectations, along with formation of donors, acceptor-type defects (electron traps) are introduced into the silicon bulk. This suggests that the current models describing charge collection in irradiated silicon detectors require an extension for taking into account trapping at low temperatures with a contribution of shallow levels. New in situ irradiation tests are needed and planned now to extend statistics of the results and gain a deeper insight into the physics of low temperature detector operation in harsh radiation environment.

  14. Reconciling Spectroscopic Electron Temperature Measurements in the Solar Corona with In Situ Charge State Observations.

    PubMed

    Esser; Edgar

    2000-03-20

    It has been a puzzle for quite some time that spectroscopic measurements in the inner corona indicate electron temperatures far too low to produce the ion fractions observed in situ in the solar wind. In the present Letter, we show that in order to reconcile the two sets of measurements, a number of conditions have to exist in the inner corona: (1) The electron distribution function has to be Maxwellian or close to Maxwellian at the coronal base, (2) the non-Maxwellian character of the distribution has to develop rapidly as a function of height and has to reach close to interplanetary properties inside of a few solar radii, and (3) ions of different elements have to flow with significantly different speeds to separate their "freezing-in" distances sufficiently so that they can encounter different distribution functions. We choose two examples to demonstrate that these conditions are general requirements if both coronal electron temperatures and in situ ion fractions are correct. However, these two examples also show that the details of the required distribution functions are very sensitive to the exact electron temperature, density, and ion flow speed profiles in the region of the corona where the ions predominantly form.

  15. Kinetics of Methane Hydrate Decomposition Studied via in Situ Low Temperature X-ray Powder Diffraction

    SciTech Connect

    Everett, Susan M; Rawn, Claudia J; Keffer, David J.; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy Joe

    2013-01-01

    Gas hydrates are known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice termed self-preservation or anomalous preservation. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Two regions of slowed decomposition for methane hydrate, 180 200 K and 230 260 K, were observed, and the kinetics were studied by in situ low temperature x-ray powder diffraction. The kinetic constants for ice formation from methane hydrate were determined by the Avrami model within each region and activation energies, Ea, were determined by the Arrhenius plot. Ea determined from the data for 180 200 K was 42 kJ/mol and for 230 260 K was 22 kJ/mol. The higher Ea in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  16. Mars dayside temperature from airglow limb profiles : comparison with in situ measurements and models

    NASA Astrophysics Data System (ADS)

    Gérard, Jean-Claude; Bougher, Stephen; Montmessin, Franck; Bertaux, Jean-Loup; Stiepen, A.

    The thermal structure of the Mars upper atmosphere is the result of the thermal balance between heating by EUV solar radiation, infrared heating and cooling, conduction and dynamic influences such as gravity waves, planetary waves, and tides. It has been derived from observations performed from different spacecraft. These include in situ measurements of orbital drag whose strength depends on the local gas density. Atmospheric temperatures were determined from the altitude variation of the density measured in situ by the Viking landers and orbital drag measurements. Another method is based on remote sensing measurements of ultraviolet airglow limb profiles obtained over 40 years ago with spectrometers during the Mariner 6 and 7 flybys and from the Mariner 9 orbiter. Comparisons with model calculations indicate that they both reflect the CO_2 scale height from which atmospheric temperatures have been deduced. Upper atmospheric temperatures varying over the wide range 270-445 K, with a mean value of 325 K were deduced from the topside scale height of the airglow vertical profile. We present an analysis of limb profiles of the CO Cameron (a(3) Pi-X(1) Sigma(+) ) and CO_2(+) doublet (B(2) Sigma_u(+) - X(2) PiΠ_g) airglows observed with the SPICAM instrument on board Mars Express. We show that the temperature in the Mars thermosphere is very variable with a mean value of 270 K, but values ranging between 150 and 400 K have been observed. These values are compared to earlier determinations and model predictions. No clear dependence on solar zenith angle, latitude or season is apparent. Similarly, exospheric variations with F10.7 in the SPICAM airglow dataset are small over the solar minimum to moderate conditions sampled by Mars Express since 2005. We conclude that an unidentified process is the cause of the large observed temperature variability, which dominates the other sources of temperature variations.

  17. Understanding Depth Variation of Deep Seismicity from in situ Measurements of Mineral Strengths at High Pressures

    SciTech Connect

    Chen, J.

    2010-01-01

    Strengths of major minerals of Earth's mantle have been measured using in situ synchrotron X-ray diffraction at high pressures. Analysis of the diffraction peak widths is used to derive the yield strengths. Systematic analysis of the experimental result for olivine, wadsleyite, ringwoodite and perovskite indicates that minerals in the upper mantle, the transition zone and the lower mantle have very distinct strength character. Increasing temperature weakens the upper mantle mineral, olivine, significantly. At high temperature and high pressure, the transition zone minerals, wadsleyite and ringwoodite, have higher strengths than the upper mantle mineral. Among all the minerals studied, the lower mantle mineral, perovskite, has the highest strength. While both the upper mantle and the transition zone minerals show a notable strength drop, the strength of the lower mantle mineral shows just an increase of relaxation rate (no strength drop) when the temperature is increased stepwise by 200 K. The strength characteristics of these major mantle minerals at high pressures and temperatures indicate that yield strength may play a crucial role in defining the profile of deep earthquake occurrence with depth.

  18. Final Report on Developing Microstructure-Property Correlation in Reactor Materials using in situ High-Energy X-rays

    SciTech Connect

    Li, Meimei; Almer, Jonathan D.; Yang, Yong; Tan, Lizhen

    2016-01-01

    This report provides a summary of research activities on understanding microstructure – property correlation in reactor materials using in situ high-energy X-rays. The report is a Level 2 deliverable in FY16 (M2CA-13-IL-AN_-0403-0111), under the Work Package CA-13-IL-AN_- 0403-01, “Microstructure-Property Correlation in Reactor Materials using in situ High Energy Xrays”, as part of the DOE-NE NEET Program. The objective of this project is to demonstrate the application of in situ high energy X-ray measurements of nuclear reactor materials under thermal-mechanical loading, to understand their microstructure-property relationships. The gained knowledge is expected to enable accurate predictions of mechanical performance of these materials subjected to extreme environments, and to further facilitate development of advanced reactor materials. The report provides detailed description of the in situ X-ray Radiated Materials (iRadMat) apparatus designed to interface with a servo-hydraulic load frame at beamline 1-ID at the Advanced Photon Source. This new capability allows in situ studies of radioactive specimens subject to thermal-mechanical loading using a suite of high-energy X-ray scattering and imaging techniques. We conducted several case studies using the iRadMat to obtain a better understanding of deformation and fracture mechanisms of irradiated materials. In situ X-ray measurements on neutron-irradiated pure metal and model alloy and several representative reactor materials, e.g. pure Fe, Fe-9Cr model alloy, 316 SS, HT-UPS, and duplex cast austenitic stainless steels (CASS) CF-8 were performed under tensile loading at temperatures of 20-400°C in vacuum. A combination of wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and imaging techniques were utilized to interrogate microstructure at different length scales in real time while the specimen was subject to thermal-mechanical loading. In addition, in situ X-ray studies were

  19. Transmission electron microscopy study in-situ of radiation-induced defects in copper at elevated temperatures

    SciTech Connect

    Daulton, T.L.; Kirk, M.A.; Rehn, L.E.

    1996-12-01

    Neutrons and high-energy ions incident upon a solid can initiate a displacement collision cascade of lattice atoms resulting in localized regions within the solid containing a high concentration of interstitial and vacancy point defects. These point defects can collapse into various types of dislocation loops and stacking fault tetrahedra (SFT) large enough that their lattice strain fields are visible under diffraction-contrast imaging using a Transmission Electron Microscope (TEM). The basic mechanisms driving the collapse of point defects produced in collision cascades is investigated in situ with TEM for fcc-Cu irradiated with heavy (100 keV Kr) ions at elevated temperature. The isothermal stability of these clusters is also examined in situ. Areal defect yields were observed to decrease abruptly for temperatures greater than 300 C. This decrease in defect yield is attributed to a proportional decrease in the probability of collapse of point defects into clusters. The evolution of the defect density under isothermal conditions appears to be influenced by three different rate processes active in the decline of the total defect density. These rate constants can be attributed to differences in the stability of various types of defect clusters and to different loss mechanisms. Based upon observed stabilities, estimations for the average binding enthalpies of vacancies to SFT are calculated for copper.

  20. Platinum-cobalt catalysts for the oxygen reduction reaction in high temperature proton exchange membrane fuel cells - Long term behavior under ex-situ and in-situ conditions

    NASA Astrophysics Data System (ADS)

    Schenk, Alexander; Grimmer, Christoph; Perchthaler, Markus; Weinberger, Stephan; Pichler, Birgit; Heinzl, Christoph; Scheu, Christina; Mautner, Franz-Andreas; Bitschnau, Brigitte; Hacker, Viktor

    2014-11-01

    Platinum cobalt catalysts (Pt-Co) have attracted much interest as cathode catalysts for proton exchange membrane fuel cells (PEMFCs) due to their high activity toward oxygen reduction reaction (ORR). Many of the reported catalysts show outstanding performance in ex-situ experiments. However, the laborious synthesis protocols of these Pt-Co catalysts disable an efficient and economic production of membrane electrode assemblies (MEAs). We present an economic, flexible and continuous Pt-M/C catalyst preparation method as part of a large scale membrane electrode assembly manufacturing. In comparison, the as-prepared Pt-Co/C based high temperature (HT)-PEM MEA showed an equal performance to a commercially available HT-PEM MEA during 600 h of operation under constant load, although the commercial one had a significantly higher Pt loading at the cathode.

  1. In situ soil moisture coupled with extreme temperatures: A study based on the Oklahoma Mesonet

    NASA Astrophysics Data System (ADS)

    Ford, Trent W.; Quiring, Steven M.

    2014-07-01

    The relationship between the observed (in situ) soil moisture and the percent hot days (%HD) in Oklahoma is examined using quantile regression. Consistent with results from previous modeling studies and observational studies using precipitation deficits as proxy, soil moisture is found to most strongly impact air temperature in the upper quantile of the %HD distribution. The utility of soil moisture for forecasting extreme heat events in Oklahoma is also assessed. Our results show that %HD can be predicted with reasonable skill using soil moisture anomalies from the previous month. These soil moisture-based forecasts of extreme temperature events can be used to support public health and water resource planning and mitigation activities in the Southern Great Plain region of the United States.

  2. Modeling in situ soil enzyme activity using continuous field soil moisture and temperature data

    NASA Astrophysics Data System (ADS)

    Steinweg, J. M.; Wallenstein, M. D.

    2010-12-01

    Moisture and temperature are key drivers of soil organic matter decomposition, but there is little consensus on how climate change will affect the degradation of specific soil compounds under field conditions. Soil enzyme activities are a useful metric of soil community microbial function because they are they are the direct agents of decomposition for specific substrates in soil. However, current standard enzyme assays are conducted under optimized conditions in the laboratory and do not accurately reflect in situ enzyme activity, where diffusion and substrate availability may limit reaction rates. The Arrhenius equation, k= A*e(-Ea/RT), can be used to predict enzyme activity (k), collision frequency (A) or activation energy (Ea), but is difficult to parameterize when activities are measured under artificial conditions without diffusion or substrate limitation. We developed a modifed equation to estimate collision frequency and activation energy based on soil moisture to model in-situ enzyme activites. Our model was parameterized using data we collected from the Boston Area Climate Experiment (BACE) in Massachusetts; a multi-factor climate change experiment that provides an opportunity to assess how changes in moisture availability and temperature may impact enzyme activity. Soils were collected from three precipitation treatments and four temperature treatments arranged in a full-factorial design at the BACE site in June 2008, August 2008, January 2009 and June 2009. Enzyme assays were performed at four temperatures (4, 15, 25 and 35°C) to calculate temperature sensitivity and activation energy over the different treatments and seasons. Enzymes activities were measured for six common enzymes involved in carbon (β-glucosidase, cellobiohydrolase, xylosidase), phosphorus (phosphatase) and nitrogen cycling (N-acetyl glucosaminidase, and leucine amino peptidase). Potential enzyme activity was not significantly affected by precipitation, warming or the interaction of

  3. Experimental system for in-situ measurement of temperature rise in animal tissue under exposure to acoustic radiation force impulse.

    PubMed

    Nitta, Naotaka; Ishiguro, Yasunao; Sasanuma, Hideki; Taniguchi, Nobuyuki; Akiyama, Iwaki

    2015-01-01

    Acoustic radiation force impulse (ARFI) has recently been used for tissue elasticity measurement and imaging. On the other hand, it is predicted that a rise in temperature occurs. In-situ measurement of temperature rise in animal experiments is important, yet measurement using thermocouples has some problems such as position mismatch of the temperature measuring junction of the thermocouple and the focal point of ultrasound. Therefore, an in-situ measurement system for solving the above problems was developed in this study. The developed system is composed mainly of an ultrasound irradiation unit including a custom-made focused transducer with a through hole for inserting a thin-wire thermocouple, and a temperature measurement unit including the thermocouple. The feasibility of the developed system was evaluated by means of experiments using a tissue-mimicking material (TMM), a TMM containing a bone model or a chicken bone, and an extracted porcine liver. The similarity between the experimental results and the results of simulation using a finite element method (FEM) implied the reasonableness of in-situ temperature rise measured by the developed system. The developed system will become a useful tool for measuring in-situ temperature rise in animal experiments and obtaining findings with respect to the relationship between ultrasound irradiation conditions and in-situ temperature rise.

  4. Determining the gelation temperature of β-lactoglobulin using in situ microscopic imaging.

    PubMed

    Woo, Hee-Dong; Moon, Tae-Wha; Gunasekaran, Sundaram; Ko, Sanghoon

    2013-09-01

    Evolution of microstructure during heat-induced gelation of β-lactoglobulin (β-LG) was investigated in situ using confocal laser scanning microscopy at various gel-preparation conditions: pH=2, 5, and 7; protein content=5, 10, and 15%; and salt (NaCl) content=0, 0.1, and 0.3 M. The number and area of evolving β-LG clusters were observed as a function of time and temperature and the data were fitted to a log-normal model and sigmoid model, respectively. The gelation temperature (Tgel) of the β-LG system was determined from both the number (Tgel/N) and total area (Tgel/A) of β-LG clusters versus temperature data. The range of Tgel/N and Tgel/A values for all the cases was 68 to 87°C. The effect of pH was the most dominant on Tgel/N and Tgel/A, whereas the effects of β-LG and salt contents were also statistically significant. Therefore, the combined effect of protein concentration, pH, and salt content is critical to determine the overall gel microstructure and Tgel. The Tgel/N and Tgel/A generally agreed well with Tgel determined by dynamic rheometry (Tgel/R). The correlations between Tgel/N and Tgel/A versus Tgel/R were 0.85 and 0.72, respectively. In addition, Tgel/N and Tgel/A values compared well with Tgel/R values reported in the literature. Based on these results, Tgel/N determined via in situ microscopy appears to be a fairly good representative of the traditionally measured gelation temperature, Tgel/R. Copyright © 2013 American Dairy Science Association. Published by Elsevier Inc. All rights reserved.

  5. Combining altimeter data and in-situ temperature and salinity profile measurements to better estimate the 3-D thermohaline fields

    NASA Astrophysics Data System (ADS)

    Guinehut, S.; Le Traon, P.-Y.; Larnicol, G.

    2003-04-01

    Our ability in describing and understanding the ocean vertical structure strongly depends upon the availability of oceanic observations. On the one hand, temperature (T) and salinity (S) profiles measurements from eXpendable BathyThermograph (XBT), Conductivity Temperature Depth (CTD) probes and profiling floats (P-ALACE, APEX, PROVOR) provide sparse in-situ data but with precise estimations of the ocean vertical structure. Apart from specific regions of interest, theses measurements are from far not sufficient to depict the three dimensional structure of the ocean variability over the world ocean. On the other hand, satellite altimetry provides synoptic observations of sea level over the world ocean. Despite sea level being a surface signal, it reflects the state of the ocean at depths and makes satellite altimetry a powerful tool for studying global ocean dynamics and thermodynamics. The objective of this study is to analyze how to effectively merge the accurate but sparse in-situ T/S profiles data with the high spatial coverage given by altimeter measurements (as synthetic T/S profiles, deduced from statistic relationship between historical sea surface height and T/S fields) to better estimate the 3-D thermohaline fields. T/S profiles data from a real-time experiment in the North Atlantic Ocean as part of the Gyroscope Project (Argo European component) are used as a consistent data set to combine with all available altimeter data (Topex/POSEIDON, ERS-2, Jason-1, ENVISAT). The merging approach uses an optimal interpolation method that takes into account analyzed error on the observations and particularly correlated errors on the altimeter measurements. Results show that the optimal combination is instrumental in reducing the aliasing due to the mesoscale variability and in adjusting the analyzed field to the in-situ fields. The ability of the merging method to describe the 3-D thermohaline structure of the upper North Atlantic Ocean is also analyzed.

  6. Global Snow Cover Estimation with Microwave Brightness Temperature Measurements and One-Class in situ Observations

    NASA Astrophysics Data System (ADS)

    Xu, X.; Liu, X.; Li, X.; Shi, Q.

    2016-12-01

    Brightness temperature (BT), which is remotely sensed by the space-borne microwave radiometer, is widely used in snow cover monitoring for its long time series imaging capabilities in all-weather conditions. Traditional linear fitting and stand-alone methods are usually uncertain with respect to the spatial distribution and temporal variation of derived snow cover, as they rarely consider local conditions and scene characteristics but fit the model with static empirical coefficients. In this paper, a novel method utilizing daily ground in situ observations is proposed and evaluated, with the purpose for accurate estimation of long-term daily snow cover. To solve the challenge that ground snow-free records are insufficient, a one-class classifier, namely the presence and background learning (PBL) algorithm, is employed to identify daily global snow cover. Benefiting from daily ground in situ observations on a global scale, the proposed method is temporally and spatially dynamic such that estimation errors are globally independent during the entire study period. The proposed method is applied to the estimation of global daily snow cover from 1987 to 2010; the results are validated by ground in situ observations and compared with available optical-based and microwave-based snow cover products. Promising accuracy and model stability are achieved in daily, monthly and yearly validations as compared against ground observations (global omission error < 0.13, overall accuracy > 0.82 in China region, and keep stable in monthly and yearly averages). The comparison against the MODIS daily snow cover product (MOD10C1) shows good agreement under cloud-free conditions (Cohen's kappa = 0.715). The comparison against the NOAA daily Interactive Multisensor Snow and Ice Mapping System (IMS) dataset suggests promising agreement in the Northern Hemisphere. Another comparison against the AMSR-E daily SWE dataset (AE_DySno) demonstrates the efficiency of the proposed method regarding to

  7. Elevated temperature, nano-mechanical testing in situ in the scanning electron microscope

    SciTech Connect

    Wheeler, J. M.; Michler, J.

    2013-04-15

    A general nano-mechanical test platform capable of performing variable temperature and variable strain rate testing in situ in the scanning electron microscope is described. A variety of test geometries are possible in combination with focused ion beam machining or other fabrication techniques: indentation, micro-compression, cantilever bending, and scratch testing. The system is intrinsically displacement-controlled, which allows it to function directly as a micro-scale thermomechanical test frame. Stable, elevated temperature indentation/micro-compression requires the indenter tip and the sample to be in thermal equilibrium to prevent thermal displacement drift due to thermal expansion. This is achieved through independent heating and temperature monitoring of both the indenter tip and sample. Furthermore, the apex temperature of the indenter tip is calibrated, which allows it to act as a referenced surface temperature probe during contact. A full description of the system is provided, and the effects of indenter geometry and of radiation on imaging conditions are discussed. The stabilization time and temperature distribution throughout the system as a function of temperature is characterized. The advantages of temperature monitoring and thermal calibration of the indenter tip are illustrated, which include the possibility of local thermal conductivity measurement. Finally, validation results using nanoindentation on fused silica and micro-compression of <100> silicon micro-pillars as a function of temperature up to 500 Degree-Sign C are presented, and procedures and considerations taken for these measurements are discussed. A brittle to ductile transition from fracture to splitting then plastic deformation is directly observed in the SEM for silicon as a function of temperature.

  8. Regulatory pathway analysis by high-throughput in situ hybridization

    SciTech Connect

    Visel, Axel; Carson, James P.; Oldekamp, Judit; Warnecke, Marei; Jakubcakova, Vladimira; Zhou, Xunlei; Shaw, Chad; Alvarez-Bolado, Gonzalo; Eichele, Gregor

    2007-10-01

    Automated in situ hybridization (ISH) permits construction of comprehensive atlases of gene expression patterns in mammals. When web-accessible, such atlases become searchable digital expression maps of individual genes and offer an entryway to elucidate genetic interactions and signaling pathways. An atlas housing ~1,000 spatial gene expression patterns of the mid-gestation mouse embryo was generated. Patterns were textually annotated using a controlled vocabulary comprising 90 anatomical features. Hierarchical clustering of annotations was carried out using distance scores calculated from the similarity between pairs of patterns across all anatomical structures. This ordered hundreds of complex expression patterns into a matrix that reflected the embryonic architecture and the relatedness of patterns of expression. Clustering yielded twelve distinct groups of expression pattern. Because of similarity of expression patterns within a group, members of this group may be components of regulatory cascades. We focused on one group, which is composed of 83 genes, including Pax6, an evolutionary conserved transcriptional master mediator of the development. Using functional studies, ISH on Pax6-deficient embryos and Pax6 binding site identification and validation by means of electromobility shift assays, we identified numerous genes that are transcriptionally regulated by Pax6. Hence cluster analysis of annotated gene expression patterns obtained by robotic ISH is an entryway for identification of components of signaling cascades in mammals.

  9. Tensile deformation mechanisms of an in-situ Ti-based metallic glass matrix composite at cryogenic temperature.

    PubMed

    Bai, J; Li, J S; Qiao, J W; Wang, J; Feng, R; Kou, H C; Liaw, P K

    2016-08-31

    Remarkable tensile ductility was first obtained in an in-situ Ti-based bulk metallic glass (BMG) composite at cryogenic temperature (77 K). The novel cryogenic tensile plasticity is related to the effective accommodation of ductile body-centered cubic dendrites at 77 K, characteristic of the prevailing slip bands and dislocations, as well as lattice disorder, which can effectively hinder the propagation of critical shear bands. The greatly increased yield strength of dendrites contributes to the high yield strength of composite at 77 K. A trend of stronger softening is observed at low temperature, and a criterion is proposed to understand the softening behavior. The current research could also provide a guidance to the promising cryogenic application of these new advanced BMG composites.

  10. Tensile deformation mechanisms of an in-situ Ti-based metallic glass matrix composite at cryogenic temperature

    SciTech Connect

    Bai, J.; Li, J. S.; Qiao, J. W.; Wang, J.; Feng, R.; Kou, H. C.; Liaw, P. K.

    2016-08-31

    Remarkable tensile ductility was first obtained in an in-situ Ti-based bulk metallic glass (BMG) composite at cryogenic temperature (77 K). The novel cryogenic tensile plasticity is related to the effective accommodation of ductile body-centered cubic dendrites at 77 K, characteristic of the prevailing slip bands and dislocations, as well as lattice disorder, which can effectively hinder the propagation of critical shear bands. The greatly increased yield strength of dendrites contributes to the high yield strength of composite at 77 K. A trend of stronger softening is observed at low temperature, and a criterion is proposed to understand the softening behavior. In conclusion, the current research could also provide a guidance to the promising cryogenic application of these new advanced BMG composites.

  11. Tensile deformation mechanisms of an in-situ Ti-based metallic glass matrix composite at cryogenic temperature

    DOE PAGES

    Bai, J.; Li, J. S.; Qiao, J. W.; ...

    2016-08-31

    Remarkable tensile ductility was first obtained in an in-situ Ti-based bulk metallic glass (BMG) composite at cryogenic temperature (77 K). The novel cryogenic tensile plasticity is related to the effective accommodation of ductile body-centered cubic dendrites at 77 K, characteristic of the prevailing slip bands and dislocations, as well as lattice disorder, which can effectively hinder the propagation of critical shear bands. The greatly increased yield strength of dendrites contributes to the high yield strength of composite at 77 K. A trend of stronger softening is observed at low temperature, and a criterion is proposed to understand the softening behavior.more » In conclusion, the current research could also provide a guidance to the promising cryogenic application of these new advanced BMG composites.« less

  12. Tensile deformation mechanisms of an in-situ Ti-based metallic glass matrix composite at cryogenic temperature

    PubMed Central

    Bai, J.; Li, J. S.; Qiao, J. W.; Wang, J.; Feng, R.; Kou, H. C.; Liaw, P. K.

    2016-01-01

    Remarkable tensile ductility was first obtained in an in-situ Ti-based bulk metallic glass (BMG) composite at cryogenic temperature (77 K). The novel cryogenic tensile plasticity is related to the effective accommodation of ductile body-centered cubic dendrites at 77 K, characteristic of the prevailing slip bands and dislocations, as well as lattice disorder, which can effectively hinder the propagation of critical shear bands. The greatly increased yield strength of dendrites contributes to the high yield strength of composite at 77 K. A trend of stronger softening is observed at low temperature, and a criterion is proposed to understand the softening behavior. The current research could also provide a guidance to the promising cryogenic application of these new advanced BMG composites. PMID:27576728

  13. Tensile deformation mechanisms of an in-situ Ti-based metallic glass matrix composite at cryogenic temperature

    NASA Astrophysics Data System (ADS)

    Bai, J.; Li, J. S.; Qiao, J. W.; Wang, J.; Feng, R.; Kou, H. C.; Liaw, P. K.

    2016-08-01

    Remarkable tensile ductility was first obtained in an in-situ Ti-based bulk metallic glass (BMG) composite at cryogenic temperature (77 K). The novel cryogenic tensile plasticity is related to the effective accommodation of ductile body-centered cubic dendrites at 77 K, characteristic of the prevailing slip bands and dislocations, as well as lattice disorder, which can effectively hinder the propagation of critical shear bands. The greatly increased yield strength of dendrites contributes to the high yield strength of composite at 77 K. A trend of stronger softening is observed at low temperature, and a criterion is proposed to understand the softening behavior. The current research could also provide a guidance to the promising cryogenic application of these new advanced BMG composites.

  14. Engineering assessment of in situ sulfate production onboard aircraft at high altitude

    NASA Astrophysics Data System (ADS)

    Smith, J.; Dykema, J. A.; Keith, D.

    2016-12-01

    Stratospheric injection of scattering aerosols has been proposed as a way to reduce global temperature increases by decreasing net atmospheric radiative forcing. Several methods have been suggested as a means of implementing solar geoengineering, and high altitude aircraft have been identified as an accessible means delivering sulfate aerosols to the lower and mid-stratosphere. This research initiative analyzes the design features of an onboard open cycle chemical plant capable of in situ sulfur to sulfate conversion, and compares the required mass to that of transporting pre-fabricated gaseous or liquid sulfate aerosol precursors. Scaling from aero-derivative gas turbine engines, commercial catalytic converters, and existing aerospace materials indicate that aircraft equipped with such a system could provide a substantial mass benefit compared to direct transport of compound sulfate products.

  15. Preparation of nasal temperature-sensitive in situ gel of Radix Bupleuri and evaluation of the febrile response mechanism.

    PubMed

    Chen, En; Chen, Jun; Cao, Shi-Lei; Zhang, Qi-zhi; Jiang, Xin-guo

    2010-04-01

    This study developed a nasal temperature-sensitive in situ gel system for Radix Bupleuri. Using 20% Poloxamer 407 as the gel base and 6% PEG 4000 adjusting the gelation temperature. The system is liquid at 4 degrees C. It can change its phase to gel above 30 degrees C, which is close to the temperature in nasal cavity. The antipyretic effect produced by Radix Bupleuri in situ gel formulation was investigated in fevered rabbits. The results show that it can prolong the effective time to 24 hours compared with 4-6 hours in Radix Bupleuri intranasal solution. The antipyretic response mechanism was researched by evaluating the relationship between body temperature and concentrations of cyclic adenosine monophosphate in cerebrospinal fluid. The results showed that the two parameters were positively correlated (r = 0.9435, P < 0.05). Six hours later after given in situ gel, the concentrations of cAMP were significantly lower than those in the solution group. It confirmed that temperature-sensitive Radix Bupleuri in situ gel applied in the nasal sprays had a longer residence and release time. Radix Bupleuri nasal temperature-sensitive in situ gel has a higher medical effect and a longer effective time. Compared to the traditional nasal spray, it is more applicable for the treatment of fever.

  16. Room temperature deformation mechanisms of alumina particles observed from in situ micro-compression and atomistic simulations.

    SciTech Connect

    Sarobol, Pylin; Chandross, Michael E.; Carroll, Jay D.; Mook, William M.; Bufford, Daniel Charles; Boyce, Brad L.; Hattar, Khalid Mikhiel; Kotula, Paul G.; Hall, Aaron Christopher

    2015-09-22

    Aerosol deposition (AD) is a solid-state deposition technology that has been developed to fabricate ceramic coatings nominally at room temperature. Sub-micron ceramic particles accelerated by pressurized gas impact, deform, and consolidate on substrates under vacuum. Ceramic particle consolidation in AD coatings is highly dependent on particle deformation and bonding; these behaviors are not well understood. In this work, atomistic simulations and in situ micro-compressions in the scanning electron microscope, and the transmission electron microscope (TEM) were utilized to investigate fundamental mechanisms responsible for plastic deformation/fracture of particles under applied compression. Results showed that highly defective micron-sized alumina particles, initially containing numerous dislocations or a grain boundary, exhibited no observable shape change before fracture/fragmentation. Simulations and experimental results indicated that particles containing a grain boundary only accommodate low strain energy per unit volume before crack nucleation and propagation. In contrast, nearly defect-free, sub-micron, single crystal alumina particles exhibited plastic deformation and fracture without fragmentation. Dislocation nucleation/motion, significant plastic deformation, and shape change were observed. Simulation and TEM in situ micro-compression results indicated that nearly defect-free particles accommodate high strain energy per unit volume associated with dislocation plasticity before fracture. As a result, the identified deformation mechanisms provide insight into feedstock design for AD.

  17. Room temperature deformation mechanisms of alumina particles observed from in situ micro-compression and atomistic simulations.

    DOE PAGES

    Sarobol, Pylin; Chandross, Michael E.; Carroll, Jay D.; ...

    2015-09-22

    Aerosol deposition (AD) is a solid-state deposition technology that has been developed to fabricate ceramic coatings nominally at room temperature. Sub-micron ceramic particles accelerated by pressurized gas impact, deform, and consolidate on substrates under vacuum. Ceramic particle consolidation in AD coatings is highly dependent on particle deformation and bonding; these behaviors are not well understood. In this work, atomistic simulations and in situ micro-compressions in the scanning electron microscope, and the transmission electron microscope (TEM) were utilized to investigate fundamental mechanisms responsible for plastic deformation/fracture of particles under applied compression. Results showed that highly defective micron-sized alumina particles, initially containingmore » numerous dislocations or a grain boundary, exhibited no observable shape change before fracture/fragmentation. Simulations and experimental results indicated that particles containing a grain boundary only accommodate low strain energy per unit volume before crack nucleation and propagation. In contrast, nearly defect-free, sub-micron, single crystal alumina particles exhibited plastic deformation and fracture without fragmentation. Dislocation nucleation/motion, significant plastic deformation, and shape change were observed. Simulation and TEM in situ micro-compression results indicated that nearly defect-free particles accommodate high strain energy per unit volume associated with dislocation plasticity before fracture. As a result, the identified deformation mechanisms provide insight into feedstock design for AD.« less

  18. Comparison of Land Skin Temperature from a Land Model, Remote Sensing, and In-situ Measurement

    NASA Technical Reports Server (NTRS)

    Wang, Aihui; Barlage, Michael; Zeng, Xubin; Draper, Clara Sophie

    2014-01-01

    Land skin temperature (Ts) is an important parameter in the energy exchange between the land surface and atmosphere. Here hourly Ts from the Community Land Model Version 4.0, MODIS satellite observations, and in-situ observations in 2003 were compared. Compared with the in-situ observations over four semi-arid stations, both MODIS and modeled Ts show negative biases, but MODIS shows an overall better performance. Global distribution of differences between MODIS and modeled Ts shows diurnal, seasonal, and spatial variations. Over sparsely vegetated areas, the model Ts is generally lower than the MODIS observed Ts during the daytime, while the situation is opposite at nighttime. The revision of roughness length for heat and the constraint of minimum friction velocity from Zeng et al. [2012] bring the modeled Ts closer to MODIS during the day, and have little effect on Ts at night. Five factors contributing to the Ts differences between the model and MODIS are identified, including the difficulty in properly accounting for cloud cover information at the appropriate temporal and spatial resolutions, and uncertainties in surface energy balance computation, atmospheric forcing data, surface emissivity, and MODIS Ts data. These findings have implications for the cross-evaluation of modeled and remotely sensed Ts, as well as the data assimilation of Ts observations into Earth system models.

  19. Microstructural Changes in MBE Growth of Low-Temperature Gallium Arsenide Observed by in Situ Ellipsometry

    NASA Astrophysics Data System (ADS)

    Eyink, Kurt Gerard

    1995-01-01

    An ellipsometer system has been developed for in-situ monitoring of III-V semiconductor growth using molecular beam epitaxy. Included as part of this work, a software package was developed for the calibration, acquisition, display and modeling of ellipsometry data. This calibration software addresses the arbitrary orientations of the analyzer and polarizer components that are present in the mounting of the ellipsometer on the MBE system. In addition, this package calculated the trajectory followed during the growth of a homogeneous film. The materials used in the modeling are restricted to either an isotropic material or a uniaxial material with the optic axis oriented normal to the surface. External to the real-time software package, a general scheme for the analysis of ellipsometric data was developed using MATLAB. The ellipsometer described above was utilized to reproducibly grow and monitor the growth of low temperature (LT) GaAs films in-situ. In particular the capping of GaAs(001) with As was monitored and a method was developed which could be used to characterize the growth temperature of GaAs in the vicinity of 190^circ C. This method utilizes the temperature for the formation of a thin film of As on GaAs(001). Using this technique to set the growth conditions, LT-GaAs films were grown and monitored in real-time with the ellipsometer and characterized ex-situ with X-ray diffraction (XRD) and transmission electron microscopy (TEM.) The ellipsometry data allowed for the observation of the formation of the epitaxial LT-GaAs film and a subsequent region of changing dielectric properties. These results are correlated with observation in double crystal X-ray diffraction (DXRD) and TEM analysis, showing that the refractive index can be used to indicate the composition of the LT-GaAs films and that the ellipsometer can observe the breakdown in the crystallinity of the LT-GaAs layers.

  20. Estimation of in-situ thermal conductivities from temperature gradient measurements

    SciTech Connect

    Hoang, V.T.

    1980-12-01

    A mathematical model has been developed to study the effect of variable thermal conductivity of the formations, and the wellbore characteristics, on the fluid temperature behavior inside the wellbore during injection or production and after shut-in. During the injection or production period the wellbore fluid temperature is controlled mainly by the fluid flow rate and the heat lost from the fluid to the formation. During the shut-in period, the fluid temperature is strongly affected by differences in the formation thermal conductivities. Based on the results of the present analysis, two methods for estimating in-situ thermal conductivity were derived. First, the line source concept is extended to estimate values of the formation thermal conductivities utilizing the fluid temperature record during the transient period of injection or production and shut-in. The second method is applied when a well is under thermal equilibrium conditions. Values of the formation thermal conductivities can also be estimated by using a continuous temperature gradient log and by measuring the thermal conductivity of the formation at a few selected wellbore locations.

  1. Prediction of melting temperatures in fluorescence in situ hybridization (FISH) procedures using thermodynamic models.

    PubMed

    Fontenete, Sílvia; Guimarães, Nuno; Wengel, Jesper; Azevedo, Nuno Filipe

    2016-01-01

    The thermodynamics and kinetics of DNA hybridization, i.e. the process of self-assembly of one, two or more complementary nucleic acid strands, has been studied for many years. The appearance of the nearest-neighbor model led to several theoretical and experimental papers on DNA thermodynamics that provide reasonably accurate thermodynamic information on nucleic acid duplexes and allow estimation of the melting temperature. Because there are no thermodynamic models specifically developed to predict the hybridization temperature of a probe used in a fluorescence in situ hybridization (FISH) procedure, the melting temperature is used as a reference, together with corrections for certain compounds that are used during FISH. However, the quantitative relation between melting and experimental FISH temperatures is poorly described. In this review, various models used to predict the melting temperature for rRNA targets, for DNA oligonucleotides and for nucleic acid mimics (chemically modified oligonucleotides), will be addressed in detail, together with a critical assessment of how this information should be used in FISH.

  2. Development of an Expanded, High Reliability Cost and Performance Database for In Situ Remediation Technologies

    DTIC Science & Technology

    2016-03-01

    FINAL REPORT Development of an Expanded, High-Reliability Cost and Performance Database for In-Situ Remediation Technologies ESTCP Project... Database for In-Situ Remediation Technologies Travis McGuire David Adamson Charles Newell Poonam Kulkarni GSI Environmental, Inc. GSI Environmental...technologies. The overall objective of this work was to develop a comprehensive remediation performance and cost database . N/A U U U UU 109 Travis

  3. In situ multipurpose time-resolved spectrometer for monitoring nanoparticle generation in a high-pressure fluid

    SciTech Connect

    Wei, Shaoyu; Saitow, Ken-ichi

    2012-07-15

    We developed a multipurpose time-resolved spectrometer for studying the dynamics of nanoparticles generated by pulsed-laser ablation (PLA) in a high-pressure fluid. The apparatus consists of a high-pressure optical cell and three spectrometers for in situ measurements. The optical cell was designed for experiments at temperatures up to 400 K and pressures up to 30 MPa with fluctuations within {+-}0.1% h{sup -1}. The three spectrometers were used for the following in situ measurements at high pressures: (i) transient absorption spectrum measurements from 350 to 850 nm to investigate the dynamics of nanoparticle generation from nanoseconds to milliseconds after laser irradiation, (ii) absorption spectrum measurements from 220 to 900 nm to observe the time evolution of nanoparticles from seconds to hours after laser ablation, and (iii) dynamic light scattering measurements to track nanoparticles with sizes from 10 nm to 10 {mu}m in the time range from seconds to hours after laser ablation. By combining these three spectrometers, we demonstrate in situ measurements of gold nanoparticles generated by PLA in supercritical fluids. This is the first report of in situ time-resolved measurements of the dynamics of nanoparticles generated in a supercritical fluid.

  4. In situ Pb-Pb dating of rutile from slowly cooled granulites by LA-MC-ICP-MS: confirmation of the high closure temperature (>=600°C) for Pb diffusion in rutile

    NASA Astrophysics Data System (ADS)

    Vry, J.; Baker, J.; Waight, T.

    2003-04-01

    We have analysed Pb isotopes in natural rutile crystals by laser ablation MC-ICP-MS to assess the potential of rapid Pb-Pb dating of rutile with this method. The rutile samples are from granulite-facies Mg- and Al-rich rocks from the Reynolds Range, Northern Territory, Australia. This metamorphic terrane has a well-constrained high-T cooling history (ca. 3^oC/Myr) defined by previous U-Pb dating of monazite and zircon (peak metamorphism at 1584 Ma), which we have supplemented with additional Rb-Sr dates of phlogopite, biotite and muscovite. The dated rutiles vary in size from 3 to 0.05 mm, have Pb concentrations of ca. 20 ppm, and were analysed with a 266 nm laser coupled to an AXIOM MC-ICP-MS (spot size of 200-50 μm). Individual larger crystals (>= 200 μm) exhibit sufficient Pb isotopic heterogeneity (206Pb/204Pb = 10000-80000) to perform isochron calculations on several short analyses of a single grain (30-60 s). The largest rutiles yielded Pb-Pb isochron ages of 1540-1555 Ma with typical uncertainties of ± 1 to 10 Ma. 207Pb/206Pb ages are typically within 1% of the Pb-Pb isochron ages testifying to the radiogenic nature of Pb in the rutile. A mean age for all the analysed rutiles was 1548.4 ± 9.1 Ma (n = 33). Comparable 207Pb/206Pb ages were also obtained from individual smaller crystals (50 μm) where the 204Pb ion beam could not be measured precisely. The results demonstrate that even small rutile crystals are extremely resistant to isotopic resetting, and that this mineral is a high-T chronometer. Phlogopite and muscovite Rb-Sr ages are <1454 and 1400-1480 Ma, respectively, with some of the phlogopite and biotite micas having been partially reset by later thermal events younger than 400 Ma. All the mica ages are considerably younger (100-70 My) than the rutile ages, which approach U-Pb ages for monazite and zircon overgrowths, even though the mica closure temperatures (350-500^oC) are comparable or slightly higher than earlier geological estimates [1] of

  5. Spatial and Temporal Variations of Surface Temperature Over Greenland As Observed In AIRS, MODIS and In-Situ Measurements

    NASA Astrophysics Data System (ADS)

    Lee, J. N.; Susskind, J.; Wu, D. L.; Nowicki, S.; Hall, D. K.; Iredell, L. F.

    2015-12-01

    This paper compares the temporal and spatial characteristics of the AIRS and MODIS surface temperatures over Greenland. To estimate uncertainties in space-based temperature measurements, we reprojected the MODIS Ice Surface Temperature (IST) into 0.5 by 0.5 degree spatial resolution. We also re-gridded AIRS Skin Temperature (Ts) with same spatial resolution but classified with different cloud conditions and surface types. These co-located data sets make intercomparison between the two instruments relatively straightforward. By this approach, the spatial comparison between AIRS Ts and MODIS IST monthly mean is in good agreement with RMS less than 2K during May 2012. This approach also allows the detection of any long-term calibration drift and the careful examination of calibration consistency in MODIS and AIRS temperature data record. The temporal correlations between temperature data are also compared with those from in-situ measurements from GC-Net and NOAA stations. The most significant diurnal difference is found during spring season (April and May) in high altitude regions, when interannual variability is relatively smaller than summer and winter.

  6. Evolution of extended defects in polycrystalline Au-irradiated UO2 using in situ TEM: Temperature and fluence effects

    NASA Astrophysics Data System (ADS)

    Onofri, C.; Sabathier, C.; Baumier, C.; Bachelet, C.; Palancher, H.; Legros, M.

    2016-12-01

    In situ Transmission Electron Microscopy irradiations were performed on polycrystalline UO2 thin foils with 4 MeV gold ions at three different temperatures: 600 °C, room and liquid nitrogen temperature. In order to study the dislocation evolution and to determine the growth mechanisms, the dislocation loop and line densities and the loop size repartition were monitored as a function of fluence, and irradiation temperature. We show that dislocation loops, with Burgers vectors along the <110> directions, evolve into dislocation lines with increasing fluence by a loop overlapping mechanism. Furthermore, a fluence offset is highlighted between the irradiations performed at high and low temperature due to an increase of the defect mobility. Indeed, a growth by Oswald ripening is probably activated at room temperature and 600 °C and changes the kinetic evolution of loops into lines. After this transformation, and for all the irradiation temperatures, a steady state equilibrium is reached where both extended defects (dislocation lines and small dislocations loops -around 5 nm in size-) are observed simultaneously. A continuous nucleation of small dislocation loops and of nanometer-sized cavities formed directly by irradiation is also highlighted.

  7. One-dimensional soil temperature simulation with Common Land Model by assimilating in situ observations and MODIS LST with the ensemble particle filter

    NASA Astrophysics Data System (ADS)

    Yu, Zhongbo; Fu, Xiaolei; Luo, Lifeng; Lü, Haishen; Ju, Qin; Liu, Di; Kalin, Dresden A.; Huang, Dui; Yang, Chuanguo; Zhao, Lili

    2014-08-01

    Soil temperature plays an important role in hydrology, agriculture, and meteorology. In order to improve the accuracy of soil temperature simulation, a soil temperature data assimilation system was developed based on the Ensemble Particle Filter (EnPF) and the Common Land Model (CLM), and then applied in the Walnut Gulch Experimental Watershed (WGEW) in Arizona, United States. Surface soil temperature in situ observations and Moderate Resolution Imaging Spectroradiometer Land Surface Temperature (MODIS LST) data were assimilated into the system. In this study, four different assimilation experiments were conducted: (1) assimilating in situ observations of instantaneous surface soil temperature each hour, (2) assimilating in situ observations of instantaneous surface soil temperature once per day, (3) assimilating verified MODIS LST once per day, and (4) assimilating original MODIS LST once per day. These four experiments reflect a transition from high-quality and more frequent in situ observations to lower quality and less frequent remote sensing data in the data assimilation system. The results from these four experiments show that the assimilated results are better than the simulated results without assimilation at all layers except the bottom layer, while the superiority gradually diminishes as the quality and frequency of the observations decrease. This demonstrates that remote sensing data can be assimilated using the ensemble particle filter in poorly gauged catchments to obtain highly accurate soil variables (e.g., soil moisture, soil temperature). Meanwhile, the results also demonstrate that the ensemble particle filter is effective in assimilating soil temperature observations to improve simulations, but the performance of the data assimilation method is affected by the frequency of assimilation and the quality of the input data.

  8. Comparison of Satellite-Derived and In-Situ Observations of Ice and Snow Surface Temperatures over Greenland

    NASA Technical Reports Server (NTRS)

    Hall, Dorothy K.; Box, Jason E.; Casey, Kimberly A.; Hook, Simon J.; Shuman, Christopher A.; Steffen, Konrad

    2008-01-01

    The most practical way to get a spatially broad and continuous measurements of the surface temperature in the data-sparse cryosphere is by satellite remote sensing. The uncertainties in satellite-derived LSTs must be understood to develop internally-consistent decade-scale land-surface temperature (LST) records needed for climate studies. In this work we assess satellite-derived "clear-sky" LST products from the Moderate Resolution Imaging Spectroradiometer (MODIS) and the Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER), and LSTs derived from the Enhanced Thematic Mapper Plus (ETM+) over snow and ice on Greenland. When possible, we compare satellite-derived LSTs with in-situ air-temperature observations from Greenland Climate Network (GC-Net) automatic-weather stations (AWS). We find that MODIS, ASTER and ETM+ provide reliable and consistent LSTs under clear-sky conditions and relatively-flat terrain over snow and ice targets over a range of temperatures from -40 to 0 C. The satellite-derived LSTs agree within a relative RMS uncertainty of approx.0.5 C. The good agreement among the LSTs derived from the various satellite instruments is especially notable since different spectral channels and different retrieval algorithms are used to calculate LST from the raw satellite data. The AWS record in-situ data at a "point" while the satellite instruments record data over an area varying in size from: 57 X 57 m (ETM+), 90 X 90 m (ASTER), or to 1 X 1 km (MODIS). Surface topography and other factors contribute to variability of LST within a pixel, thus the AWS measurements may not be representative of the LST of the pixel. Without more information on the local spatial patterns of LST, the AWS LST cannot be considered valid ground truth for the satellite measurements, with RMS uncertainty approx.2 C. Despite the relatively large AWS-derived uncertainty, we find LST data are characterized by high accuracy but have uncertain absolute precision.

  9. In-Situ X-ray Spectroscopic Studies of the Fundamental Chemistry of Pb and Pb-Bi Corrosion Processes at High Temperatures: Development and Assessment of Composite Corrosion Resistant Materials.

    SciTech Connect

    Carlo Segre

    2009-12-30

    Over the course of this project, we have a number of accomplishments. The following list is presented as a summary statement for the project. Specific details from previous Quarterly Reports are given. (1) We established that it is possible to use EXAFS to study the interface layer between a material and the liquid Pb overlayer. We have discovered that molybdenum grows a selflimiting oxide layer which does not spall even at the highest temperatures studied. There have been 2 publications resulting from these studies. (2) We have fabricated a high temperature environmental chamber capable of extending the Pb overlayer studies by varying the incident x-ray beam angle to perform depth profiling of the Pb layer. This chamber will continue to be available to nuclear materials program researchers who wish to use the MRCAT beam line. (3) We have developed a collaboration with researchers at the Paul Scherrer Institute to study corrosion layers on zircalloy. One publication has resulted from this collaboration and another is in progress. (4) We have developed a collaboration with Prof. G.R. Odette of UCSB in which we studied the local structure of Ti and Y in nanoclusters found in oxygen dispersion strengthened steels. There are two publications in progress form this collaboration and we have extended the project to anomalous small angle x-ray scattering as well as EXAFS. (5) We have promoted the use of EXAFS for the study of nuclear materials to the community over the past 4 years and we have begun to see an increase in demand for EXAFS from the community at the MRCAT beam line. (6) This grant was instrumental in nucleating interest in establishing a new Collaborative Access Team at the Advanced Photon Source, the Nuclear and Radiological Research CAT (NRR-CAT). The co-PI (Jeff Terry) is the lead investigator on this project and it has been approved by the APS Scientific Advisory Committee for further planning. The status of the NRR-CAT project is being discussed in a

  10. Influence of temperature on carbon and nitrogen dynamics during in situ aeration of aged waste in simulated landfill bioreactors.

    PubMed

    Tong, Huanhuan; Yin, Ke; Giannis, Apostolos; Ge, Liya; Wang, Jing-Yuan

    2015-09-01

    The effect of temperature on carbon and nitrogen compounds during in situ aeration of aged waste was investigated in lab-scale simulated landfill bioreactors at 35, 45 and 55 °C, respectively. The bioreactor operated at 55 °C presented the highest carbon mineralization rate in the initial stage, suggesting accelerated biodegradation rates under thermophilic conditions. The nitrogen speciation study indicated that organic nitrogen was the dominant species of total N in aerobic bioreactors due to ammonia removal. Leachate organic nitrogen was further fractionated to elucidate the fate of individual constituent. Detailed investigation revealed the higher bioconversion rates of N-humic and N-fulvic compounds compared to hydrophilic compounds in thermophilic conditions. At the end, waste material in 55 °C bioreactor was richer in highly matured humic substances (HS) verifying the high bioconversion rates.

  11. Oil-Well Cement and C[subscript 3]S Hydration Under High Pressure as Seen by In Situ X-Ray Diffraction, Temperatures 80[degrees]C with No Additives

    SciTech Connect

    Jupe, Andrew C.; Wilkinson, Angus P.; Funkhouser, Gary P.

    2013-01-10

    The hydration kinetics of a white cement and batches of both Class G and H oil-well cements were examined between 0 and 60 MPa, at {le}80 C, using in situ synchrotron X-ray diffraction. This gives a continuous measure of the C{sub 3}S (Ca{sub 3}SiO{sub 5}), CH (Ca(OH){sub 2}), C{sub 4}AF (Ca{sub 2}FeAlO{sub 5}), ettringite, and other phases in the hydrating slurries. Slurries prepared from single-phase C{sub 3}S; synthetic C{sub 4}AF, and gypsum; and white cement, synthetic C{sub 4}AF and gypsum were also examined. An increasing pressure enhanced the rate of hydration for all slurries. Analysis of the data, using a kinetic model, provided rate constants that were used to obtain activation volumes for C{sub 3}S hydration. For all the cement and C{sub 3}S slurries studied, similar activation volumes were obtained (average {Delta}{double_dagger}{approx}-35 cm{sup 3}/mol), indicating that the presence of cement phases other than C{sub 3}S has a modest influence on the pressure dependence of C{sub 3}S hydration. An alternative analysis, using the time at which 90% of the initial C{sub 3}S remained, gave similar activation volumes. Pressure accelerated the formation of ettringite from synthetic C{sub 4}AF in the presence of gypsum. However, in slurries containing cement, the pressure dependence of C{sub 3}S hydration plays a major role in determining the pressure dependence of ettringite formation.

  12. Effects of Temperature, Salinity, and Substrate on the Colonization of Surfaces In Situ by Aquatic Bdellovibrios

    PubMed Central

    Kelley, J. I.; Turng, B.; Williams, H. N.; Baer, M. L.

    1997-01-01

    Recent studies suggest that surfaces are a more conducive habitat than the water column for the proliferation of bdellovibrios in the aquatic environment. The effect of temperature and salinity on the colonization of bdellovibrios on oyster shell, glass, and polystyrene surfaces in situ was investigated over an annual cycle. Sterile surfaces were suspended in various bodies of water for intervals ranging from 24 to 120 h. The results revealed that bdellovibrios associated with different types of surfaces over a broad temperature and salinity range. After 24 h of submersion in waters with temperatures from 9.0 to 26.7(deg)C, the ranges in log(inf10) values per square centimeter for the three surfaces were as follows: oyster shell, 2.2 to 2.5; glass, 0.3 to 2.2; and polystyrene, 0.7 to 1.6. Bdellovibrios were not recovered from surfaces submerged in water at temperatures below 8(deg)C during the 120-h experimental cycle. The number of bdellovibrios and culturable bacteria on oyster shells was significantly higher than the numbers on glass and polystyrene at all time intervals. The number of bdellovibrios was positively correlated with temperature and salinity on all surfaces. A positive correlation between the number of recoverable bacteria and temperature was observed, but the results with respect to salinity were diverse. The numbers of bdellovibrios recovered from oyster shells (up to 48 h) and water samples were significantly increased at salinities greater than 11(permil) compared to those in lower-salinity environments. The results of this study reveal that like many other bacteria in the aquatic environment, bdellovibrios prefer to associate with surfaces. This association provides the predators a rich source of prey bacteria in surface biofilms and perhaps protection in the gel-like matrix of the biofilm. PMID:16535502

  13. Kinetics of methane hydrate decomposition studied via in situ low temperature X-ray powder diffraction.

    PubMed

    Everett, S Michelle; Rawn, Claudia J; Keffer, David J; Mull, Derek L; Payzant, E Andrew; Phelps, Tommy J

    2013-05-02

    Gas hydrate is known to have a slowed decomposition rate at ambient pressure and temperatures below the melting point of ice. As hydrate exothermically decomposes, gas is released and water of the clathrate cages transforms into ice. Based on results from the decomposition of three nominally similar methane hydrate samples, the kinetics of two regions, 180-200 and 230-260 K, within the overall decomposition range 140-260 K, were studied by in situ low temperature X-ray powder diffraction. The kinetic rate constants, k(a), and the reaction mechanisms, n, for ice formation from methane hydrate were determined by the Avrami model within each region, and activation energies, E(a), were determined by the Arrhenius plot. E(a) determined from the data for 180-200 K was 42 kJ/mol and for 230-260 K was 22 kJ/mol. The higher E(a) in the colder temperature range was attributed to a difference in the microstructure of ice between the two regions.

  14. Brightness temperature simulation of snow cover based on snow grain size evolution using in situ data

    NASA Astrophysics Data System (ADS)

    Wu, Lili; Li, Xiaofeng; Zhao, Kai; Zheng, Xingming; Jiang, Tao

    2016-07-01

    Snow depth parameter inversion from passive microwave remote sensing is of great significance to hydrological process and climate systems. The Helsinki University of Technology (HUT) model is a commonly used snow emission model. Snow grain size (SGS) is one of the important input parameters, but SGS is difficult to obtain in broad areas. The time series of SGS are first evolved by an SGS evolution model (Jordan 91) using in situ data. A good linear relationship between the effective SGS in HUT and the evolution SGS was found. Then brightness temperature simulations are performed based on the effective SGS and evolution SGS. The results showed that the biases of the simulated brightness temperatures based on the effective SGS and evolution SGS were -6.5 and -3.6 K, respectively, for 18.7 GHz and -4.2 and -4.0 K for 36.5 GHz. Furthermore, the model is performed in six pixels with different land use/cover type in other areas. The results showed that the simulated brightness temperatures based on the evolution SGS were consistent with those from the satellite. Consequently, evolution SGS appears to be a simple method to obtain an appropriate SGS for the HUT model.

  15. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    DOE PAGES

    Huang, Shenyan; Gao, Yanfei; An, Ke; ...

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticitymore » theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.« less

  16. Low-temperature in situ large strain plasticity of ceramic SiC nanowires and its atomic-scale mechanism.

    PubMed

    Han, X D; Zhang, Y F; Zheng, K; Zhang, X N; Zhang, Z; Hao, Y J; Guo, X Y; Yuan, J; Wang, Z L

    2007-02-01

    Large strain plasticity is phenomenologically defined as the ability of a material to exhibit an exceptionally large deformation rate during mechanical deformation. It is a property that is well established for metals and alloys but is rarely observed for ceramic materials especially at low temperature ( approximately 300 K). With the reduction in dimensionality, however, unusual mechanical properties are shown by ceramic nanomaterials. In this Letter, we demonstrated unusually large strain plasticity of ceramic SiC nanowires (NWs) at temperatures close to room temperature that was directly observed in situ by a novel high-resolution transmission electron microscopy technique. The continuous plasticity of the SiC NWs is accompanied by a process of increased dislocation density at an early stage, followed by an obvious lattice distortion, and finally reaches an entire structure amorphization at the most strained region of the NW. These unusual phenomena for the SiC NWs are fundamentally important for understanding the nanoscale fracture and strain-induced band structure variation for high-temperature semiconductors. Our result may also provide useful information for further studying of nanoscale elastic-plastic and brittle-ductile transitions of ceramic materials with superplasticity.

  17. Deformation mechanisms in a precipitation-strengthened ferritic superalloy revealed by in situ neutron diffraction studies at elevated temperatures

    SciTech Connect

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Wu, Wei; Teng, Zhenke; Liaw, Peter K

    2014-10-22

    In this study, the ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)Al B2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticity theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.

  18. Deformation mechanisms in a precipitation-strengthened ferritic super alloy revealed by in situ neutron dffraction studies at elevated temperatures

    SciTech Connect

    Huang, Shenyan; Gao, Yanfei; An, Ke; Zheng, Lili; Teng, Zhenke; Wu, Wei; Liaw, Peter K.

    2015-01-01

    The ferritic superalloy Fe–10Ni–6.5Al–10Cr–3.4Mo strengthened by ordered (Ni,Fe)AlB2-type precipitates is a candidate material for ultra-supercritical steam turbine applications above 923 K. Despite earlier success in improving its room-temperature ductility, the creep resistance of this material at high temperatures needs to be further improved, which requires a fundamental understanding of the high-temperature deformation mechanisms at the scales of individual phases and grains. In situ neutron diffraction has been utilized to investigate the lattice strain evolution and the microscopic load-sharing mechanisms during tensile deformation of this ferritic superalloy at elevated temperatures. Finite-element simulations based on the crystal plasticity theory are employed and compared with the experimental results, both qualitatively and quantitatively. Based on these interphase and intergranular load-partitioning studies, it is found that the deformation mechanisms change from dislocation slip to those related to dislocation climb, diffusional flow and possibly grain boundary sliding, below and above 873 K, respectively. Insights into microstructural design for enhancing creep resistance are also discussed.

  19. A review of uncertainty in in situ measurements and data sets of sea surface temperature

    NASA Astrophysics Data System (ADS)

    Kennedy, John J.

    2014-03-01

    Archives of in situ sea surface temperature (SST) measurements extend back more than 160 years. Quality of the measurements is variable, and the area of the oceans they sample is limited, especially early in the record and during the two world wars. Measurements of SST and the gridded data sets that are based on them are used in many applications so understanding and estimating the uncertainties are vital. The aim of this review is to give an overview of the various components that contribute to the overall uncertainty of SST measurements made in situ and of the data sets that are derived from them. In doing so, it also aims to identify current gaps in understanding. Uncertainties arise at the level of individual measurements with both systematic and random effects and, although these have been extensively studied, refinement of the error models continues. Recent improvements have been made in the understanding of the pervasive systematic errors that affect the assessment of long-term trends and variability. However, the adjustments applied to minimize these systematic errors are uncertain and these uncertainties are higher before the 1970s and particularly large in the period surrounding the Second World War owing to a lack of reliable metadata. The uncertainties associated with the choice of statistical methods used to create globally complete SST data sets have been explored using different analysis techniques, but they do not incorporate the latest understanding of measurement errors, and they want for a fair benchmark against which their skill can be objectively assessed. These problems can be addressed by the creation of new end-to-end SST analyses and by the recovery and digitization of data and metadata from ship log books and other contemporary literature.

  20. In Situ deposition of YBCO high-T(sub c) superconducting thin films by MOCVD and PE-MOCVD

    NASA Technical Reports Server (NTRS)

    Zhao, J.; Noh, D. W.; Chern, C.; Li, Y. Q.; Norris, P.; Gallois, B.; Kear, B.

    1990-01-01

    Metalorganic Chemical Vapor Deposition (MOCVD) offers the advantages of a high degree of compositional control, adaptability for large scale production, and the potential for low temperature fabrication. The capability of operating at high oxygen partial pressure is particularly suitable for in situ formation of high temperature superconducting (HTSC) films. Yttrium barium copper oxide (YBCO) thin films having a sharp zero-resistance transition with T( sub c) greater than 90 K and Jc approx. 10 to the 4th power A on YSZ have been prepared, in situ, at a substrate temperature of about 800 C. Moreover, the ability to form oxide films at low temperature is very desirable for device applications of HTSC materials. Such a process would permit the deposition of high quality HTSC films with a smooth surface on a variety of substrates. Highly c-axis oriented, dense, scratch resistant, superconducting YBCO thin films with mirror-like surfaces have been prepared, in situ, at a reduced substrate temperature as low as 570 C by a remote microwave-plasma enhanced metalorganic chemical vapor deposition (PE-MOCVD) process. Nitrous oxide was used as a reactant gas to generate active oxidizing species. This process, for the first time, allows the formation of YBCO thin films with the orthorhombic superconducting phase in the as-deposited state. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K with a transition width of about 5 K. MOCVD was carried out in a commercial production scale reactor with the capability of uniform deposition over 100 sq cm per growth run. Preliminary results indicate that PE-MOCVD is a very attractive thin film deposition process for superconducting device technology.

  1. In-situ deposition of YBCO high-Tc superconducting thin films by MOCVD and PE-MOCVD

    NASA Technical Reports Server (NTRS)

    Zhao, J.; Noh, D. W.; Chern, C.; Li, Y. Q.; Norris, P. E.; Kear, B.; Gallois, B.

    1991-01-01

    Metal-Organic Chemical Vapor Deposition (MOCVD) offers the advantages of a high degree of compositional control, adaptability for large scale production, and the potential for low temperature fabrication. The capability of operating at high oxygen partial pressure is particularly suitable for in situ formation of high temperature superconducting (HTSC) films. Yttrium barium copper oxide (YBCO) thin films having a sharp zero-resistance transition with T(sub c) greater than 90 K and J(sub c) of approximately 10(exp 4) A on YSZ have been prepared, in situ, at a substrate temperature of about 800 C. Moreover, the ability to form oxide films at low temperature is very desirable for device applications of HTSC materials. Such a process would permit the deposition of high quality HTSC films with a smooth surface on a variety of substrates. Highly c-axis oriented, dense, scratch resistant, superconducting YBCO thin films with mirror-like surfaces have been prepared, in situ, at a reduced substrate temperature as low as 570 C by a remote microwave-plasma enhanced metal-organic chemical vapor deposition (PE-MOCVD) process. Nitrous oxide was used as a reactant gas to generate active oxidizing species. This process, for the first time, allows the formation of YBCO thin films with the orthorhombic superconducting phase in the as-deposited state. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K with a transition width of about 5 K. MOCVD was carried out in a commercial production scale reactor with the capability of uniform deposition over 100 sq cm per growth run. Preliminary results indicate that PE-MOCVD is a very attractive thin film deposition process for superconducting device technology.

  2. Note: High-pressure in situ x-ray laminography using diamond anvil cell

    NASA Astrophysics Data System (ADS)

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-01

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences.

  3. Note: High-pressure in situ x-ray laminography using diamond anvil cell

    SciTech Connect

    Nomura, Ryuichi; Uesugi, Kentaro

    2016-04-15

    A high-pressure in situ X-ray laminography technique was developed using a newly designed, laterally open diamond anvil cell. A low X-ray beam of 8 keV energy was used, aiming at future application to dual energy X-ray chemical imaging techniques. The effects of the inclination angle and the imaging angle range were evaluated at ambient pressure using the apparatus. Sectional images of ruby ball samples were successfully reconstructed at high pressures, up to approximately 50 GPa. The high-pressure in situ X-ray laminography technique is expected to provide new insights into the deep Earth sciences.

  4. High pressure synthesis and in situ Raman spectroscopy of H2 and HD clathrate hydrates.

    PubMed

    Zaghloul, Mohamed A S; Celli, Milva; Salem, N M; Elsheikh, S M; Ulivi, Lorenzo

    2012-10-28

    By means of a newly constructed high pressure and low temperature optical apparatus we have measured the Raman spectra of H(2) and HD simple clathrate hydrates, synthesized in situ by the application of more than 2500 bar gas pressure on solid water. High resolution spectra of the molecular vibration have been measured at low temperature (about 20 K). In the case of HD this band is simpler than in the case of H(2), where the presence of the ortho- and para-species complicated the interpretation of the spectrum. We have determined frequency positions of the bands arising from multiple occupancy of the large cages of the sII clathrate, some of which are almost superimposed. The intensity of the bands gives information on the average and distribution of cage occupation, and of the ortho-para (o-p) ratio of H(2) molecules. Hydrogen o-p conversion rate is measured, for molecules in the small cages and in the large cages, and it is observed that these are different. A model considering both intrinsic and extrinsic conversion processes is applied to the measured data. The intrinsic conversion rate so derived is compared favorably to that measured for pure hydrogen in different situations.

  5. High pressure synthesis and in situ Raman spectroscopy of H2 and HD clathrate hydrates

    NASA Astrophysics Data System (ADS)

    Zaghloul, Mohamed A. S.; Celli, Milva; Salem, N. M.; Elsheikh, S. M.; Ulivi, Lorenzo

    2012-10-01

    By means of a newly constructed high pressure and low temperature optical apparatus we have measured the Raman spectra of H2 and HD simple clathrate hydrates, synthesized in situ by the application of more than 2500 bar gas pressure on solid water. High resolution spectra of the molecular vibration have been measured at low temperature (about 20 K). In the case of HD this band is simpler than in the case of H2, where the presence of the ortho- and para-species complicated the interpretation of the spectrum. We have determined frequency positions of the bands arising from multiple occupancy of the large cages of the sII clathrate, some of which are almost superimposed. The intensity of the bands gives information on the average and distribution of cage occupation, and of the ortho-para (o-p) ratio of H2 molecules. Hydrogen o-p conversion rate is measured, for molecules in the small cages and in the large cages, and it is observed that these are different. A model considering both intrinsic and extrinsic conversion processes is applied to the measured data. The intrinsic conversion rate so derived is compared favorably to that measured for pure hydrogen in different situations.

  6. Two stage, low temperature, catalyzed fluidized bed incineration with in situ neutralization for radioactive mixed wastes

    SciTech Connect

    Wade, J.F.; Williams, P.M.

    1995-05-17

    A two stage, low temperature, catalyzed fluidized bed incineration process is proving successful at incinerating hazardous wastes containing nuclear material. The process operates at 550{degrees}C and 650{degrees}C in its two stages. Acid gas neutralization takes place in situ using sodium carbonate as a sorbent in the first stage bed. The feed material to the incinerator is hazardous waste-as defined by the Resource Conservation and Recovery Act-mixed with radioactive materials. The radioactive materials are plutonium, uranium, and americium that are byproducts of nuclear weapons production. Despite its low temperature operation, this system successfully destroyed poly-chlorinated biphenyls at a 99.99992% destruction and removal efficiency. Radionuclides and volatile heavy metals leave the fluidized beds and enter the air pollution control system in minimal amounts. Recently collected modeling and experimental data show the process minimizes dioxin and furan production. The report also discusses air pollution, ash solidification, and other data collected from pilot- and demonstration-scale testing. The testing took place at Rocky Flats Environmental Technology Site, a US Department of Energy facility, in the 1970s, 1980s, and 1990s.

  7. Improved design for a low temperature scanning tunneling microscope with an in situ tip treatment stage.

    PubMed

    Kim, J-J; Joo, S H; Lee, K S; Yoo, J H; Park, M S; Kwak, J S; Lee, Jinho

    2017-04-01

    The Low Temperature Scanning Tunneling Microscope (LT-STM) is an extremely valuable tool not only in surface science but also in condensed matter physics. For years, numerous new ideas have been adopted to perfect LT-STM performances-Ultra-Low Vibration (ULV) laboratory and the rigid STM head design are among them. Here, we present three improvements for the design of the ULV laboratory and the LT-STM: tip treatment stage, sample cleaving stage, and vibration isolation system. The improved tip treatment stage enables us to perform field emission for the purpose of tip treatment in situ without exchanging samples, while our enhanced sample cleaving stage allows us to cleave samples at low temperature in a vacuum without optical access by a simple pressing motion. Our newly designed vibration isolation system provides efficient space usage while maintaining vibration isolation capability. These improvements enhance the quality of spectroscopic imaging experiments that can last for many days and provide increased data yield, which we expect can be indispensable elements in future LT-STM designs.

  8. A comparison of ISCCP land surface temperature with other satellite and in situ observations

    NASA Astrophysics Data System (ADS)

    JiméNez, Carlos; Prigent, Catherine; Catherinot, Julie; Rossow, William; Liang, Pan; Moncet, Jean-Luc

    2012-04-01

    Land surface skin temperature (LST) estimates from the International Satellite Cloud Climatology Project (ISCCP) are compared with estimates from the satellite instruments AIRS and MODIS, and in situ observations from CEOP. ISCCP has generally slightly warmer nighttime LSTs compared with AIRS and MODIS (global) and CEOP (at specific sites). Differences are smaller than 2K, similar to other reported biases between satellite estimates. Larger differences are found in the day-time LSTs, especially for those regions where large LST values occur. Inspection of the AIRS and ISCCP brightness temperatures at the top of the atmosphere (TOA-BT) reveals that where the LSTs differ so too do the TOA-BT values. Area-averaged day-time TOA-BT values can differ as much as 5K in very dry regions. This could be related to differences in sensor calibration, but also to the large LST gradients at the AIRS mid-day overpass that likely amplify the impact of sensor mismatches. Part of the studied LST differences are also explained by discrepancies in the AIRS and ISCCP characterization of the surface (emissivity) and the atmosphere (water vapor). ISCCP calibration procedures are currently being revised to account better for sensor spectral response differences, and alternative atmospheric and surface data sets are being tested as part of a complete ISCCP reprocessing. This is expected to result in an improved ISCCP LST record.

  9. Improved design for a low temperature scanning tunneling microscope with an in situ tip treatment stage

    NASA Astrophysics Data System (ADS)

    Kim, J.-J.; Joo, S. H.; Lee, K. S.; Yoo, J. H.; Park, M. S.; Kwak, J. S.; Lee, Jinho

    2017-04-01

    The Low Temperature Scanning Tunneling Microscope (LT-STM) is an extremely valuable tool not only in surface science but also in condensed matter physics. For years, numerous new ideas have been adopted to perfect LT-STM performances—Ultra-Low Vibration (ULV) laboratory and the rigid STM head design are among them. Here, we present three improvements for the design of the ULV laboratory and the LT-STM: tip treatment stage, sample cleaving stage, and vibration isolation system. The improved tip treatment stage enables us to perform field emission for the purpose of tip treatment in situ without exchanging samples, while our enhanced sample cleaving stage allows us to cleave samples at low temperature in a vacuum without optical access by a simple pressing motion. Our newly designed vibration isolation system provides efficient space usage while maintaining vibration isolation capability. These improvements enhance the quality of spectroscopic imaging experiments that can last for many days and provide increased data yield, which we expect can be indispensable elements in future LT-STM designs.

  10. In-situ neutron diffraction measurements of temperature and stresses during friction stir welding of 6061-T6 aluminum alloy

    SciTech Connect

    Woo, Wan Chuck; Feng, Zhili; Wang, Xun-Li; Brown, D. W.; Clausen, B; An, Ke; Choo, Hahn; Hubbard, Camden R; David, Stan A

    2007-01-01

    The evolution of temperature and thermal stresses during friction stir welding of Al6061-T6 was investigated by means of in-situ, time-resolved neutron diffraction technique. A method is developed to deconvolute the temperature and stress from the lattice spacing changes measured by neutron diffraction. The deep penetration capability of neutrons made it possible for the first time to obtain the temperature and thermal stresses inside a friction stir weld.

  11. In-situ neutron diffraction measurements of temperature and stresses during friction stir welding of 6061-T6 aluminum alloy

    SciTech Connect

    Feng, Zhili; Wang, Xun-Li; David, Stan A; Choo, Hahn; Hubbard, Camden R; Woo, Wan Chuck; Brown, D. W.; Clausen, B; An, Ke

    2007-01-01

    The evolution of temperature and thermal stresses during friction stir welding of Al6061-T6 was investigated by means of in situ, time resolved neutron diffraction technique. A method was developed to deconvolute the temperature and stress from the lattice spacing changes measured by neutron diffraction. The deep penetration capability of neutrons made it possible for the first time to obtain the temperature and thermal stresses inside a friction stir weld.

  12. High T sub c Y-Ba-Cu-O thin films prepared by in situ low-temperature codeposition of Y, BaF sub 2 , and Cu on. alpha. -Al sub 2 O sub 3 substrates

    SciTech Connect

    Chromik, S.; Hanic, F.; Adam, R.; Jergel, M.; Liday, J.; Benacka, S. )

    1990-05-28

    Thin Y-Ba-CU-O films were prepared {ital in}-{ital situ} by low-temperature codeposition on Al{sub 2}O{sub 3} substrates. The temperatures during preparation did not exceed 600 {degree}C. As a source of Ba the BaF{sub 2} was used. The zero resistance {ital T}{sub {ital c}} values were higher than 84 K, {ital J}{sub {ital c}} =4{times}10{sup 4} A/cm{sup 2} at 4.2 K/OT. The Auger electron spectroscopy analysis has shown almost a homogeneous distribution of the film components throughout the film thickness. X-ray diffraction revealed the presence of unoriented 1-2-3 phase besides BaF{sub 2} and CuO and, one undefined phase, which might be oxyfluoride compound.

  13. Experimental Investigation and High Resolution Simulation of In-Situ Combustion Processes

    SciTech Connect

    Margot Gerritsen; Tony Kovscek

    2008-04-30

    This final technical report describes work performed for the project 'Experimental Investigation and High Resolution Numerical Simulator of In-Situ Combustion Processes', DE-FC26-03NT15405. In summary, this work improved our understanding of in-situ combustion (ISC) process physics and oil recovery. This understanding was translated into improved conceptual models and a suite of software algorithms that extended predictive capabilities. We pursued experimental, theoretical, and numerical tasks during the performance period. The specific project objectives were (i) identification, experimentally, of chemical additives/injectants that improve combustion performance and delineation of the physics of improved performance, (ii) establishment of a benchmark one-dimensional, experimental data set for verification of in-situ combustion dynamics computed by simulators, (iii) develop improved numerical methods that can be used to describe in-situ combustion more accurately, and (iv) to lay the underpinnings of a highly efficient, 3D, in-situ combustion simulator using adaptive mesh refinement techniques and parallelization. We believe that project goals were met and exceeded as discussed.

  14. High pressure rheometer for in situ formation and characterization of methane hydrates

    NASA Astrophysics Data System (ADS)

    Webb, Eric B.; Rensing, Patrick J.; Koh, Carolyn A.; Dendy Sloan, E.; Sum, Amadeu K.; Liberatore, Matthew W.

    2012-01-01

    We present a novel setup for a high pressure rheometer operating with concentric cylinders geometry for in situ studies of hydrate formation and rheological characterization. The apparatus uses an external high pressure mixing cell to saturate water-in-oil emulsions with methane gas. The capability of mixing combined with a true rheometer design make this apparatus unique in terms of setup and sample formation. We have used the apparatus to form gas hydrates in situ from water-in-oil emulsions and characterize suspension rheological properties such as yield stress and shear-thinning behavior.

  15. Highly efficient method towards in situ immobilization of invertase using cryogelation.

    PubMed

    Olcer, Zehra; Ozmen, Mehmet Murat; Sahin, Zeynep M; Yilmaz, Faruk; Tanriseven, Aziz

    2013-12-01

    A novel method was developed for the immobilization of Saccharomyces cerevisiae invertase within supermacroporous polyacrylamide cryogel and was used to produce invert sugar. First, the cross-linking of invertase with soluble polyglutaraldehyde (PGA) was carried out prior to immobilization in order to increase the bulkiness of invertase and thus preventing the leakage of the cross-linked enzyme after immobilization by entrapment. And then, in situ immobilization of PGA cross-linked invertase within cryogel synthesis was achieved by free radical polymerization in semi-frozen state. The method resulted in 100 % immobilization and 74 % activity yields. The immobilized invertase retained all the initial activity for 30 days and 30 batch reactions. Immobilization had no effect on optimum temperature and it was 60 °C for both free and immobilized enzyme. However, optimum pH was affected upon immobilization. Optimum pH values for free and immobilized enzyme were 4.5 and 5.0, respectively. The immobilized enzyme was more stable than the free enzyme at high pH and temperatures. The kinetic parameters for free and immobilized invertase were also determined. The newly developed method is simple yet effective and could be used for the immobilization of some other enzymes and microorganisms.

  16. Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

    SciTech Connect

    Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W.

    2010-07-19

    Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

  17. In meso in situ serial X-ray crystallography of soluble and membrane proteins at cryogenic temperatures.

    PubMed

    Huang, Chia Ying; Olieric, Vincent; Ma, Pikyee; Howe, Nicole; Vogeley, Lutz; Liu, Xiangyu; Warshamanage, Rangana; Weinert, Tobias; Panepucci, Ezequiel; Kobilka, Brian; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2016-01-01

    Here, a method for presenting crystals of soluble and membrane proteins growing in the lipid cubic or sponge phase for in situ diffraction data collection at cryogenic temperatures is introduced. The method dispenses with the need for the technically demanding and inefficient crystal-harvesting step that is an integral part of the lipid cubic phase or in meso method of growing crystals. Crystals are dispersed in a bolus of mesophase sandwiched between thin plastic windows. The bolus contains tens to hundreds of crystals, visible with an in-line microscope at macromolecular crystallography synchrotron beamlines and suitably disposed for conventional or serial crystallographic data collection. Wells containing the crystal-laden boluses are removed individually from hermetically sealed glass plates in which crystallization occurs, affixed to pins on goniometer bases and excess precipitant is removed from around the mesophase. The wells are snap-cooled in liquid nitrogen, stored and shipped in Dewars, and manually or robotically mounted on a goniometer in a cryostream for diffraction data collection at 100 K, as is performed routinely with standard, loop-harvested crystals. The method is a variant on the recently introduced in meso in situ serial crystallography (IMISX) method that enables crystallographic measurements at cryogenic temperatures where crystal lifetimes are enormously enhanced whilst reducing protein consumption dramatically. The new approach has been used to generate high-resolution crystal structures of a G-protein-coupled receptor, α-helical and β-barrel transporters and an enzyme as model integral membrane proteins. Insulin and lysozyme were used as test soluble proteins. The quality of the data that can be generated by this method was attested to by performing sulfur and bromine SAD phasing with two of the test proteins.

  18. In meso in situ serial X-ray crystallography of soluble and membrane proteins at cryogenic temperatures

    PubMed Central

    Huang, Chia-Ying; Olieric, Vincent; Ma, Pikyee; Howe, Nicole; Vogeley, Lutz; Liu, Xiangyu; Warshamanage, Rangana; Weinert, Tobias; Panepucci, Ezequiel; Kobilka, Brian; Diederichs, Kay; Wang, Meitian; Caffrey, Martin

    2016-01-01

    Here, a method for presenting crystals of soluble and membrane proteins growing in the lipid cubic or sponge phase for in situ diffraction data collection at cryogenic temperatures is introduced. The method dispenses with the need for the technically demanding and inefficient crystal-harvesting step that is an integral part of the lipid cubic phase or in meso method of growing crystals. Crystals are dispersed in a bolus of mesophase sandwiched between thin plastic windows. The bolus contains tens to hundreds of crystals, visible with an in-line microscope at macromolecular crystallography synchrotron beamlines and suitably disposed for conventional or serial crystallographic data collection. Wells containing the crystal-laden boluses are removed individually from hermetically sealed glass plates in which crystallization occurs, affixed to pins on goniometer bases and excess precipitant is removed from around the mesophase. The wells are snap-cooled in liquid nitrogen, stored and shipped in Dewars, and manually or robotically mounted on a goniometer in a cryostream for diffraction data collection at 100 K, as is performed routinely with standard, loop-harvested crystals. The method is a variant on the recently introduced in meso in situ serial crystallography (IMISX) method that enables crystallo­graphic measurements at cryogenic temperatures where crystal lifetimes are enormously enhanced whilst reducing protein consumption dramatically. The new approach has been used to generate high-resolution crystal structures of a G-protein-coupled receptor, α-helical and β-barrel transporters and an enzyme as model integral membrane proteins. Insulin and lysozyme were used as test soluble proteins. The quality of the data that can be generated by this method was attested to by performing sulfur and bromine SAD phasing with two of the test proteins. PMID:26894538

  19. In situ ammonia production as a sanitation agent during anaerobic digestion at mesophilic temperature.

    PubMed

    Ottoson, J R; Schnürer, A; Vinnerås, B

    2008-03-01

    To measure the sanitizing effect of mesophilic (37 degrees C) anaerobic digestion in high ammonia concentrations produced in situ. Indicator organisms and salmonella were transferred to small-scale anaerobic batch cultures and D-values were calculated. Batch cultures were started with material from two biogas processes operating at high (46 mmol l(-1)) and low (1.6 mmol l(-1)) ammonia concentration. D-values were shortened from c. 3 days to <1 day for the bacteria. MS2 had the same D-value (1.3 days) independent of ammonia concentration whereas PhiX174 and 28B were faster inactivated in the control (1.1 and 7.9 days) than in the high ammonia (8.9 and 39 days) batch cultures. Running biogas processes at high levels of ammonia shortens the time to meet EU regulation concerning reduction of salmonella and enterococci (5 log). Unless a minimum retention time of 2 days, post-treatment digestion is needed to achieve sufficient sanitation in continuous biogas processes. Running mesophilic biogas processes at high ammonia level produces residue with a high fertilizer value. With some stipulations concerning management parameters, such processes provide a method of bacterial sanitation without preceding pasteurization of the incoming organic waste.

  20. Experimental in situ investigations of turbulence under high pressure.

    PubMed

    Song, Kwonyul; Al-Salaymeh, Ahmed; Jovanovic, Jovan; Rauh, Cornelia; Delgado, Antonio

    2010-02-01

    In tube injection systems applied in high-pressure processing of packed biomaterials and foods, the pressure-transmitting medium is injected into the vessel to increase the pressure up to 1000 MPa, generating a submerged liquid-free jet. The presence of a turbulent-free jet during the pressurization phase and its positive influence on the homogeneity of the product treatment has already been examined by computational fluid dynamics investigations. However, no experimental data have supported the existence and properties of turbulent flow under high-pressure (HP) conditions up to 400 MPa. This contribution presents the development of two experimental setups: HP-laser Doppler anemometry and HP-hot wire anemometry. For the first time the time-averaged velocity profiles of a free jet during pressurization up to 300 MPa at different Reynolds numbers (Re) have been obtained. In this article, the dependence of the velocity profiles on the Re is discussed in detail. Moreover, the relaminarization phenomenon of the turbulent pipe flow most likely caused by the compressibility effects and viscosity changes of the pressure-transmitting medium is examined.

  1. Estimation of soil thermal properties using in-situ temperature measurements in the active layer and permafrost.

    Treesearch

    D.J. Nicolsky; V.E. Romanovsky; G.G. Panteleev

    2008-01-01

    A variational data assimilation algorithm is developed to reconstruct thermal properties, porosity, and parametrization of the unfrozen water content for fully saturated soils. The algorithm is tested with simulated synthetic temperatures. The simulations are performed to determine the robustness and sensitivity of algorithm to estimate soil properties from in-situ...

  2. How rainfall, relative humidity and temperature influence volatile emissions from apple trees in situ.

    PubMed

    Vallat, Armelle; Gu, Hainan; Dorn, Silvia

    2005-07-01

    emissions from apple trees in situ.

  3. High-resolution anatomy from in situ human brain.

    PubMed

    Toga, A W; Ambach, K L; Schluender, S

    1994-11-01

    We have generated a spatially accurate, high-resolution three-dimensional (3D) volume of brain anatomy from cryosectioned whole human head. The head of a female cadaver was cryosectioned on a heavy duty cryomacrotome (PMV, Stockholm Sweden) modified for quantitative digital image capture. Serial images (1024(2), 24-bit) were captured directly from the cryoplaned specimen blockface in 500-micron intervals and reconstructed to a 3D data volume. Data were placed into the Talairach coordinate system to create a volume of brain anatomy for atlas reference. We resampled the volume at 500 microns along the sagittal, coronal, and horizontal planes and enhanced the images by digitally editing the background. The spatial resolution of the original digitized images provided sufficient anatomic detail to clearly delineate gray and white matter and neural structures, including major fiber pathways, subthalamic nuclei, and laminae. We developed a compact disk and controlling software program to enable the viewer to select planes of orientation, display, and copy individual to sections at higher resolution. Animation proved useful in the conveyance of system anatomy as structures are shown traversing through the neuroaxis. Postmortem cryosectioning paired with this computerized presentation allowed the complete 3D volume data to be distributed and shared as an educational, clinical, and research resource.

  4. Novel, high sensitivity and high frequency instruments for in-situ measurements of volcanic gases

    NASA Astrophysics Data System (ADS)

    Burton, Mike; Chiarugi, Antonio; D'Amato, Francesco; Viciani, Silvia; Queisser, Manuel; La Spina, Alessandro

    2017-04-01

    The accurate, precise and traceable measurement of volcanic gas compositions and fluxes is a key pillar upon which our understanding of volcanic processes and geological volatile cycles rests. While enormous progress has been made in the quality and quantity of in-situ gas composition measurements in recent years, the number of instruments which are both field deployable and able to accurately measure magmatic gas compositions remains quite limited. This makes intercomparisons and validations, key activities for any quantitative field study, challenging. Furthermore, the potential of UAV and airborne technology can only be fully realised when we have high frequency measurements of volcanic gases from several gas sensors simultaneously, as gas concentrations can vary quickly during flight, and any frequency response delay between individual gas sensors may introduce significant artifacts in retrieved gas ratios. For these reasons, within the European Research Council project CO2Volc, we have produced and field-tested new, custom-built TDLS- and LED-based in-situ gas sensing systems, capable of measuring H2O, CO2, SO2, HCl and HF at 5-10 Hz and sub-ppm precision for CO2 and SO2, and 50 ppb detection limit for HCl and HF. Here, we report results from the field tests, and examine the potential new applications they offer.

  5. In situ Raman and X-ray spectroscopies to monitor microbial activities under high hydrostatic pressure.

    PubMed

    Oger, Phil M; Daniel, Isabelle; Picard, Aude

    2010-02-01

    Until recently, monitoring of cells and cellular activities at high hydrostatic pressure (HHP) was mainly limited to ex situ observations. Samples were analyzed prior to and following the depressurization step to evaluate the effect of the pressure treatment. Such ex situ measurements have several drawbacks: (i) it does not allow for kinetic measurements and (ii) the depressurization step often leads to artifactual measurements. Here, we describe recent advances in diamond anvil cell (DAC) technology to adapt it to the monitoring of microbial processes in situ. The modified DAC is asymmetrical, with a single anvil and a diamond window to improve imaging quality and signal collection. Using this novel DAC combined to Raman and X-ray spectroscopy, we monitored the metabolism of glucose by baker's yeast and the reduction of selenite by Agrobacterium tumefaciens in situ under HHP. In situ spectroscopy is also a promising tool to study piezophilic microorganisms.

  6. 4-Diamond Formation from Amorphouse Carbon and Graphite in the Presence of COH Fluids : An InSitu High-Pressure and -Temperature Laser-Heated Diamond Anvil Cell Experimental Study

    SciTech Connect

    Zhang, J.; Prakapenka, V.; Kubo, A.; Kavner, A.; Green, H.W.; Dobrzhinetskaya, L.

    2011-10-14

    Microdiamonds from orogenic belts contain nanometer-size fluid inclusions suggesting diamond formation from supercritical carbon - oxygen - hydrogen (COH) fluids. Here we report experimental results of diamond nucleation from amorphous carbon and polycrystalline graphite in the presence of COH fluids in a laser-heated diamond anvil cell. Our results show that: (i) diamonds can nucleate from graphite or amorphous carbon at pressures of 9-11 GPa and temperatures of 1200-1400 K in the presence of COH fluids; (ii) it is easier to nucleate diamond from amorphous carbon than from graphite with or without the COH fluids; and (iii) the fluid from decomposition of glucose is more efficient in promoting the graphite-to-diamond transformation than the fluid from decomposition of oxalic acid dihydrate. Carbon crystallinity has strong effects on the kinetics of diamond nucleation and growth. The experimental results demonstrated the critical role of presence and composition of supercritical COH fluids for promoting the graphite-to-diamond transformation.

  7. In-Situ F2-Region Plasma Density and Temperature Measurements from the International Space Station

    NASA Technical Reports Server (NTRS)

    Coffey, Victoria; Wright, Kenneth; Minow, Joseph

    2008-01-01

    The International Space Station orbit provides an ideal platform for in-situ studies of space weather effects on the mid and low latitude F-2 region ionosphere. The Floating Potential Measurement Unit (FPMU) operating on the ISS since Aug 2006. is a suite of plasma instruments: a Floating Potential Probe (FPP), a Plasma Impedance Probe (PIP), a Wide-sweep langmuir Probe (WLP), and a Narrow-sweep Langmuir Probe (NLP). This instrument package provides a new opportunity lor collaborative multi-instrument studies of the F-region ionosphere during both quiet and disturbed periods. This presentation first describes the operational parameters for each of the FPMU probes and shOWS examples of an intra-instrument validation. We then show comparisons with the plasma density and temperature measurements derived from the TIMED GUVI ultraviolet imager, the Millstone Hill ground based incoherent scatter radar, and DIAS digisondes, Finally we show one of several observations of night-time equatorial density holes demonstrating the capabilities of the probes lor monitoring mid and low latitude plasma processes.

  8. In situ SAXS study on size changes of platinum nanoparticles with temperature

    NASA Astrophysics Data System (ADS)

    Wang, W.; Chen, X.; Cai, Q.; Mo, G.; Jiang, L. S.; Zhang, K.; Chen, Z. J.; Wu, Z. H.; Pan, W.

    2008-09-01

    Poly(vinylpyrrolidone) (PVP)-coated platinum (Pt) nanoparticles were prepared in methanol-water reduction method. In situ small-angle X-ray scattering (SAXS) and X-ray diffraction (XRD) techniques were used to probe the size change of particles and crystallites with temperature. Tangent-by-tangent (TBT) method of SAXS data analysis was improved and used to get the particle size distribution (PSD) from SAXS intensity. Scherrer’s equation was used to derive the crystallite size from XRD pattern. Combining SAXS and XRD results, a step-like characteristic of the Pt nanoparticle growth has been found. Three stages (diffusion, aggregation, and agglomeration) can be used to describe the growth of the Pt nanoparticles and nanocrystallites. Aggregation was found to be the main growth mode of the Pt nanoparticles during heating. The maximum growth rates of Pt nanoparticles and Pt nanocrystallites, as well as the maximum aggregation degree of Pt nanocrystallites were found, respectively, at 250 °C, 350 °C and 300 °C. These results are helpful to understanding the growth mode of nanoparticles, as well as controlling the nanoparticle size.

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

    NASA Astrophysics Data System (ADS)

    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.

  10. Enzymatically degradable temperature-sensitive polypeptide as a new in-situ gelling biomaterial.

    PubMed

    Jeong, Yuri; Joo, Min Kyung; Bahk, Kyung Hyun; Choi, Yun Young; Kim, Ho-Tae; Kim, Won-Ki; Lee, Hwa Jeong; Sohn, Youn Soo; Jeong, Byeongmoon

    2009-07-01

    We are reporting a poly (ethylene glycol)-block-poly(alanine-co-phenyl alanine) (PEG-PAF) aqueous solution that undergoes sol-to-gel transition as the temperature increases. The sol-to-gel transition was observed at as low a concentration as 3.0-7.0 wt.%. Micellar aggregation accompanying small conformational changes of the peptide from random coils to beta-sheets is suggested as the sol-to-gel transition mechanism of the PEG-PAF aqueous solution. The PEG-PAF is stable in phosphate buffered saline, however, it degraded in the subcutaneous layer of rats. In vitro study showed that proteolytic enzymes such as cathepsin B, cathepsin C, and elastase that are present in the subcutaneous layer of the mammalian tissue might be responsible for the degradation of the polymer in rats. As a feasibility study of this material, a single shot of an aqueous insulin formulation (13.8 mg insulin/kg) showed a hypoglycemic effect over 18 days in rats. The current functional polypeptide may be very promising as an in-situ gelling system for tissue engineering, cell/stem cell therapy, and drug delivery.

  11. {ital In situ} growth of highly oriented Pb(Zr{sub 0.5}Ti{sub 0.5})O{sub 3} thin films by low-temperature metal{endash}organic chemical vapor deposition

    SciTech Connect

    Bai, G.; Tsu, I.; Wang, A.; Foster, C.M.; Murray, C.E.; Dravid, V.P.

    1998-03-01

    Highly oriented, polycrystalline Pb(Zr{sub 0.5}Ti{sub 0.5})O{sub 3} (PZT) thin films were successfully grown on RuO{sub 2}/SiO{sub 2}/(001)Si using metal{endash}organic chemical vapor deposition (MOCVD) at 525{degree}C. The orientation of the PZT film was controlled by using MOCVD-deposited highly textured RuO{sub 2} bottom electrodes. A (001)-oriented PZT film was observed for growth on (101)-textured RuO{sub 2}. In contrast, for (110) RuO{sub 2}, the growth of (001) PZT was greatly suppressed while the growth of both (110) and (111) were enhanced, resulting in a poorly (001)-textured polycrystalline film. The as-grown PZT films exhibited a dense columnar microstructure with an average grain size of 150{endash}250 nm. Both PZT films showed excellent ferroelectric properties without any postgrowth annealing. The (001) highly oriented PZT films showed significantly higher values of remnant polarization (P{sub r}=49.7{mu}C/cm{sup 2}) and saturation polarization (P{sub s}=82.5{mu}C/cm{sup 2}). In comparison, for the PZT films grown on (110) RuO{sub 2}, P{sub r} and P{sub s} were 21.5 and 35.4{mu}C/cm{sup 2}, respectively. {copyright} {ital 1998 American Institute of Physics.}

  12. High in situ repeatability of behaviour indicates animal personality in the beadlet anemone Actinia equina (Cnidaria).

    PubMed

    Briffa, Mark; Greenaway, Julie

    2011-01-01

    'Animal personality' means that individuals differ from one another in either single behaviours or suites of related behaviours in a way that is consistent over time. It is usually assumed that such consistent individual differences in behaviour are driven by variation in how individuals respond to information about their environment, rather than by differences in external factors such as variation in microhabitat. Since behavioural variation is ubiquitous in nature we might expect 'animal personality' to be present in diverse taxa, including animals with relatively simple nervous systems. We investigated in situ startle responses in a sea anemone, Actinia equina, to determine whether personalities might be present in this example of an animal with a simple nervous system. We found very high levels of repeatability among individuals that were re-identified in the same locations over a three week sampling period. In a subset of the data, where we used tide-pool temperature measurements to control for a key element of variation in microhabitat, these high levels of repeatability remained. Although a range of other consistent differences in micro-habitat features could have contributed to consistent differences between the behaviour of individuals, these data suggest the presence of animal personality in A. equina. Rather than being restricted to certain groups, personality may be a general feature of animals and may be particularly pronounced in species with simple nervous systems.

  13. High temperature furnace

    DOEpatents

    Borkowski, Casimer J.

    1976-08-03

    A high temperature furnace for use above 2000.degree.C is provided that features fast initial heating and low power consumption at the operating temperature. The cathode is initially heated by joule heating followed by electron emission heating at the operating temperature. The cathode is designed for routine large temperature excursions without being subjected to high thermal stresses. A further characteristic of the device is the elimination of any ceramic components from the high temperature zone of the furnace.

  14. An In-situ Tensile Test Apparatus for Polymers in High Pressure Hydrogen

    SciTech Connect

    Alvine, Kyle J.; Kafentzis, Tyler A.; Pitman, Stan G.; Johnson, Kenneth I.; Skorski, Daniel C.; Tucker, Joseph C.; Roosendaal, Timothy J.; Dahl, Michael E.

    2014-10-10

    Degradation of material properties by high-pressure hydrogen is an important factor in determining the safety and reliability of materials used in high-pressure hydrogen storage and delivery. Hydrogen damage mechanisms have a time dependence that is linked to hydrogen outgassing after exposure to the hydrogen atmosphere that makes ex-situ measurements of mechanical properties problematic. Designing in-situ measurement instruments for high-pressure hydrogen is challenging due to known hydrogen incompatibility with many metals and standard high-power motor materials like Nd. Here we detail the design and operation of a solenoid based in-situ tensile tester under high-pressure hydrogen environments up to 5,000 psi. Modulus data from high-density polyethylene (HDPE) samples tested under high-pressure hydrogen are also reported as compared to baseline measurements taken in air.

  15. An in situ tensile test apparatus for polymers in high pressure hydrogen.

    PubMed

    Alvine, K J; Kafentzis, T A; Pitman, S G; Johnson, K I; Skorski, D; Tucker, J C; Roosendaal, T J; Dahl, M E

    2014-10-01

    Degradation of material properties by high-pressure hydrogen is an important factor in determining the safety and reliability of materials used in high-pressure hydrogen storage and delivery. Hydrogen damage mechanisms have a time dependence that is linked to hydrogen outgassing after exposure to the hydrogen atmosphere that makes ex situ measurements of mechanical properties problematic. Designing in situ measurement instruments for high-pressure hydrogen is challenging due to known hydrogen incompatibility with many metals and standard high-power motor materials such as Nd. Here we detail the design and operation of a solenoid based in situ tensile tester under high-pressure hydrogen environments up to 42 MPa (6000 psi). Modulus data from high-density polyethylene samples tested under high-pressure hydrogen at 35 MPa (5000 psi) are also reported as compared to baseline measurements taken in air.

  16. An in situ tensile test apparatus for polymers in high pressure hydrogen

    SciTech Connect

    Alvine, K. J. Kafentzis, T. A.; Pitman, S. G.; Johnson, K. I.; Skorski, D.; Tucker, J. C.; Roosendaal, T. J.; Dahl, M. E.

    2014-10-15

    Degradation of material properties by high-pressure hydrogen is an important factor in determining the safety and reliability of materials used in high-pressure hydrogen storage and delivery. Hydrogen damage mechanisms have a time dependence that is linked to hydrogen outgassing after exposure to the hydrogen atmosphere that makes ex situ measurements of mechanical properties problematic. Designing in situ measurement instruments for high-pressure hydrogen is challenging due to known hydrogen incompatibility with many metals and standard high-power motor materials such as Nd. Here we detail the design and operation of a solenoid based in situ tensile tester under high-pressure hydrogen environments up to 42 MPa (6000 psi). Modulus data from high-density polyethylene samples tested under high-pressure hydrogen at 35 MPa (5000 psi) are also reported as compared to baseline measurements taken in air.

  17. In Situ Solid-State Reactions Monitored by X-ray Absorption Spectroscopy: Temperature-Induced Proton Transfer Leads to Chemical Shifts.

    PubMed

    Stevens, Joanna S; Walczak, Monika; Jaye, Cherno; Fischer, Daniel A

    2016-10-24

    The dramatic colour and phase alteration with the solid-state, temperature-dependent reaction between squaric acid and 4,4'-bipyridine has been probed in situ with X-ray absorption spectroscopy. The electronic and chemical sensitivity to the local atomic environment through chemical shifts in the near-edge X-ray absorption fine structure (NEXAFS) revealed proton transfer from the acid to the bipyridine base through the change in nitrogen protonation state in the high-temperature form. Direct detection of proton transfer coupled with structural analysis elucidates the nature of the solid-state process, with intermolecular proton transfer occurring along an acid-base chain followed by a domino effect to the subsequent acid-base chains, leading to the rapid migration along the length of the crystal. NEXAFS thereby conveys the ability to monitor the nature of solid-state chemical reactions in situ, without the need for a priori information or long-range order.

  18. An in situ-based analysis of the relationship between land surface "skin" and screen-level air temperatures

    NASA Astrophysics Data System (ADS)

    Good, Elizabeth Jane

    2016-08-01

    This paper presents an analysis of the relationship between land surface temperatures (LST) and screen-level air temperatures (T2m) using in situ observations from 19 Atmospheric Radiation Measurement (ARM) deployments located in a range of geographical regimes. The diurnal cycle is resolved using 1 min observations: a particular focus of the study is on the relationship between daily extremes of LST (LSTmax, LSTmin) and T2m (Tmax, Tmin). Temperature differences are analyzed with respect to cloud, wind speed, and snow cover. Under cloud-free, low wind speed conditions, daytime LST is often several degrees Celsius (°C) higher than T2m at low-to-middle latitudes and at high latitudes during the summer months. In contrast, LST and T2m are often close (e.g., within 2°C) under cloudy and/or moderate-to-high wind speed conditions or when solar insolation is low or absent. LSTmin and Tmin are generally well correlated (r > 0.8, often r > 0.9), while seasonal correlations between LSTmax and Tmax are weaker (r > 0.6, often r > 0.8). At high latitudes, LST and T2m are well coupled in spring/autumn/winter; the relationship between LST and T2m tends to weaken with decreasing latitude. The timing of daily extremes is also investigated and it is found that LSTmin and Tmin typically occur close to sunrise, with Tmin occurring slightly after LSTmin. LSTmax occurs close to solar noon, with Tmax typically occurring 1-3 hours later. This study will inform temperature data users on differences between LST and T2m and aid development of methods to estimate T2m using satellite LSTs.

  19. Esimation of field-scale thermal conductivities of unsaturatedrocks from in-situ temperature data

    SciTech Connect

    Mukhopadhyay, Sumit; Tsang, Yvonne W.; Birkholzer, Jens T.

    2006-06-26

    A general approach is presented here which allows estimationof field-scale thermal properties of unsaturated rock using temperaturedata collected from in situ heater tests. The approach developed here isused to determine the thermal conductivities of the unsaturated host rockof the Drift Scale Test (DST) at Yucca Mountain, Nevada. The DST wasdesigned to obtain thermal, hydrological, mechanical, and chemical (THMC)data in the unsaturated fractured rock of Yucca Mountain. Sophisticatednumerical models have been developed to analyze these THMC data. However,though the objective of those models was to analyze "field-scale" (of theorder of tens-of-meters) THMC data, thermal conductivities measured from"laboratory-scale" core samples have been used as input parameters.While, in the absence of a better alternative, using laboratory-scalethermal conductivity values in field-scale models can be justified, suchapplications introduce uncertainties in the outcome of the models. Thetemperature data collected from the DST provides a unique opportunity toresolve some of these uncertainties. These temperature data can be usedto estimate the thermal conductivity of the DST host rock and, given thelarge volume of rock affected by heating at the DST, such an estimatewill be a more reliable effective thermal conductivity value for fieldscale application. In this paper, thus, temperature data from the DST areused to develop an estimate of the field-scale thermal conductivityvalues of the unsaturated host rock of the DST. An analytical solution isdeveloped for the temperature rise in the host rock of the DST; and usinga nonlinear fitting routine, a best-fit estimate of field-scale thermalconductivity for the DST host rock is obtained. Temperature data from theDST show evidence of two distinct thermal regimes: a zone below boiling(wet) and a zone above boiling (dry). Estimates of thermal conductivityfor both the wet and dry zones are obtained in this paper. Sensitivity ofthese estimates

  20. Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritical conditions

    SciTech Connect

    Diefenbacher, Jason; McKelvy, Michael; Chizmeshya, Andrew V.G.; Wolf, George H.

    2005-01-01

    A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 deg. C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.

  1. Externally controlled pressure and temperature microreactor for in situ x-ray diffraction, visual and spectroscopic reaction investigations under supercritical and subcritial conditions

    SciTech Connect

    Diefenbacher, J.; McKelvy, M.; Chizemeshya, A.V.; Wolf, G.H.

    2010-07-13

    A microreactor has been developed for in situ, spectroscopic investigations of materials and reaction processes with full external pressure and temperature control from ambient conditions to 400 C and 310 bar. The sample chamber is in direct contact with an external manifold, whereby gases, liquids or fluids can be injected and their activities controlled prior to and under investigation conditions. The microreactor employs high strength, single crystal moissanite windows which allow direct probe beam interaction with a sample to investigate in situ reaction processes and other materials properties. The relatively large volume of the cell, along with full optical accessibility and external temperature and pressure control, make this reaction cell well suited for experimental investigations involving any combination of gas, fluid, and solid interactions. The microreactor's capabilities are demonstrated through an in situ x-ray diffraction study of the conversion of a meta-serpentine sample to magnesite under high pressure and temperature. Serpentine is one of the mineral candidates for the implementation of mineral carbonation, an intriguing carbon sequestration candidate technology.

  2. In-situ neutron scattering studies of magnetic shape memory alloys under stress, temperature, and magnetic fields

    SciTech Connect

    Brown, Donald W; Sisneros, Thomas A; Kabra, Saurabh; Schlagel, Deborah

    2010-01-01

    We have utilized the SMARTS engineering neutron diffractometer to study the crystallographic orientation and phase transformations in the ferromagnetic shape memory alloy Ni 2MnGa under conditions of temperature (200-600K), stress (500MPa), and magnetic field (2T). Neutrons are uniquely suited to probe the crystallographic response of materials to external stimuli because of their high penetration, which allows them to sample the bulk of the material (as opposed to the surface) as well as pass through environmental chambers. A single crystal of Ni{sub 5}MnGa was repeatedly thermally cycled through the Austenitic-Martensitic phase transformation under varying conditions of applied stress, magnetic field or both. In-situ neutron diffraction was used to quantitatively monitor the population of the crystallographic variants in the martensitic phase as a function of the external stimuli during cooling. Neutron diffraction was used to monitor variant selection in the Ferromagnetic Shape Memory Alloy Ni{sub 2}Mn Ga during austenitic to martensitic transformation under varying conditions of externally applied stress and magnetic field. Qualitatively, the results were to be expected in this simple example. The shorter and magnetically soft c-axis of the tetragonal martensitic phase aligned with the compressive stress or magnetic field. However, neutron diffraction proved useful in directly quantifying the selection of the preferred variant by external influence. For instance, by quantifying the variant selection, the neutron diffraction results made apparent that the sample 'remembered' a loading cycle following a 'reset' cycle with no external applied stress. Moreover, the power of in-situ neutron diffraction will become more apparent when applied to more complex, less understood, samples such as polycrystalline samples or composite samples.

  3. In Situ 13C NMR at Elevated-Pressures and -Temperatures Investigating the Conversion of CO2 to Magnesium and Calcium Carbonate Minerals

    NASA Astrophysics Data System (ADS)

    Surface, J. A.; Conradi, M. S.; Skemer, P. A.; Hayes, S. E.

    2013-12-01

    We have constructed specialized NMR hardware to conduct in situ elevated-pressure, elevated-temperature 13C NMR studies of unmixed heterogeneous mixtures of solids, liquids, gases, and supercritical fluids. Specifically, our aim is to monitor CO2 uptake in both ultramafic rocks and in more porous geological materials to understand the mechanisms of chemisorption as a function of temperature, pressure and pH. In this in situ NMR probe, we are able to simulate processes at geologically relevant fluid pressures and temperatures, monitoring the kinetics of CO2 conversion to carbonates. The in situ NMR experiments consist of heterogeneous mixtures of rock, salty brine solution, and moderate pressure CO2 gas at elevated temperatures. The purpose of studying these reactions is to determine efficacy of carbonate formation in various geological reservoirs. Via 13C NMR, we have spectroscopically characterized and quantified the conversion of CO2 to magnesium carbonate and calcium carbonate minerals. When CO2 reacts with the calcium or magnesium in a mineral or rock sample, the 13C chemical shift, linewidth, lineshape, and relaxation times change dramatically. This change can be monitored in situ and provide instantaneous and continuous characterization that maps the chemistry that is taking place. For example, on the pathway to MgCO3 formation, there are a number of phases of Mg(OH)x(H2O)y(CO3)z that are apparent via NMR spectroscopy. We will demonstrate that NMR can be used for quantitative characterization of multiple metastable mineral phases in pure forms and in mixtures. Results are confirmed via powder XRD and Raman spectroscopy of aquo- hydro- carbonato- magnesium species and calcium carbonate species. We also have monitored the 13C spectroscopy to analyze the phase of CO2 (liquid, supercritical, or gas) and its conversion into other forms, such as bicarbonate and carbonate species, providing a "window" into the in situ pH of the reacting system. Reference: 'In Situ

  4. Characterization of Cross-Sectioned Gallium Nitride High-Electron-Mobility Transistors with In Situ Biasing

    NASA Astrophysics Data System (ADS)

    Hilton, A. M.; Brown, J. L.; Moore, E. A.; Hoelscher, J. A.; Heller, E. R.; Dorsey, D. L.

    2015-10-01

    AlGaN/GaN high-electron-mobility transistors (HEMTs) were characterized in cross-section by Kelvin probe force microscopy (KPFM) during in situ biasing. The HEMTs used in this study were specially designed to maintain full and representative transistor functionality after cross-sectioning perpendicular to the gate width dimension to expose the active channel from source to drain. A cross-sectioning procedure was established that produces samples with high-quality surfaces and minimal degradation in initial transistor performance. A detailed description of the cross-sectioning procedure is provided. Samples were characterized by KPFM, effectively mapping the surface potential of the device in two-dimensional cross-section, including under metallization layers (i.e., gate, field plates, and ohmic contacts). Under the gate and field plate layers are where electric field, temperature, and temperature gradients are all most commonly predicted to have peak values, and where degradation and failure are most likely, and so this is where direct measurements are most critical. In this work, the surface potential of the operating device was mapped in cross-section by KPFM. Charge redistribution was observed during and after biasing, and the surface potential was seen to decay with time back to the prebias condition. This work is a first step toward directly mapping and localizing the steady-state and transient charge distribution due to point defects (traps) before, during, and after device operation, including normally inaccessible regions such as under metallization layers. Such measurements have not previously been demonstrated for GaN HEMT technology.

  5. Temperature-dependent structure and phase variation of nickel silicide nanowire arrays prepared by in situ silicidation

    SciTech Connect

    Liu, Hailong; She, Guangwei; Mu, Lixuan; Shi, Wensheng

    2012-12-15

    Graphical abstract: Display Omitted Highlight: ► Nickel silicides nanowire arrays prepared by a simple in situ silicidation method. ► Phases of nickel silicides could be varied by tuning the reaction temperature. ► A growth model was proposed for the nickel silicides nanowires. ► Diffusion rates of Ni and Si play a critical role for the phase variation. -- Abstract: In this paper, we report an in situ silicidizing method to prepare nickel silicide nanowire arrays with varied structures and phases. The in situ reaction (silicidation) between Si and NiCl{sub 2} led to conversion of Si nanowires to nickel silicide nanowires. Structures and phases of the obtained nickel silicides could be varied by changing the reaction temperature. At a relatively lower temperature of 700 °C, the products are Si/NiSi core/shell nanowires or NiSi nanowires, depending on the concentration of NiCl{sub 2} solution. At a higher temperature (800 °C and 900 °C), other phases of the nickel silicides, including Ni{sub 2}Si, Ni{sub 31}Si{sub 12}, and NiSi{sub 2}, were obtained. It is proposed that the different diffusion rates of Ni and Si atoms at different temperatures played a critical role in the formation of nickel silicide nanowires with different phases.

  6. What in situ measurements of thermal electrons tell us about electron heating in the high-latitude ionosphere

    NASA Astrophysics Data System (ADS)

    Lund, E. J.; Lessard, M.; Cohen, I. J.; Lynch, K. A.

    2012-12-01

    The transfer of energy from precipitating particles and incoming photons to ionospheric plasma is a key issue in the physics of the high-latitude ionosphere. However, in situ measurements of electron temperature in the ionosphere have historically been difficult to make. Over the past decade, we have flown several rockets equipped with an electron retarding potential analyzer (ERPA), an instrument designed to measure thermal electrons in the ionosphere. These missions include launches into the cusp (SERSIO, SCIFER-2) and nightside aurora (CASCADES-2, ACES, MICA). In the cusp, the soft electron precipitation which is found in regions of ion outflow leads to increases in electron temperature due to energy deposition in the E and lower F region. The electron temperature increase at sounding rocket altitudes (500--1500~km) is delayed by ˜100~s with respect to the precipitation. By contrast, the higher energy of precipitating electrons in the nightside aurora makes them less effective at heating ionospheric electrons at these altitudes, while in downward current regions ionospheric electrons are found to be cooler than in upward current regions. We discuss the implications of these results for the ionospheric ion outflow problem as well as future prospects for in situ electron temperature measurements.

  7. In-situ monitoring of etching of bovine serum albumin using low-temperature atmospheric plasma jet

    NASA Astrophysics Data System (ADS)

    Kousal, J.; Shelemin, A.; Kylián, O.; Slavínská, D.; Biederman, H.

    2017-01-01

    Bio-decontamination of surfaces by means of atmospheric pressure plasma is nowadays extensively studied as it represents promising alternative to commonly used sterilization/decontamination techniques. The non-equilibrium atmospheric pressure plasmas were already reported to be highly effective in removal of a wide range of biological residual from surfaces. Nevertheless the kinetics of removal of biological contamination from surfaces is still not well understood as the majority of performed studies were based on ex-situ evaluation of etching rates, which did not allow investigating details of plasma action on biomolecules. This study therefore presents a real-time, in-situ ellipsometric characterization of removal of bovine serum albumin (BSA) from surfaces by low-temperature atmospheric plasma jet operated in argon. Non-linear and at shorter distances between treated samples and nozzle of the plasma jet also non-monotonic dependence of the removal rate on the treatment duration was observed. According to additional measurements focused on the determination of chemical changes of treated BSA as well as temperature measurements, the observed behavior is most likely connected with two opposing effects: the formation of a thin layer on the top of BSA deposit enriched in inorganic compounds, whose presence causes a gradual decrease of removal efficiency, and slight heating of BSA that facilitates its degradation and volatilization induced by chemically active radicals produced by the plasma.

  8. In-situ neutron diffraction study of cathode/electrolyte interactions under electrical load and elevated temperature

    NASA Astrophysics Data System (ADS)

    Tonus, F.; Skinner, S. J.

    2016-05-01

    Fuel cells are proposed as a future energy conversion technology that will reduce greenhouse gas emissions at the point of operation due to their ability to produce electrical energy from non-hydrocarbon fuel sources. The Solid Oxide Fuel Cell (SOFC) is amongst the most efficient fuel cell types, however, due to the high cell operating temperature cation diffusion occurs between the different components of the cell, resulting in rapid degradation of the power output. In this paper we investigate cation migration between the promising intermediate temperature-SOFC cathode La1-xSrxCo1-yFeyO3-δ (LSCF) and a fluorite type electrolyte Ce1-xPrxO2-δ (CPO). The crystallographic structure evolution and degradation of the materials were studied by neutron diffraction in-situ under pseudo-operating conditions, i.e. at 600 °C under air and under electrical polarisation. The lattice parameter and cation occupancy evolution were analysed by Rietveld refinement as a function of time and applied potential. The materials were found to be stable, as no impurity formation, lattice parameter or site occupancy evolution was observed during the experiment. However La migration prior to the experiment from LSCF to CPO was observed as well as B-site vacancies in LSCF.

  9. A Low-Power and In Situ Annealing Mitigation Technique for Fast Neutrons Irradiation of Integrated Temperature Sensing Diodes

    SciTech Connect

    Francis, Laurent A.; Andre, Nicolas; Gerard, Pierre; Flandre, Denis; Ali, S. Zeeshan; Udrea, Florin

    2015-07-01

    High doses of fast neutrons is detrimental to the performance of most common solid-state devices such as diodes and transistors. The ionizing effect is observed in particular for diodes used as simple integrated temperature sensors, or thermo-diodes, when their junction voltage is measured at constant current bias. In this work, we present a low-power and in situ mitigation technique based on Silicon-on-Insulator (SOI) micro-hot-plates to recover thermo-diodes. The basic operating principle consists in annealing the temperature-sensitive diodes integrated on the membrane during or after their irradiation in order to restore similar sensing characteristics over time. We measured thermo-diodes integrated to micro-hot-plates during their irradiation by fast neutrons (23 MeV peak) with total doses about 2.97±0.08 kGy. The membrane annealing is taking place at 450 deg. C using 40 mW of electrical power. Thanks to the annealing, the diode keeps a total measurement error below 0.5 deg. C. In this harsh radiation environment and beside the good tolerance of the thermo-diodes and the membrane materials to the total ionizing dose, the thermo-diode located on the heating membrane keeps a constant sensitivity. The demonstrated resistance of micro-hot-plates and the integrated thermo-diodes to fast neutron radiations can extend their use in nuclear plants and for radiation detectors. (authors)

  10. In-Situ Measurement of Internal Temperature Distribution of Sintered Materials Using Ultrasonic Technique

    NASA Astrophysics Data System (ADS)

    Ihara, I.; Tomomatsu, T.

    2011-03-01

    It is often required to measure internal temperature distribution of a heated material because it is closely related to the materials properties and behavior. In this work, an effective ultrasonic method has been applied to the monitoring of internal temperature distributions of an alumina being heated. The principle of the method is based on the temperature dependence of the velocity of ultrasound propagating through a heated material. In the method, a combined technique of ultrasonic pulse-echo measurements and a finite difference calculation is employed to determine the one-dimensional temperature distribution in a heated material. Shear wave is used for the ultrasonic measurements to improve the accuracy in determining temperature. To verify the feasibility of the method, pulse-echo measurements with a shear wave transducer have been performed for an alumina rod of 14 mm diameter and 25 mm length whose single-end is being heated. The internal temperature distribution and its variation of the alumina are then measured during the heating. The temperature distributions determined by the ultrasonic method almost agree with those obtained by an infrared method. Thus, it is demonstrated that the ultrasonic method has the potential for in-process monitoring of the transient temperature variation of ceramics being processed at high temperatures.

  11. In situ high-resolution transmission electron microscopy synthesis observation of nanostructured carbon coated LiFePO 4

    NASA Astrophysics Data System (ADS)

    Trudeau, M. L.; Laul, D.; Veillette, R.; Serventi, A. M.; Mauger, A.; Julien, C. M.; Zaghib, K.

    In situ high-resolution transmission electron microscopy (HRTEM) studies of the structural transformations that occur during the synthesis of carbon-coated LiFePO 4 (C-LiFePO 4) and heat treatment to elevated temperatures were conducted in two different electron microscopes. Both microscopes have sample holders that are capable of heating up to 1500 °C, with one working under high vacuum and the other capable of operating with the sample surrounded by a low gaseous environment. The C-LiFePO 4 samples were prepared using three different compositions of precursor materials with Fe(0), Fe(II) or Fe(III), a Li-containing salt and a polyethylene- block-poly(ethylene glycol)-50% ethylene oxide or lactose. The in situ TEM studies suggest that low-cost Fe(0) and a low-cost carbon-containing compound such as lactose are very attractive precursors for mass production of C-LiFePO 4, and that 700 °C is the optimum synthesis temperature. At temperatures higher than 800 °C, LiFePO 4 has a tendency to decompose. The same in situ measurements have been made on particles without carbon coat. The results show that the homogeneous deposit of the carbon deposit at 700 °C is the result of the annealing that cures the disorder of the surface layer of bare LiFePO 4. Electrochemical tests supported the conclusion that the C-LiFePO 4 derived from Fe(0) is the most attractive for mass production.

  12. Temperature monitoring along the Rhine River based on airborne thermal infrared remote sensing: qualitative results compared to satellite data and validation with in situ measurements

    NASA Astrophysics Data System (ADS)

    Fricke, Katharina; Baschek, Björn

    2014-10-01

    Water temperature is an important parameter of water quality and influences other physical and chemical parameters. It also directly influences the survival and growth of animal and plant species in river ecosystems. In situ measurements do not allow for a total spatial coverage of water bodies and rivers that is necessary for monitoring and research at the Federal Institute of Hydrology (BfG), Germany. Hence, the ability of different remote sensing products to identify and investigate water inflows and water temperatures in Federal waterways is evaluated within the research project 'Remote sensing of water surface temperature'. The research area for a case study is the Upper and Middle Rhine River from the barrage in Iffezheim to Koblenz. Satellite products (e. g. Landsat and ASTER imagery) can only be used for rivers at least twice as wide as the spatial resolution of the satellite images. They can help to identify different water bodies only at tributaries with larger inflow volume (Main and Mosel) or larger temperature differences between the inflow (e. g. from power plants working with high capacity) and the river water. To identify and investigate also smaller water inflows and temperature differences, thermal data with better ground and thermal resolution is required. An aerial survey of the research area was conducted in late October 2013. Data of the surface was acquired with two camera systems, a digital camera with R, G, B, and Near-IR channels, and a thermal imaging camera measuring the brightness temperature in the 8-12 m wavelength region (TIR). The resolution of the TIR camera allowed for a ground resolution of 4 m, covering the whole width of the main stream and larger branches. The RGB and NIR data allowed to eliminate land surface temperatures from the analysis and to identify clouds and shadows present during the data acquisition. By degrading the spatial resolution and adding sensor noise, artificial Landsat ETM+ and TIRS datasets were created

  13. In situ high-pressure study of FeP: Implications for planetary cores

    NASA Astrophysics Data System (ADS)

    Gu, Tingting; Wu, Xiang; Qin, Shan; Dubrovinsky, Leonid

    2011-02-01

    FeP with MnP-type structure is isostructural with high-pressure FeS polymorphs (both post-troilite FeS and FeS VI), which are believed to exist in planetary cores. Due to similar PTX phase diagrams of binary Fe-P and Fe-S, phosphorus can incorporate with iron-sulfur at planetary core conditions. To understand such substitution and the high-pressure behavior of FeP, we investigate the structural stability of FeP up to 15.6 GPa and 1800 ± 200 K by combined in situ powder X-ray diffraction and Mössbauer spectroscopy. Our experimental results show that FeP remains the MnP-type structure throughout the PT range covered. Isothermal equation of state of FeP is obtained with V0 of 92.91(8) Å 3, B0 of 205(7) GPa, and B0 of 4. The shortest axis of the MnP-type FeP cell, the b-axis, is the most compressible, due to the soft edge-sharing octahedra along the b-axis. Mössbauer results show that no electronic structure changes occur up to 15.6 GPa, but indicate decreasing distortion of FeP 6 octahedron with pressure increasing. The behavior of FeP is quite different from that of FeS under high pressure and high temperature, suggesting that phosphorus will have a significant impact on stability and electronic properties of FeS within terrestrial planet cores.

  14. High temperature reactors

    NASA Astrophysics Data System (ADS)

    Dulera, I. V.; Sinha, R. K.

    2008-12-01

    With the advent of high temperature reactors, nuclear energy, in addition to producing electricity, has shown enormous potential for the production of alternate transport energy carrier such as hydrogen. High efficiency hydrogen production processes need process heat at temperatures around 1173-1223 K. Bhabha Atomic Research Centre (BARC), is currently developing concepts of high temperature reactors capable of supplying process heat around 1273 K. These reactors would provide energy to facilitate combined production of hydrogen, electricity, and drinking water. Compact high temperature reactor is being developed as a technology demonstrator for associated technologies. Design has been also initiated for a 600 MWth innovative high temperature reactor. High temperature reactor development programme has opened new avenues for research in areas like advanced nuclear fuels, high temperature and corrosion resistant materials and protective coatings, heavy liquid metal coolant technologies, etc. The paper highlights design of these reactors and their material related requirements.

  15. The high - low-p clinoenstatite transition: in situ xrd and ultrasonic study

    NASA Astrophysics Data System (ADS)

    Müller, H. J.; Wunder, B.; Lathe, C.; Schilling, F. R.

    2003-04-01

    Using single-crystal X-ray diffraction analyses in a diamond anvil cell Angel et al. (1992) published the transformation of MgSiO_3 from LCEn to a C2/c-polymorph (HCEn) at around 5.5 - 8.0 GPa and room-T (RT)conditions. This LCEn - HCEn-transition is not quenchable. However, the knowledge of the exact phase boundary positions for the MgSiO_3-transitions is essential as pyroxene is an important component of the Earth's mantle and will significantly influence elastic properties (e.g. v_p, v_s) of the mantle. We determined the HCEn - LCEn-transition by in-situ XRD experiments under high P, T using the multi-anvil appar atus MAX80 at the synchrotron facility HASYLAB, Hamburg. Our preliminary results only represent the minimum P-conditions of the HCEn - LCEn phase boundary, which is approximated by equation P (GPa) = 0.0021T (/C) + 6.06. Nevertheless, our results are in good agreement to data published by Angel & Hugh-Jones (1994). The invariant point defined by the intersection of the HCEn - LCEn equilibrium determined within this study and the OEn - LCEn reaction after Angel &Hugh-Jones (1994) lies at about 7.9 GPa and 875/C. This is in contrast to earlier experimental results of Kanzaki (1991) and Ulmer &Stalder (2001). The samples for the ultrasonic interferometry experiments were prepared by hot-isostatic pressing also using the MAX80. Adjacent XRD ruled out any phase transition during the hip-process. For the ultrasonic measurements one of the six anvils of MAX80 were exchanged by an anvil equipped with lithium niobate p- and s-wave transducers of 33.3 MHz natural frequency (Mueller et al., 2002). Corresponding to the XRD experiments HCEn was formed by increasing the pressure at RT. The velocities of elastic compressional and shear waves were measured under in situ conditions using the classical digital sweep technique. After the phase transition to LCEn as a result of rising the temperature at given pressure the measurements were repeated. The newly developed

  16. High temperature superconductors

    NASA Technical Reports Server (NTRS)

    Wu, Maw-Kuen

    1987-01-01

    The two principle objectives are to develop materials that superconduct at higher temperatures and to better understand the mechanisms behind high temperature superconductivity. Experiments on the thermal reaction, structure, and physical properties of materials that exhibit superconductivity at high temperatures are discussed.

  17. High temperature sensor

    DOEpatents

    Tokarz, Richard D.

    1982-01-01

    A high temperature sensor includes a pair of electrical conductors separated by a mass of electrical insulating material. The insulating material has a measurable resistivity within the sensor that changes in relation to the temperature of the insulating material within a high temperature range (1,000 to 2,000 K.). When required, the sensor can be encased within a ceramic protective coating.

  18. Using High-Resolution Hand-Held Radiometers To Measure In-Situ Thermal Resistance

    NASA Astrophysics Data System (ADS)

    Burch, Douglas M.; Krintz, Donald F.

    1984-03-01

    A field study was carried out to investigate the accuracy of using high-resolution radiometers to determine the in situ thermal resistance of building components having conventional residential construction. Two different types of radiometers were used to determine the thermal resistances of the walls of six test buildings located at the National Bureau of Standards. These radiometer thermal resistance measurements were compared to reference thermal resistance values determined from steady-state series resistance predictions, time-averaged heat-flow-sensor measurements, and guarded-hot-box measurements. When measurements were carried out 5 hours after sunset when the outdoor temperature was relatively steady and the heating plant was operated in a typical cyclic fashion, the following results were obtained: for lightweight wood-frame cavity walls, the radiometer procedures were found to distinguish wall thermal resistance 4.4 h.ft2- °F/Btu (0.77 m2•K/W) systematically higher than corresponding reference values. Such a discrimination will per-mit insulated and uninsulated walls to be distinguished. However, in the case of walls having large heat capacity (e.g., masonry and log), thermal storage effects produced large time lags between the outdoor diurnal temperature variation and the heat-flow response at the inside surface. This phenomenon caused radiometer thermal resistances to deviate substantially from corresponding reference values. This study recommends that the ANSI/ASHRAE Standard 101-1981 be modified requiring the heating plant to be operated in a typical cyclic fashion instead of being turned off prior to and during radiometer measurements.

  19. The dual temperature/pH-sensitive multiphase behavior of poly(N-isopropylacrylamide-co-acrylic acid) microgels for potential application in in situ gelling system.

    PubMed

    Xiong, Wei; Gao, Xiang; Zhao, Yanbing; Xu, Huibi; Yang, Xiangliang

    2011-05-01

    Poly(N-isopropylacrylamide-co-acrylic acid) microgels (PNA) may be an excellent formulation for in situ gelling system due to their high sensitivity and fast response rate. Four monodispersed PNA microgels with various contents of acrylic acid (AA) were synthesized by emulsion polymerization in this paper. Their hydrodynamic diameters decreased reversibly with both decreasing pH and increasing temperature. The dual temperature/pH-sensitivity was influenced by many factors such as AA content, cross-link density and ion strength. In addition, high concentration PNA dispersions underwent multiple phase transition according to different temperatures, pHs and concentrations, which were summarized in a 3D sol-gel phase diagram in this study. According to the sol-gel phase transition, 8% PNA-025 dispersion maintained a relatively low viscosity and favorable fluidity at pH 5.0 in the temperature range of 25-40°C, but it rapidly increased in viscosity at pH 7.4 and gelled at 37°C. This feature enabled the dual temperature/pH-sensitive microgels to overcome the troubles in syringing of temperature sensitive materials during the injection. Apart from this, PNA could form gel well in in vitro (e.g., medium and serum) and in in vivo with low cytotoxicity. Therefore, it is promising for PNA to be applied in the in situ gelling system.

  20. Methane-based in situ temperature rise measurement in a diode-pumped rubidium laser.

    PubMed

    Wang, Rui; Yang, Zining; Wang, Hongyan; Xu, Xiaojun

    2017-02-15

    We measured active zone temperature rise of an operational diode-pumped rubidium laser non-perturbatively with methane-based near-infrared tunable diode laser spectroscopy (TDLAS). For a Rb+ methane diode-pumped alkali laser (DPAL), the temperature rise was obtained. Especially, the temperature differences (∼10  K) between lasing and un-lasing cases were well identified, which demonstrated a high sensitivity of the method. To our knowledge, this is the first demonstration of extending the methane-based TDLAS method to DPAL study.

  1. High resolution transmission electron microscopic in-situ observations of plastic deformation of compressed nanocrystalline gold

    SciTech Connect

    Wang, Guoyong; Lian, Jianshe; Jiang, Qing; Sun, Sheng; Zhang, Tong-Yi

    2014-09-14

    Nanocrystalline (nc) metals possess extremely high strength, while their capability to deform plastically has been debated for decades. Low ductility has hitherto been considered an intrinsic behavior for most nc metals, due to the lack of five independent slip systems actively operating during deformation in each nanograin. Here we report in situ high resolution transmission electron microscopic (HRTEM) observations of deformation process of nc gold under compression, showing the excellent ductility of individual and aggregate nanograins. Compression causes permanent change in the profile of individual nanograins, which is mediated by dislocation slip and grain rotation. The high rate of grain boundary sliding and large extent of widely exited grain rotation may meet the boundary compatibility requirements during plastic deformation. The in situ HRTEM observations suggest that nc gold is not intrinsically brittle under compressive loading.

  2. In situ temperature control and measurement with femtosecond optical tweezers: offering biomedical application

    NASA Astrophysics Data System (ADS)

    Mondal, Dipankar; Goswami, Debabrata

    2017-02-01

    We present here the control and measurement of temperature rise using femtosecond optical tweezers at near infrared (NIR) region. Based on our theoretical development, we have designed our experimental techniques. The high temporal sensitivity of position autocorrelation and equipartition theorem is simultaneously applied to elucidate temperature control and high precision measurement around focal volume. Experimentally we have made the benign NIR wavelength to induce local heating by adding very low fluorescent dye molecule with low average power. Local temperature control in aqueous solution exciting within optically absorbing window of the low quantum yield molecules can be possible due to non-radiative relaxation via thermal emission. The stochastic nature of Brownian particle has enough information of its surroundings. We have mapped the nano-dimension beam waist environment by probing the fluctuation of trapped particle. We have observed up to 30K temperature rise from room temperature at sub micro molar concentration. The gradient of temperature is as sharp as the fluence of pulsed laser focused by high numerical aperture objective. Thus, pulsed laser radiation always allows finer surgical techniques involving minimal thermal injuries. Our new techniques with multiphoton absorbing non-fluorescent dye can further be used to selective phototherapeutic diagnosis of cancer cells due to peak power dependent nonlinear phenomenon (NLO).

  3. Microbial diversity in long-term water-flooded oil reservoirs with different in situ temperatures in China.

    PubMed

    Zhang, Fan; She, Yue-Hui; Chai, Lu-Jun; Banat, Ibrahim M; Zhang, Xiao-Tao; Shu, Fu-Chang; Wang, Zheng-Liang; Yu, Long-Jiang; Hou, Du-Jie

    2012-01-01

    Water-flooded oil reservoirs have specific ecological environments due to continual water injection and oil production and water recycling. Using 16S rRNA gene clone library analysis, the microbial communities present in injected waters and produced waters from four typical water-flooded oil reservoirs with different in situ temperatures of 25 °C, 40 °C, 55 °C and 70 °C were examined. The results obtained showed that the higher the in situ temperatures of the oil reservoirs is, the less the effects of microorganisms in the injected waters on microbial community compositions in the produced waters is. In addition, microbes inhabiting in the produced waters of the four water-flooded oil reservoirs were varied but all dominated by Proteobacteria. Moreover, most of the detected microbes were not identified as indigenous. The objective of this study was to expand the pictures of the microbial ecosystem of water-flooded oil reservoirs.

  4. The difference between laboratory and in-situ pixel-averaged emissivity: The effects on temperature-emissivity separation

    NASA Technical Reports Server (NTRS)

    Matsunaga, Tsuneo

    1993-01-01

    Advanced Spaceborne Thermal Emission and Reflection Radiometer (ASTER) is a Japanese future imaging sensor which has five channels in thermal infrared (TIR) region. To extract spectral emissivity information from ASTER and/or TIMS data, various temperature-emissivity (T-E) separation methods have been developed to date. Most of them require assumptions on surface emissivity, in which emissivity measured in a laboratory is often used instead of in-situ pixel-averaged emissivity. But if these two emissivities are different, accuracies of separated emissivity and surface temperature are reduced. In this study, the difference between laboratory and in-situ pixel-averaged emissivity and its effect on T-E separation are discussed. TIMS data of an area containing both rocks and vegetation were also processed to retrieve emissivity spectra using two T-E separation methods.

  5. Fitting of satellite and in-situ ocean surface temperatures Results for polymode during the winter of 1977-1978

    NASA Technical Reports Server (NTRS)

    Maul, G. A.; Bravo, N. J.

    1983-01-01

    For the period considered, December 1977 through February 1978, bivariate Gaussian discriminant function cloud identification revealed that more than 93 percent of the 8-km resolution GOES infrared pixels were cloud contaminated. Cloud-free in-situ calibration points were distributed in nonrandom groups; this resulted in systematic errors when using least squares techniques. Surfaces and regression lines were least squares fitted between satellite and in-situ data; use was also made of differences and ratios. The best results were achieved with a regression in the form of the infrared radiative transfer equation; but this was no better than + or - 0.9 K. Because of extensive cloudiness, the linear regressions were seldom useful, and temperature ratios with + or - 1.3 K experimental errors best represent the applicability of GEOS data to sea surface temperatures.

  6. First results from the in-situ temperature measurements by the newly developed downhole tool during the drilling cruise in the hydrothermal fields of the mid-Okinawa Trough

    NASA Astrophysics Data System (ADS)

    Kitada, K.; Wu, H. Y.; Miyazaki, J.; Akiyama, K.; Nozaki, T.; Ishibashi, J. I.; Kumagai, H.; Maeda, L.

    2016-12-01

    The Okinawa trough is an active backarc basin behind the Ryukyu subduction zone and exhibits active rifting associated with extension of the continental margin. The temperature measurement in this area is essential for understanding hydrothermal system and hydraulic structure. During the CK16-01 cruise this March, we have conducted the in-situ temperature measurements by the newly developed downhole tool, TRDT (Thermo-Resistant Downhole Thermometer) in hydrothermal fields of the mid-Okinawa Trough. The purpose of this measurement is to investigate the in-situ temperature structure in deep-hot zones and its variation after coring and/or drilling. TRDT was designed by JAMSTEC as a memory downhole tool to measure in-situ borehole temperature under the extreme high temperature environment. First trial was conducted in the CK14-04 cruise by the free fall deployment to reduce the operation time. However, there was no temperature data recorded due to the strong vibration during the operation. After CK14-04 cruise, TRDT was modified to improve the function against vibration and shock. The improved TRDT passed the high temperature, vibration and shock tests to ensure the data acquisition of borehole logging. During the CK16-01 cruise, we have first successfully collected the in-situ temperature data from hydrothermal borehole in the Iheya North Knoll with wireline system. The temperature at depth of 187mbsf continued to increase almost linearly from 220 to 245°C during the 20 minute measurements time. This suggests that the inside borehole was cooled down by pumping seawater through drill pipes during the coring and lowering down the TRDT tool to the bottom hole. The in-situ temperature were extrapolated with exponential curve using nonlinear least squares fitting and the estimated equilibrium temperature was 278°C. To recover the in-situ temperature more precisely, the measurement time should kept as long as possible by considering the temperature rating. The operational

  7. A Novel Method for In-Situ Monitoring of Local Voltage, Temperature and Humidity Distributions in Fuel Cells Using Flexible Multi-Functional Micro Sensors

    PubMed Central

    Lee, Chi-Yuan; Fan, Wei-Yuan; Chang, Chih-Ping

    2011-01-01

    In this investigation, micro voltage, temperature and humidity sensors were fabricated and integrated for the first time on a stainless steel foil using micro-electro-mechanical systems (MEMS). These flexible multi-functional micro sensors have the advantages of high temperature resistance, flexibility, smallness, high sensitivity and precision of location. They were embedded in a proton exchange membrane fuel cell (PEMFC) and used to simultaneously measure variations in the inner voltage, temperature and humidity. The accuracy and reproducibility of the calibrated results obtained using the proposed micro sensors is excellent. The experimental results indicate that, at high current density and 100%RH or 75%RH, the relative humidity midstream and downstream saturates due to severe flooding. The performance of the PEM fuel cell can be stabilized using home-made flexible multi-functional micro sensors by the in-situ monitoring of local voltage, temperature and humidity distributions within it. PMID:22319361

  8. A novel method for in-situ monitoring of local voltage, temperature and humidity distributions in fuel cells using flexible multi-functional micro sensors.

    PubMed

    Lee, Chi-Yuan; Fan, Wei-Yuan; Chang, Chih-Ping

    2011-01-01

    In this investigation, micro voltage, temperature and humidity sensors were fabricated and integrated for the first time on a stainless steel foil using micro-electro-mechanical systems (MEMS). These flexible multi-functional micro sensors have the advantages of high temperature resistance, flexibility, smallness, high sensitivity and precision of location. They were embedded in a proton exchange membrane fuel cell (PEMFC) and used to simultaneously measure variations in the inner voltage, temperature and humidity. The accuracy and reproducibility of the calibrated results obtained using the proposed micro sensors is excellent. The experimental results indicate that, at high current density and 100%RH or 75%RH, the relative humidity midstream and downstream saturates due to severe flooding. The performance of the PEM fuel cell can be stabilized using home-made flexible multi-functional micro sensors by the in-situ monitoring of local voltage, temperature and humidity distributions within it.

  9. A global database of lake surface temperatures collected by in situ and satellite methods from 1985–2009

    PubMed Central

    Sharma, Sapna; Gray, Derek K; Read, Jordan S; O’Reilly, Catherine M; Schneider, Philipp; Qudrat, Anam; Gries, Corinna; Stefanoff, Samantha; Hampton, Stephanie E; Hook, Simon; Lenters, John D; Livingstone, David M; McIntyre, Peter B; Adrian, Rita; Allan, Mathew G; Anneville, Orlane; Arvola, Lauri; Austin, Jay; Bailey, John; Baron, Jill S; Brookes, Justin; Chen, Yuwei; Daly, Robert; Dokulil, Martin; Dong, Bo; Ewing, Kye; de Eyto, Elvira; Hamilton, David; Havens, Karl; Haydon, Shane; Hetzenauer, Harald; Heneberry, Jocelyne; Hetherington, Amy L; Higgins, Scott N; Hixson, Eric; Izmest’eva, Lyubov R; Jones, Benjamin M; Kangur, Külli; Kasprzak, Peter; Köster, Olivier; Kraemer, Benjamin M; Kumagai, Michio; Kuusisto, Esko; Leshkevich, George; May, Linda; MacIntyre, Sally; Müller-Navarra, Dörthe; Naumenko, Mikhail; Noges, Peeter; Noges, Tiina; Niederhauser, Pius; North, Ryan P; Paterson, Andrew M; Plisnier, Pierre-Denis; Rigosi, Anna; Rimmer, Alon; Rogora, Michela; Rudstam, Lars; Rusak, James A; Salmaso, Nico; Samal, Nihar R; Schindler, Daniel E; Schladow, Geoffrey; Schmidt, Silke R; Schultz, Tracey; Silow, Eugene A; Straile, Dietmar; Teubner, Katrin; Verburg, Piet; Voutilainen, Ari; Watkinson, Andrew; Weyhenmeyer, Gesa A; Williamson, Craig E; Woo, Kara H

    2015-01-01

    Global environmental change has influenced lake surface temperatures, a key driver of ecosystem structure and function. Recent studies have suggested significant warming of water temperatures in individual lakes across many different regions around the world. However, the spatial and temporal coherence associated with the magnitude of these trends remains unclear. Thus, a global data set of water temperature is required to understand and synthesize global, long-term trends in surface water temperatures of inland bodies of water. We assembled a database of summer lake surface temperatures for 291 lakes collected in situ and/or by satellites for the period 1985–2009. In addition, corresponding climatic drivers (air temperatures, solar radiation, and cloud cover) and geomorphometric characteristics (latitude, longitude, elevation, lake surface area, maximum depth, mean depth, and volume) that influence lake surface temperatures were compiled for each lake. This unique dataset offers an invaluable baseline perspective on global-scale lake thermal conditions as environmental change continues. PMID:25977814

  10. A global database of lake surface temperatures collected by in situ and satellite methods from 1985–2009

    USGS Publications Warehouse

    Sharma, Sapna; Gray, Derek; Read, Jordan S.; O'Reilly, Catherine; Schneider, Philipp; Qudrat, Anam; Gries, Corinna; Stefanoff, Samantha; Hampton, Stephanie; Hook, Simon; Lenters, John; Livingstone, David M.; McIntyre, Peter B.; Adrian, Rita; Allan, Mathew; Anneville, Orlane; Arvola, Lauri; Austin, Jay; Bailey, John E.; Baron, Jill S.; Brookes, Justin D; Chen, Yuwei; Daly, Robert; Ewing, Kye; de Eyto, Elvira; Dokulil, Martin; Hamilton, David B.; Havens, Karl; Haydon, Shane; Hetzenaeur, Harald; Heneberry, Jocelyn; Hetherington, Amy; Higgins, Scott; Hixson, Eric; Izmest'eva, Lyubov; Jones, Benjamin M.; Kangur, Kulli; Kasprzak, Peter; Kraemer, Benjamin; Kumagai, Michio; Kuusisto, Esko; Leshkevich, George; May, Linda; MacIntyre, Sally; Dörthe Müller-Navarra,; Naumenko, Mikhail; Noges, Peeter; Noges, Tiina; Pius Niederhauser,; North, Ryan P.; Andrew Paterson,; Plisnier, Pierre-Denis; Rigosi, Anna; Rimmer, Alon; Rogora, Michela; Lars Rudstam,; Rusak, James A.; Salmaso, Nico; Samal, Nihar R.; Daniel E. Schindler,; Geoffrey Schladow,; Schmidt, Silke R.; Tracey Schultz,; Silow, Eugene A.; Straile, Dietmar; Teubner, Katrin; Verburg, Piet; Voutilainen, Ari; Watkinson, Andrew; Weyhenmeyer, Gesa A.; Craig E. Williamson,; Kara H. Woo,

    2015-01-01

    Global environmental change has influenced lake surface temperatures, a key driver of ecosystem structure and function. Recent studies have suggested significant warming of water temperatures in individual lakes across many different regions around the world. However, the spatial and temporal coherence associated with the magnitude of these trends remains unclear. Thus, a global data set of water temperature is required to understand and synthesize global, long-term trends in surface water temperatures of inland bodies of water. We assembled a database of summer lake surface temperatures for 291 lakes collected in situ and/or by satellites for the period 1985–2009. In addition, corresponding climatic drivers (air temperatures, solar radiation, and cloud cover) and geomorphometric characteristics (latitude, longitude, elevation, lake surface area, maximum depth, mean depth, and volume) that influence lake surface temperatures were compiled for each lake. This unique dataset offers an invaluable baseline perspective on global-scale lake thermal conditions as environmental change continues.

  11. A global database of lake surface temperatures collected by in situ and satellite methods from 1985-2009

    NASA Astrophysics Data System (ADS)

    Sharma, Sapna; Gray, Derek K.; Read, Jordan S.; O'Reilly, Catherine M.; Schneider, Philipp; Qudrat, Anam; Gries, Corinna; Stefanoff, Samantha; Hampton, Stephanie E.; Hook, Simon; Lenters, John D.; Livingstone, David M.; McIntyre, Peter B.; Adrian, Rita; Allan, Mathew G.; Anneville, Orlane; Arvola, Lauri; Austin, Jay; Bailey, John; Baron, Jill S.; Brookes, Justin; Chen, Yuwei; Daly, Robert; Dokulil, Martin; Dong, Bo; Ewing, Kye; de Eyto, Elvira; Hamilton, David; Havens, Karl; Haydon, Shane; Hetzenauer, Harald; Heneberry, Jocelyne; Hetherington, Amy L.; Higgins, Scott N.; Hixson, Eric; Izmest'Eva, Lyubov R.; Jones, Benjamin M.; Kangur, Külli; Kasprzak, Peter; Köster, Olivier; Kraemer, Benjamin M.; Kumagai, Michio; Kuusisto, Esko; Leshkevich, George; May, Linda; MacIntyre, Sally; Müller-Navarra, Dörthe; Naumenko, Mikhail; Noges, Peeter; Noges, Tiina; Niederhauser, Pius; North, Ryan P.; Paterson, Andrew M.; Plisnier, Pierre-Denis; Rigosi, Anna; Rimmer, Alon; Rogora, Michela; Rudstam, Lars; Rusak, James A.; Salmaso, Nico; Samal, Nihar R.; Schindler, Daniel E.; Schladow, Geoffrey; Schmidt, Silke R.; Schultz, Tracey; Silow, Eugene A.; Straile, Dietmar; Teubner, Katrin; Verburg, Piet; Voutilainen, Ari; Watkinson, Andrew; Weyhenmeyer, Gesa A.; Williamson, Craig E.; Woo, Kara H.

    2015-03-01

    Global environmental change has influenced lake surface temperatures, a key driver of ecosystem structure and function. Recent studies have suggested significant warming of water temperatures in individual lakes across many different regions around the world. However, the spatial and temporal coherence associated with the magnitude of these trends remains unclear. Thus, a global data set of water temperature is required to understand and synthesize global, long-term trends in surface water temperatures of inland bodies of water. We assembled a database of summer lake surface temperatures for 291 lakes collected in situ and/or by satellites for the period 1985-2009. In addition, corresponding climatic drivers (air temperatures, solar radiation, and cloud cover) and geomorphometric characteristics (latitude, longitude, elevation, lake surface area, maximum depth, mean depth, and volume) that influence lake surface temperatures were compiled for each lake. This unique dataset offers an invaluable baseline perspective on global-scale lake thermal conditions as environmental change continues.

  12. A global database of lake surface temperatures collected by in situ and satellite methods from 1985-2009.

    PubMed

    Sharma, Sapna; Gray, Derek K; Read, Jordan S; O'Reilly, Catherine M; Schneider, Philipp; Qudrat, Anam; Gries, Corinna; Stefanoff, Samantha; Hampton, Stephanie E; Hook, Simon; Lenters, John D; Livingstone, David M; McIntyre, Peter B; Adrian, Rita; Allan, Mathew G; Anneville, Orlane; Arvola, Lauri; Austin, Jay; Bailey, John; Baron, Jill S; Brookes, Justin; Chen, Yuwei; Daly, Robert; Dokulil, Martin; Dong, Bo; Ewing, Kye; de Eyto, Elvira; Hamilton, David; Havens, Karl; Haydon, Shane; Hetzenauer, Harald; Heneberry, Jocelyne; Hetherington, Amy L; Higgins, Scott N; Hixson, Eric; Izmest'eva, Lyubov R; Jones, Benjamin M; Kangur, Külli; Kasprzak, Peter; Köster, Olivier; Kraemer, Benjamin M; Kumagai, Michio; Kuusisto, Esko; Leshkevich, George; May, Linda; MacIntyre, Sally; Müller-Navarra, Dörthe; Naumenko, Mikhail; Noges, Peeter; Noges, Tiina; Niederhauser, Pius; North, Ryan P; Paterson, Andrew M; Plisnier, Pierre-Denis; Rigosi, Anna; Rimmer, Alon; Rogora, Michela; Rudstam, Lars; Rusak, James A; Salmaso, Nico; Samal, Nihar R; Schindler, Daniel E; Schladow, Geoffrey; Schmidt, Silke R; Schultz, Tracey; Silow, Eugene A; Straile, Dietmar; Teubner, Katrin; Verburg, Piet; Voutilainen, Ari; Watkinson, Andrew; Weyhenmeyer, Gesa A; Williamson, Craig E; Woo, Kara H

    2015-01-01

    Global environmental change has influenced lake surface temperatures, a key driver of ecosystem structure and function. Recent studies have suggested significant warming of water temperatures in individual lakes across many different regions around the world. However, the spatial and temporal coherence associated with the magnitude of these trends remains unclear. Thus, a global data set of water temperature is required to understand and synthesize global, long-term trends in surface water temperatures of inland bodies of water. We assembled a database of summer lake surface temperatures for 291 lakes collected in situ and/or by satellites for the period 1985-2009. In addition, corresponding climatic drivers (air temperatures, solar radiation, and cloud cover) and geomorphometric characteristics (latitude, longitude, elevation, lake surface area, maximum depth, mean depth, and volume) that influence lake surface temperatures were compiled for each lake. This unique dataset offers an invaluable baseline perspective on global-scale lake thermal conditions as environmental change continues.

  13. Analysis of Lake Level and Temperature Variation in the Great Salt Lake using ICESat, MODIS, and In-Situ Data

    NASA Astrophysics Data System (ADS)

    Arricale, A. J.; Xie, H.; Bolten, J. D.; Zhang, G.

    2011-12-01

    Many of today's lakes are without in-situ gauges to measure lake level or lake water temperature due to their remote locations. Retrieving this data from individual remote lakes and comparing them to each other is important for investigating changes in climate, anthropological activities, or watershed changes in a particular area. However, it is important to first check the reliability of the remote sensing data by investigating lakes that already have in-situ data and comparing both data sets. This study utilizes remote sensing data from the Ice, Cloud, and Land Elevation Satellite (ICESat) and the Moderate Resolution Imaging Spectrometer (MODIS) onboard the Aqua and Terra satellites. Global Land Surface Altimetry Data (GLA14) from ICESat are compared with in-situ lake level measurements for the Great Salt Lake (GSL) from 2003 to 2009 to check the reliability of the instrument. Both data sets revealed a decreasing trend in lake level with an r^2 value of 0.88 between the ICESat and in-situ data. Thermal imagery (8-daily, 1 km resolution) from MODIS included 818 (1028) images from the Aqua (Terra) satellite from 2002 to 2011 (2000 to 2011). These thermal images were used to calculate the surface water temperature (SWT) of the Great Salt Lake north and south of the railroad causeway which divides the lake in half. After analyzing the data it is evident that the shallower north half of the lake has a higher SWT in the summer and cooler SWT in the winter than the south half by 1 C°. The average monthly SWT and in-situ air temperatures for the GSL are compared well (r^2 value of 0.93) and there is a decreasing trend in air temperatures (from 2002 to 2010), resulting in a decreasing SWT trend for both Terra and Aqua data sets. We conclude there is great potential for the use of satellites to measure lake's characteristics that are usually not possible of using in-situ measurements due to remote or harsh weather conditions.

  14. Comparison of satellite-derived sear surface temperatures with in situ skin measurements

    NASA Astrophysics Data System (ADS)

    Schluessel, P.; Shin, H.-Y.; Emery, W. J.; Grassl, H.

    1987-03-01

    Sea surface temperatures (SSTs), computed from sensor systems on the National Oceanographic and Atmospheric Administration (NOAA) polar-orbiting satellites, are compared with surface skin temperatures (from an infrared radiometer mounted on a ship) and subsurface temperature measurements. Three split window retrieval methods using channels 4 and 5 of the NOAA 7 advanced very high resolution radiometer (AVHRR) sensor were investigated. These methods were (1) using AVHRR alone, (2) using AVHRR with atmospheric temperature and water vapor profiles from the TIROS operational vertical sounder (TOVS), and (3) using AVHRR and data from the high-resolution infrared sounder (HIRS). TOVS sensors (including HIRS) are carried by the same satellite as the AVHRR and provide simultaneous corrections for the AVHRR-based SST estimates. The importance of scan angle correction to define the correct atmospheric path is discussed, and the improvement of SST retrievals using sensor combinations is demonstrated with satellite versus ship skin temperature mean differences ranging from 0.55° to 0.73°C for AVHRR alone, from -0.39° to 0.71°C for AVHRR plus TOVS, and from 0.22° to 0.33°C for AVHRR plus HIRS. The improved SST accuracy by AVHRR plus HIRS is due to additional correction for the atmospheric water vapor and temperature structures, made possible with some of the HIRS channels. Significant differences between ship skin and subsurface temperatures were observed, with the mean deviation being 0.2°C for a range of temperature differences between -0.25° and 0.6°C.

  15. In-situ optical monitoring of AlAs wet oxidation using a novel low-temperature low-pressure steam furnace design

    SciTech Connect

    Feld, S.A.; Loehr, J.P.; Sherriff, R.E.; Wiemeri, J.; Kaspi, R.

    1998-02-01

    To reproducibly define small features by oxidizing AlGaAs layers, it is essential to have good control over the oxidation reaction. The authors have integrated a glass viewport into a low-pressure (5 torr) cold-walled oxidation chamber to enable in situ optical monitoring of the sample during oxidation. To gain additional control, they reduced the oxidation temperature to 325 C, consequently slowing the oxidation rate to 2 {micro}m/h. Real-time in situ optical measurements of AlAs oxidation rates were performed using this system and the results were compared with a standard model. Oxide-semiconductor distributed Bragg reflectors (DBRs) were also fabricated and measured, yielding highly reflective mirrors suitable for vertical-cavity surface-emitting laser (VCSEL) fabrication.

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

    PubMed

    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.

  17. Initial characterization of a highly contaminated high explosives outfall in preparation for in situ bioremediation

    SciTech Connect

    Betty A. Strietelmeier; Patrick J. Coyne; Patricia A. Leonard; W. Lamar Miller; Jerry R. Brian

    1999-12-01

    In situ bioremediation is a viable, cost-effective treatment for environmental contamination of many kinds. The feasibility of using biological techniques to remediate soils contaminated with high explosives (HE) requires laboratory evaluation before proceeding to a larger scale field operation. Laboratory investigations have been conducted at pilot scale which indicate that an anaerobic process could be successful at reducing levels of HE, primarily HMX, RDX and TNT, in contaminated soils. A field demonstration project has been designed to create an anaerobic environment for the degradation of HE materials. The first step in this project, initial characterization of the test area, was conducted and is the subject of this report. The levels of HE compounds found in the samples from the test area were higher than the EPA Method 8330 was able to extract without subsequent re-precipitation; therefore, a new method was developed using a superior extractant system. The test area sampling design was relatively simple as one might expect in an initial characterization. A total of 60 samples were each removed to a depth of 4 inches using a 1 inch diameter corer. The samples were spaced at relatively even intervals across a 20 foot cross-section through the middle of four 7-foot-long adjacent plots which are designed to be a part of an in situ bioremediation experiment. Duplicate cores were taken from each location for HE extraction and analysis in order to demonstrate and measure the heterogeneity of the contamination. Each soil sample was air dried and ball-milled to provide a homogeneous solid for extraction and analysis. Several samples had large consolidated pieces of what appeared to be solid HE. These were not ball-milled due to safety concerns, but were dissolved and the solutions were analyzed. The new extraction method was superior in that results obtained for several of the contaminants were up to 20 times those obtained with the EPA extraction method. The

  18. High temperature refrigerator

    DOEpatents

    Steyert, Jr., William A.

    1978-01-01

    A high temperature magnetic refrigerator which uses a Stirling-like cycle in which rotating magnetic working material is heated in zero field and adiabatically magnetized, cooled in high field, then adiabatically demagnetized. During this cycle said working material is in heat exchange with a pumped fluid which absorbs heat from a low temperature heat source and deposits heat in a high temperature reservoir. The magnetic refrigeration cycle operates at an efficiency 70% of Carnot.

  19. High-resolution in situ measurement of nitrate in runoff from the Greenland Ice Sheet.

    PubMed

    Beaton, Alexander David; Wadham, Jemma L; Hawkings, Jon; Bagshaw, Elizabeth A; Lamarche-Gagnon, Guillaume; Mowlem, Matthew C; Tranter, Martyn

    2017-09-27

    We report the first in situ high-resolution nitrate time series from two proglacial meltwater rivers draining the Greenland Ice Sheet, using a recently developed submersible analyser based on lab-on-chip (LOC) technology. The low sample volume (320 μL) required by the LOC analyser meant that low concentration (few to sub μM), highly turbid subglacial meltwater could be filtered and colourimetrically analysed in situ. These data are linked to an unparalleled, multi-component data set. Nitrate concentrations in rivers draining Leverett Glacier in South-West Greenland and Kiattuut Sermiat in Southern Greenland exhibited a clear diurnal signal and a gradual decline at the commencement of the melt season, displaying trends would not be discernible using traditional daily manual sampling. Nitrate concentrations varied by 4.4 μM (+/- 0.2 μM) over a 10-day period at Kiattuut Sermiat and 3.0 μM (+/- 0.2 μM) over a 14 day period at Leverett Glacier. Marked changes in nitrate concentrations were observed when discharge began to increase. High resolution in situ measurements such as these have the potential to significantly advance the understanding of nutrient cycling in remote systems, where the dynamics of nutrient release are complex but are important for downstream biogeochemical cycles.

  20. High-temperature thermodynamics.

    NASA Technical Reports Server (NTRS)

    Margrave, J. L.

    1967-01-01

    High temperature thermodynamics requiring species and phases identification, crystal structures, molecular geometries and vibrational, rotational and electronic energy levels and equilibrium constants

  1. In Situ Balloon-Borne Ice Particle Imaging in High-Latitude Cirrus

    NASA Astrophysics Data System (ADS)

    Kuhn, Thomas; Heymsfield, Andrew J.

    2016-09-01

    Cirrus clouds reflect incoming solar radiation, creating a cooling effect. At the same time, these clouds absorb the infrared radiation from the Earth, creating a greenhouse effect. The net effect, crucial for radiative transfer, depends on the cirrus microphysical properties, such as particle size distributions and particle shapes. Knowledge of these cloud properties is also needed for calibrating and validating passive and active remote sensors. Ice particles of sizes below 100 µm are inherently difficult to measure with aircraft-mounted probes due to issues with resolution, sizing, and size-dependent sampling volume. Furthermore, artefacts are produced by shattering of particles on the leading surfaces of the aircraft probes when particles several hundred microns or larger are present. Here, we report on a series of balloon-borne in situ measurements that were carried out at a high-latitude location, Kiruna in northern Sweden (68N 21E). The method used here avoids these issues experienced with the aircraft probes. Furthermore, with a balloon-borne instrument, data are collected as vertical profiles, more useful for calibrating or evaluating remote sensing measurements than data collected along horizontal traverses. Particles are collected on an oil-coated film at a sampling speed given directly by the ascending rate of the balloon, 4 m s-1. The collecting film is advanced uniformly inside the instrument so that an always unused section of the film is exposed to ice particles, which are measured by imaging shortly after sampling. The high optical resolution of about 4 µm together with a pixel resolution of 1.65 µm allows particle detection at sizes of 10 µm and larger. For particles that are 20 µm (12 pixel) in size or larger, the shape can be recognized. The sampling volume, 130 cm3 s-1, is well defined and independent of particle size. With the encountered number concentrations of between 4 and 400 L-1, this required about 90- to 4-s sampling times to

  2. Calibrating IR Cameras for In-Situ Temperature Measurement During the Electron Beam Melting Process using Inconel 718 and Ti-Al6-V4

    SciTech Connect

    Dinwiddie, Ralph Barton; Lloyd, Peter D; Dehoff, Ryan R; Lowe, Larry E

    2016-01-01

    The Department of Energy s (DOE) Manufacturing Demonstration Facility (MDF) at Oak Ridge National Laboratory (ORNL) provides world-leading capabilities in advanced manufacturing (AM) facilities which leverage previous, on-going government investments in materials science research and characterization. MDF contains systems for fabricating components with complex geometries using AM techniques (i.e. 3D-Printing). Various metal alloy printers, for example, use electron beam melting (EBM) systems for creating these components which are otherwise extremely difficult- if not impossible- to machine. ORNL has partnered with manufacturers on improving the final part quality of components and developing new materials for further advancing these devices. One method being used to study (AM) processes in more depth relies on the advanced imaging capabilities at ORNL. High performance mid-wave infrared (IR) cameras are used for in-situ process monitoring and temperature measurements. However, standard factory calibrations are insufficient due to very low transmissions of the leaded glass window required for X-ray absorption. Two techniques for temperature calibrations will be presented and compared. In-situ measurement of emittance will also be discussed. Ample information can be learned from in-situ IR process monitoring of the EBM process. Ultimately, these imaging systems have the potential for routine use for online quality assurance and feedback control.

  3. Mineralogical determination in situ of a highly heterogeneous material using a miniaturized laser ablation mass spectrometer with high spatial resolution

    NASA Astrophysics Data System (ADS)

    Neubeck, Anna; Tulej, Marek; Ivarsson, Magnus; Broman, Curt; Riedo, Andreas; McMahon, Sean; Wurz, Peter; Bengtson, Stefan

    2016-04-01

    Techniques enabling in situ elemental and mineralogical analysis on extraterrestrial planets are strongly required for upcoming missions and are being continuously developed. There is ample need for quantitative and high-sensitivity analysis of elemental as well as isotopic composition of heterogeneous materials. Here we present in situ spatial and depth elemental profiles of a heterogeneous rock sample on a depth-scale of nanometres using a miniaturized laser ablation mass spectrometer (LMS) designed for planetary space missions. We show that the LMS spectra alone could provide highly detailed compositional, three-dimensional information and oxidation properties of a natural, heterogeneous rock sample. We also show that a combination of the LMS and Raman spectroscopy provide comprehensive mineralogical details of the investigated sample. These findings are of great importance for future space missions where quick, in situ determination of the mineralogy could play a role in the process of selecting a suitable spot for drilling.

  4. High temperature measuring device

    DOEpatents

    Tokarz, Richard D.

    1983-01-01

    A temperature measuring device for very high design temperatures (to 2,000.degree. C.). The device comprises a homogenous base structure preferably in the form of a sphere or cylinder. The base structure contains a large number of individual walled cells. The base structure has a decreasing coefficient of elasticity within the temperature range being monitored. A predetermined quantity of inert gas is confined within each cell. The cells are dimensionally stable at the normal working temperature of the device. Increases in gaseous pressure within the cells will permanently deform the cell walls at temperatures within the high temperature range to be measured. Such deformation can be correlated to temperature by calibrating similarly constructed devices under known time and temperature conditions.

  5. Ice Sheet Temperature Records - Satellite and In Situ Data from Antarctica and Greenland

    NASA Astrophysics Data System (ADS)

    Shuman, C. A.; Comiso, J. C.

    2001-12-01

    Recently completed decadal-length surface temperature records from Antarctica and Greenland are providing insights into the challenge of detecting climate change. Ice and snow cover at high latitudes influence the global climate system by reflecting much of the incoming solar energy back to space. An expected consequence of global warming is a decrease in area covered by snow and ice and an increase in Earth's absorption of solar radiation. Models have predicted that the effects of climate warming may be amplified at high latitudes; thinning of the Greenland ice sheet margins and the breakup of Antarctic Peninsula ice shelves suggest this process may have begun. Satellite data provide an excellent means of observing climate parameters across both long temporal and remote spatial domains but calibration and validation of their data remains a challenge. Infrared sensors can provide excellent temperature information but cloud cover and calibration remain as problems. Passive-microwave sensors can obtain data during the long polar night and through clouds but have calibration issues and a much lower spatial resolution. Automatic weather stations are generally spatially- and temporally-restricted and may have long gaps due to equipment failure. Stable isotopes of oxygen and hydrogen from ice sheet locations provide another means of determining temperature variations with time but are challenging to calibrate to observed temperatures and also represent restricted areas. This presentation will discuss these issues and elaborate on the development and limitations of composite satellite, automatic weather station, and proxy temperature data from selected sites in Antarctica and Greenland.

  6. In situ rheological measurements at extreme pressure and temperature using synchrotron X-ray diffraction and radiography.

    PubMed

    Raterron, Paul; Merkel, Sébastien

    2009-11-01

    Dramatic technical progress seen over the past decade now allows the plastic properties of materials to be investigated under extreme pressure and temperature conditions. Coupling of high-pressure apparatuses with synchrotron radiation significantly improves the quantification of differential stress and specimen textures from X-ray diffraction data, as well as specimen strains and strain rates by radiography. This contribution briefly reviews the recent developments in the field and describes state-of-the-art extreme-pressure deformation devices and analytical techniques available today. The focus here is on apparatuses promoting deformation at pressures largely in excess of 3 GPa, namely the diamond anvil cell, the deformation-DIA apparatus and the rotational Drickamer apparatus, as well as on the methods used to carry out controlled deformation experiments while quantifying X-ray data in terms of materials rheological parameters. It is shown that these new techniques open the new field of in situ investigation of materials rheology at extreme conditions, which already finds multiple fundamental applications in the understanding of the dynamics of Earth-like planet interior.

  7. Highly water-absorbing silk yarn with interpenetrating network via in situ polymerization.

    PubMed

    Lee, Ka I; Wang, Xiaowen; Guo, Xia; Yung, Ka-Fu; Fei, Bin

    2017-02-01

    Silk was modified via in situ polymerization of two monomers acrylamide and sodium acrylate by swelling in an effective LiBr dissolution system. Swelling of natural silks in LiBr solutions of low concentration was clearly observed under optical microscope, and their conformational changes were revealed by X-ray diffraction (XRD) and Fourier transform infrared (FTIR) spectroscopy. Dissolution tests and FTIR spectra of these modified silks suggested the presence of interpenetrating network of polyacrylamide and poly(sodium acrylate) in the silk yarns. These modified silks exhibited superior water absorption to that of raw silk and greatly improved mechanical properties in both dry and wet states. These novel modified silks also showed low cytotoxicity towards skin keratinocytes, having potential applications in biomedical textiles. This modification method by in situ polymerization after swelling in LiBr provides a new route to highly enhance the properties and performance of silk for various applications.

  8. Spline model of the high latitude scintillation based on in situ satellite data

    NASA Astrophysics Data System (ADS)

    Priyadarshi, S.; Wernik, A. W.

    2013-12-01

    We present a spline model for the high latitude ionospheric scintillation using satellite in situ measurements made by the Dynamic Explorer 2 (DE 2) satellite. DE 2 satellite measurements give observations only along satellite orbit but our interpolation model fills the gaps between the satellite orbits. This analytical model is based on products of cubic B-splines and coefficients determined by least squares fit to the binned data and constrained to make the fit periodic in 24 hours of geomagnetic local time, periodic in 360 degrees of invariant longitude, in geomagnetic indices and solar radio flux. Discussion of our results clearly shows the seasonal and diurnal behavior of ionospheric parameters important in scintillation modeling for different geophysical and solar activity conditions. We also show that results obtained from our analytical model match observations obtained from in situ measurements. Shishir Priyadarshi Space Research Centre, Poland

  9. Novel in situ method for locating virtual source in high-rate electron-beam evaporation

    NASA Astrophysics Data System (ADS)

    Bhatia, M. S.

    1994-07-01

    The concept of virtual source simplifies calculation of thickness distribution on extended substrates in high rate vacuum coating employing electron-beam heating. The height of the point (virtual source), from which vapor can be assumed to emanate in accordance with Knudsen's cosine law, to yield the experimentally obtained thickness distribution, is calculated and this establishes the position of virtual source. Such as post facto determination is cumbersome as it is valid for the prescribed material evaporating at a certain rate in a specified geometry. A change in any of these entails a fresh measurement. Experimenters who use a large number of materials and deposit at different rates therefore have to carry out a number of trials before they can locate the virtual source at the desired deposition parameters. An in situ method for obtaining virtual source position can go a long way in reducing the labor of these experiments. A novel in situ method is described to locate the virtual source.

  10. Effects of growth temperature and growth rate on polytypes in gold-catalyzed GaAs nanowires studied by in situ X-ray diffraction

    NASA Astrophysics Data System (ADS)

    Takahasi, Masamitu; Kozu, Miwa; Sasaki, Takuo

    2016-04-01

    The polytypism of GaAs nanowires was investigated by in situ X-ray diffraction under different growth conditions. The growth of nanowires was found to start with the formation of the zincblende structure, followed by the growth of the wurtzite structure. The observed growth process of nanowires was well reproduced by simulations based on a layer-by-layer nucleation model. At a low growth temperature and a high growth rate, stacking faults were found to be frequently introduced owing to the reduction in energy barrier. As a result, the zincblend and wurtzite segments in nanowires were highly fragmented and the wurtzite structure was formed in the early stage of growth.

  11. Two-step in situ biodiesel production from microalgae with high free fatty acid content.

    PubMed

    Dong, Tao; Wang, Jun; Miao, Chao; Zheng, Yubin; Chen, Shulin

    2013-05-01

    The yield of fatty acid methyl ester (FAME) from microalgae biomass is generally low via traditional extraction-conversion route due to the deficient solvent extraction. In this study a two-step in situ process was investigated to obtain a high FAME yield from microalgae biomass that had high free fatty acids (FFA) content. This was accomplished with a pre-esterification process using heterogeneous catalyst to reduce FFA content prior to the base-catalyzed transesterification. The two-step in situ process resulted in a total FAME recovery up to 94.87±0.86%, which was much higher than that obtained by a one-step acid or base catalytic in situ process. The heterogeneous catalyst, Amberlyst-15, could be used for 8 cycles without significant loss in activity. This process have the potential to reduce the production cost of microalgae-derived FAME and be more environmental compatible due to the higher FAME yield with reduced catalyst consumption.

  12. Simultaneous and in situ analysis of thermal and volumetric properties of starch gelatinization over wide pressure and temperature ranges.

    PubMed

    Randzio, Stanislaw L; Orlowska, Marta

    2005-01-01

    A method for simultaneous and in situ analysis of thermal and volumetric properties of starch gelatinization from 0.1 to 100 MPa and from 283 to 430 K is described. The temperature of a very sensitive calorimetric detector containing a starch-water emulsion at a selected pressure is programmed to rise at a slow rate; volume variations are performed automatically to keep the selected pressure constant while the heat exchange rate and the volume are recorded. The method is demonstrated with a novel investigation of pressure effects on a sequence of three phase transitions in an aqueous emulsion of wheat starch (56 wt % water). The volume changes during the main endothermic transition (M), associated with melting of the crystalline part of the starch granules and a helix-coil transformation in amylopectin, but also with an important swelling, were separated into a volume in