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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

    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

  6. 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.

  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. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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%.

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

    SciTech Connect

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

    2013-03-15

    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 Degree-Sign 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.

  2. 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

  3. 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

  4. 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)

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. In situ Expression of Functional Genes Reveals Nitrogen Cycling at High Temperatures in Terrestrial Hydrothermal Systems

    NASA Astrophysics Data System (ADS)

    Loiacono, S. T.; Meyer-Dombard, D. R.

    2011-12-01

    An essential element for life, nitrogen occurs in all living organisms and is critical for the synthesis of amino acids, proteins, nucleic acids, and other forms of biomass. Thus, nitrogen cycling likely plays a vital role in microbial metabolic processes as well as nutrient availability. For microorganisms in "extreme" environments, this means developing adaptations that allow them to survive in harsh conditions and still perform the metabolisms essential to sustain life. Recent studies have screened biofilms and thermal sediments of Yellowstone National Park (YNP) thermal features for the presence of nifH genes, which code for a key enzyme in the nitrogen fixation process [1-4]. Furthermore, analysis of nitrogen isotopes in biofilms across a temperature and chemical gradient revealed that nitrogen fixation likely varies across the chemosynthetic/photosynthetic ecotone [5]. Although research has evaluated and confirmed the presence of nifH genes in various thermophilic microbial communities, the existence of a gene in the DNA of an organism does not verify its use. Instead, other methods, such as culturing, isotope tracer assays, and gene expression studies are required to provide direct evidence of biological nitrogen fixation. Culturing and isotope tracer approaches have successfully revealed high-temperature biological nitrogen fixation in both marine hydrothermal vent microbial communities [6] and in acidic, terrestrial hydrothermal sediment [3]. Transcriptomics-based techniques (using mRNA extracted from samples to confirm in situ expression of targeted genes) have been much more limited in number, and only a few studies have, to date, investigated in situ expression of the nifH gene in thermophilic microbial communities [2, 7]. This study explores the presence and expression of nifH genes in several features of the Lower Geyser Basin (LGB) of YNP. Nucleic acids from chemosynthetic and photosynthetic microbial communities were extracted and then amplified

  11. 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

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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.

  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. Effect of In-situ Cure on Measurement of Glass Transition Temperatures in High-temperature Thermosetting Polymers

    DTIC Science & Technology

    2015-01-01

    presented at Proceedings of SAMPE, 16 May 2015. PA#15140 14. ABSTRACT Using the dicyanate ester of bisphenol E (also known as Primaset LECy), we have...93524 ABSTRACT Using the dicyanate ester of bisphenol E (also known as Primaset LECy), we have illustrated the difficulties inherent in measurement of...high-temperature thermosetting polymers, utilizing cyanate ester resins as examples throughout. In common practice, the glass transition

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. [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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. 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).

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. 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.

  8. 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

  9. 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

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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).

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. [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%.

  12. 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.

  13. 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

  14. 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

  15. 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.

  16. 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...

  17. In-situ fabrication of MoSi2/SiC-Mo2C gradient anti-oxidation coating on Mo substrate and the crucial effect of Mo2C barrier layer at high temperature

    NASA Astrophysics Data System (ADS)

    Liu, Jun; Gong, Qianming; Shao, Yang; Zhuang, Daming; Liang, Ji

    2014-07-01

    MoSi2/SiC-Mo2C gradient coating on molybdenum was in situ prepared with pack cementation process by two steps: (1) carburizing with graphite powder to obtain a Mo2C layer on Mo substrate, and (2) siliconizing with Si powder to get a composite MoSi2/SiC layer on the upper part of Mo2C layer. The microstructure and elemental distribution in the coating were investigated with scanning electron microscopy (SEM), back scattered electron (BSE), energy dispersive spectroscopy (EDS), electron probe microanalysis (EPMA) and X-ray diffraction (XRD). Cyclic oxidation tests (at 500 °C, 1200 °C, 1400 °C and 1600 °C) demonstrated excellent oxidation resistance for the gradient composite coating and the mass loss was only 0.23% in 60 min at 1600 °C. XRD, EPMA, thermal dynamic and phase diagram analyses indicated that the Mo2C barrier layer played the key role in slowing down the diffusion of C and Si toward inner Mo substrate at high temperature and principally this contributed to the excellent anti-oxidation for Mo besides the outer MoSi2/SiC composite layer.

  18. Comparison of Model Temperatures to NOAA In Situ Data at the Greenland Summit

    NASA Astrophysics Data System (ADS)

    Shuman, Christopher; Cullather, Richard; Nowicki, Sophie; Schnaubelt, Michael

    2015-04-01

    slightly warm at the low end, and too cool at the high end while the 2-meter temperatures exaggerate this offset (rotation). ERAI surface temps are slightly too warm at the low end but are fairly close across the full range but their derived 2-meter temps become even warmer at low end of the range. Additional analyses are anticipated including assessing if the elevation differences between the gridded data and the in situ instruments can explain some of the observed differences.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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

  6. 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

  7. 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.

  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. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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

  19. 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

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. 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.

  20. 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}.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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.

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. 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

  11. 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.

  12. 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

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. In Situ Microstructural Control and Mechanical Testing Inside the Transmission Electron Microscope at Elevated Temperatures

    NASA Astrophysics Data System (ADS)

    Wang, Baoming; Haque, M. A.

    2015-08-01

    With atomic-scale imaging and analytical capabilities such as electron diffraction and energy-loss spectroscopy, the transmission electron microscope has allowed access to the internal microstructure of materials like no other microscopy. It has been mostly a passive or post-mortem analysis tool, but that trend is changing with in situ straining, heating and electrical biasing. In this study, we design and demonstrate a multi-functional microchip that integrates actuators, sensors, heaters and electrodes with freestanding electron transparent specimens. In addition to mechanical testing at elevated temperatures, the chip can actively control microstructures (grain growth and phase change) of the specimen material. Using nano-crystalline aluminum, nickel and zirconium as specimen materials, we demonstrate these novel capabilities inside the microscope. Our approach of active microstructural control and quantitative testing with real-time visualization can influence mechanistic modeling by providing direct and accurate evidence of the fundamental mechanisms behind materials behavior.

  12. 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.

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. Tissue microarray (TMA) technology: miniaturized pathology archives for high-throughput in situ studies.

    PubMed

    Bubendorf, L; Nocito, A; Moch, H; Sauter, G

    2001-09-01

    Tissue microarray (TMA) technology allows a massive acceleration of studies correlating molecular in situ findings with clinico-pathological information. In this technique, cylindrical tissue samples are taken from up to 1000 different archival tissue blocks and subsequently placed into one empty 'recipient' paraffin block. Sections from TMA blocks can be used for all different types of in situ tissue analyses including immunohistochemistry and in situ hybridization. Multiple studies have demonstrated that findings obtained on TMAs are highly representative of their donor tissues, despite the small size of the individual specimens (diameter 0.6 mm). It is anticipated that TMAs will soon become a widely used tool for all types of tissue-based research. The availability of TMAs containing highly characterized tissues will enable every researcher to perform studies involving thousands of tumours rapidly. Therefore, TMAs will lead to a significant acceleration of the transition of basic research findings into clinical applications.

  12. 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.

  13. 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.

  14. Ultrasonic Sensors for High Temperature Applications

    NASA Astrophysics Data System (ADS)

    Tittmann, Bernhard; Aslan, Mustafa

    1999-05-01

    Many processes take place under conditions other than ambient, and chief among these is high temperature. Examples of high temperature industrial processes are resin transfer molding, molten metal infiltration and rheocasting of composite metals alloys. The interaction of waves with viscous fluids is an additional complication adding to an already complicated problem of operating a sensor at high temperature for extended periods of time. This report attempts to provide an insight into the current state of the art of sensor techniques for in-situ high temperature monitoring.

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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.

  1. 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.

  2. 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

  3. 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.

  4. 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.

  5. 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.

  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 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. 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

  1. 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.

  2. 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.

  3. 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.

  4. 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

  5. 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.

  6. 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.

  7. 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)

  8. 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.

  9. 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.

  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. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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.

  2. 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.

  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 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.

  5. 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.

  6. 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

  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. 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.

  9. 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

  10. 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.

  11. 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.

  12. In situ transmission infrared spectroscopy of high-kappa oxide atomic layer deposition onto silicon surfaces

    NASA Astrophysics Data System (ADS)

    Ho, Ming-Tsung

    Ultra-thin aluminum oxide (Al2O3) and hafnium oxide (HfO2) layers have been grown by atomic layer deposition (ALD) using tri-methyl-aluminum (TMA) and tetrakis-ethyl-methyl-amino-hafnium (TEMAH) respectively with heavy water (D2O) as the oxidizing agent. Several different silicon surfaces were used as substrates such as hydrogen terminated silicon (H/Si), SC2 (or RCA 2) cleaned native silicon oxide (SiO 2/Si), and silicon (oxy)nitride. In-situ transmission Fourier transform infrared spectroscopy (FTIR) has been adopted for the study of the growth mechanisms during ALD of these films. The vibrational spectra of gas phase TEMAH and its reaction byproducts with oxidants have also been investigated. Density functional theory (DFT) normal mode calculations show a good agreement with the experimental data when it is combined with linear wave-number scaling method and Fermi resonance mechanism. Ether (-C-O-C-) and tertiary alkylamine (N(R1R 2R3)) compounds are the two most dominant products of TEMAH reacting with oxygen gas and water. When ozone is used as the oxidant, gas phase CH2O, CH3NO2, CH3-N=C=O and other compounds containing -(C=O)- and --C-O-C- (or --O-C-) segments are observed. With substrate temperatures less than 400°C and 300°C for TMA and TEMAH respectively, Al oxide and Hf oxide ALD can be appropriately performed on silicon surfaces. Thin silicon (oxy)nitride thermally grown in ammonia on silicon substrate can significantly reduce silicon oxide interlayer formation during ALD and post-deposition annealing. The crystallization temperature of amorphous ALD grown HfO2 on nitridized silicon is 600°C, which is 100°C higher than on the other silicon surfaces. When HfO2 is grown on H/Si(111) at 100°C deposition temperature, minimum 5--10 ALD cycles are required for the full surface coverage. The steric effect can be seen by the evolution of the H-Si stretching mode at 2083 cm-1. The observed red shift of H-Si stretching to ˜ 2060 cm-1 can be caused by Si

  13. 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.

  14. In situ growth of monolayer porous gold nanoparticles film as high-performance SERS substrates

    NASA Astrophysics Data System (ADS)

    Song, Chunyuan; Wei, Yuhan; Da, Bingtao; Zhang, Haiting; Cong, Xing; Yang, Boyue; Yang, Yanjun; Wang, Lianhui

    2016-07-01

    Surface-enhanced Raman scattering (SERS) has recently received considerable attention as an ultrasensitive analytic technique. However, its wide application is limited by lack of excellent SERS-active substrates. In this work a SERS substrate with arrayed monolayer films of porous gold nanoparticles is prepared on a solid substrate by a facile, in situ and one-step growth approach. Specifically, the solid substrate was coated with a layer of dense positive charges first by layer-by-layer assembly, followed by patterned a PDMS film with arrayed wells on the substrate. Then the growth solution including chlorauric acid, cetyltrimethylammonium chloride, and ascorbic acid in a certain proportion was transferred into the wells for in situ and one-step growth of porous gold nanoparticles on the substrate. The growth time, feed ratio of the reagents, and repeat times of the in situ growth were studied systematically to obtain optimal parameters for preparing an optimal SERS substrate. The as-prepared optimal SERS substrate not only has good SERS performance with the enhancement factor up to ∼1.10 × 106, but also shows good uniformity and stability. The SERS substrate was further utilized to be ultrasensitive SERS-based chemical sensors for ppb-level detection of highly toxic dyfonate. The preliminary result indicates that the as-prepared SERS substrate has good SERS performance and shows a number of great potential applications in SERS-based sensors.

  15. In-situ Production of High Density Polyethylene and Other Useful Materials on Mars

    NASA Technical Reports Server (NTRS)

    Flynn, Michael

    2005-01-01

    This paper describes a revolutionary materials structure and power storage concept based on the in-situ production of abiotic carbon 4 compounds. One of the largest single mass penalties required to support the human exploration of Mars is the surface habitat. This proposal will use physical chemical technologies to produce high density polyethylene (HDPE) inflatable structures and construction materials from Mars atmospheric CO2. The formation of polyethylene from Mars CO2 is based on the use of the Sabatier and modified Fischer Tropsch reactions. The proposed system will fully integrate with existing in-situ propellant production concepts. The technology will also be capable of supplementing human caloric requirements, providing solid and liquid fuels for energy storage, and providing significant reduction in mission risk. The NASA Mars Reference Mission Definition Team estimated that a conventional Mars surface habitat structure would weigh 10 tonnes. It is estimated that this technology could reduce this mass by 80%. This reduction in mass will significantly contribute to the reduction in total mission cost need to make a Mars mission a reality. In addition the potential reduction of risk provided by the ability to produce C4 and potentially higher carbon based materials in-situ on Mars is significant. Food, fuel, and shelter are only three of many requirements that would be impacted by this research.

  16. In Situ Observations of Thermoreversible Gelation and Phase Separation of Agarose and Methylcellulose Solutions under High Pressure.

    PubMed

    Kometani, Noritsugu; Tanabe, Masahiro; Su, Lei; Yang, Kun; Nishinari, Katsuyoshi

    2015-06-04

    Thermoreversible sol-gel transitions of agarose and methylcellulose (MC) aqueous solutions on isobaric cooling or heating under high pressure up to 400 MPa have been investigated by in situ observations of optical transmittance and falling-ball experiments. For agarose, which undergoes the gelation on cooling, the application of pressure caused a gradual rise in the cloud-point temperature over the whole pressure range examined, which is almost consistent with the pressure dependence of gelling temperature estimated by falling-ball experiments, suggesting that agarose gel is stabilized by compression and that the gelation occurs nearly in parallel with phase separation under ambient and high-pressure conditions. For MC, which undergoes the gelation on heating, the cloud-point temperature showed a slight rise with an initial elevation of pressure up to ∼150 MPa, whereas it showed a marked depression above 200 MPa. In contrast, the gelling temperature of MC, which is nearly identical to the cloud-point temperature at ambient pressure, showed a monotonous rise with increasing pressure up to 350 MPa, which means that MC undergoes phase separation prior to gelation on heating under high pressure above 200 MPa. Similar results were obtained for the melting process of MC gel on cooling. The unique behavior of the sol-gel transition of MC under high pressure has been interpreted in terms of the destruction of hydrophobic hydration by compression.

  17. 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 increase associated with swelling and a volume decrease associated with the transition itself. Thermodynamic parameters for this transition together with their pressure dependencies have been obtained from four independent experiments at each pressure. The data are thermodynamically consistent, but are poorly described by the Clapeyron equation. The negative volume change of the slow exothermic transition (A) appearing just after the main endothermic transition (M) is small, spread out over a wide temperature interval, and occurs at higher temperatures with increasing pressures. This transition is probably associated with reassociation of the unwound helixes of amylopectin with parts of amylopectin molecules other than their original helix duplex partner. The positive volume change of the high-temperature, endothermic transition (N) with a small enthalpy change is probably associated with a nematic-isotropic transformation ending the formation of a homogeneous SOL phase (in the sense of Flory), and is also pushed to higher temperatures with increasing pressures. Knowledge of the state of wheat starch

  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-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

  20. A generalized method for high throughput in-situ experiment data analysis: An example of battery materials exploration

    NASA Astrophysics Data System (ADS)

    Aoun, Bachir; Yu, Cun; Fan, Longlong; Chen, Zonghai; Amine, Khalil; Ren, Yang

    2015-04-01

    A generalized method is introduced to extract critical information from series of ranked correlated data. The method is generally applicable to all types of spectra evolving as a function of any arbitrary parameter. This approach is based on correlation functions and statistical scedasticity formalism. Numerous challenges in analyzing high throughput experimental data can be tackled using the herein proposed method. We applied this method to understand the reactivity pathway and formation mechanism of a Li-ion battery cathode material during high temperature synthesis using in-situ high-energy X-ray diffraction. We demonstrate that Pearson's correlation function can easily unravel all major phase transition and, more importantly, the minor structural changes which cannot be revealed by conventionally inspecting the series of diffraction patterns. Furthermore, a two-dimensional (2D) reactivity pattern calculated as the scedasticity along all measured reciprocal space of all successive diffraction pattern pairs unveils clearly the structural evolution path and the active areas of interest during the synthesis. The methods described here can be readily used for on-the-fly data analysis during various in-situ operando experiments in order to quickly evaluate and optimize experimental conditions, as well as for post data analysis and large data mining where considerable amount of data hinders the feasibility of the investigation through point-by-point inspection.

  1. Design and development of an environmental cell for dynamic in situ observation of gas-solid reactions at elevated temperatures

    NASA Astrophysics Data System (ADS)

    Deshmukh, Pushkarraj Vasant

    In situ monitoring of events in transmission electron microscopy provides information on how materials behave in their true state while varying environmental conditions (i.e. temperature and pressure) and exposure to reactant gas mixtures. In-situ results are usually different from static, post-reaction observations because they provide valuable real time---rather than post mortem---information. To facilitate applications that demand in situ observations, a transmission electron microscope specimen holder assembly has been developed in this dissertation. This assembly incorporates a gas flow and heating mechanism along with a novel window-type environmental cell. A controlled mixture of up to four different gases can be circulated through the cell during an experiment. In addition, the specimen can be heated up to a temperature of 1500°C using a specially designed carbon dioxide laser mechanism. This heating technique provides major advantages over conventional methods in terms of product life, specimen heating time and design size. The cell design incorporates a gas reaction chamber less than 1 mm in height, enclosed between a pair of 20 nm thick silicon nitride windows. The chamber can accommodate a specimen or a grid having a diameter of 3 mm and thicknesses in the range of 50 to 100 microns. The volume for the gas environment within the chamber is approximately 3 mm 3 and the gas path length is less than 1 mm. This holder has been designed by incorporating cutting edge heating and Si3N4 window fabrication technology to achieve excellent resolution along with a low thermal drift. Successful application of the holder has been shown to provide scientists with an economical alternative to dedicated transmission electron microscopes for a vast array of in situ applications. These applications include understanding the basic material properties, catalysis reactions, semiconductor device development, and nano structure fabrication.

  2. 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.

  3. In situ gas analysis for high pressure applications using property measurements

    NASA Astrophysics Data System (ADS)

    Moeller, J.; Span, R.; Fieback, T.

    2013-10-01

    As the production, distribution, and storage of renewable energy based fuels usually are performed under high pressures and as there is a lack of in situ high pressure gas analysis instruments on the market, the aim of this work was to develop a method for in situ high pressure gas analysis of biogas and hydrogen containing gas mixtures. The analysis is based on in situ measurements of optical, thermo physical, and electromagnetic properties in gas mixtures with newly developed high pressure sensors. This article depicts the calculation of compositions from the measured properties, which is carried out iteratively by using highly accurate equations of state for gas mixtures. The validation of the method consisted of the generation and measurement of several mixtures, of which three are presented herein: a first mixture of 64.9 mol. % methane, 17.1 mol. % carbon dioxide, 9 mol. % helium, and 9 mol. % ethane at 323 K and 423 K in a pressure range from 2.5 MPa to 17 MPa; a second mixture of 93.0 mol. % methane, 4.0 mol. % propane, 2.0 mol. % carbon dioxide, and 1.0 mol. % nitrogen at 303 K, 313 K, and 323 K in a pressure range from 1.2 MPa to 3 MPa; and a third mixture of 64.9 mol. % methane, 30.1 mol. % carbon dioxide, and 5.0 mol. % nitrogen at 303 K, 313 K, and 323 K in a pressure range from 2.5 MPa to 4 MPa. The analysis of the tested gas mixtures showed that with measured density, velocity of sound, and relative permittivity the composition can be determined with deviations below 1.9 mol. %, in most cases even below 1 mol. %. Comparing the calculated compositions with the generated gas mixture, the deviations were in the range of the combined uncertainty of measurement and property models.

  4. In-situ short-circuit protection system and method for high-energy electrochemical cells

    DOEpatents

    Gauthier, Michel; Domroese, Michael K.; Hoffman, Joseph A.; Lindeman, David D.; Noel, Joseph-Robert-Gaetan; Radewald, Vern E.; Rouillard, Jean; Rouillard, Roger; Shiota, Toshimi; Trice, Jennifer L.

    2003-04-15

    An in-situ thermal management system for an energy storage device. The energy storage device includes a plurality of energy storage cells each being coupled in parallel to common positive and negative connections. Each of the energy storage cells, in accordance with the cell's technology, dimensions, and thermal/electrical properties, is configured to have a ratio of energy content-to-contact surface area such that thermal energy produced by a short-circuit in a particular cell is conducted to a cell adjacent the particular cell so as to prevent the temperature of the particular cell from exceeding a breakdown temperature. In one embodiment, a fuse is coupled in series with each of a number of energy storage cells. The fuses are activated by a current spike capacitively produced by a cell upon occurrence of a short-circuit in the cell, thereby electrically isolating the short-circuited cell from the common positive and negative connections.

  5. In-situ short circuit protection system and method for high-energy electrochemical cells

    DOEpatents

    Gauthier, Michel; Domroese, Michael K.; Hoffman, Joseph A.; Lindeman, David D.; Noel, Joseph-Robert-Gaetan; Radewald, Vern E.; Rouillard, Jean; Rouillard, Roger; Shiota, Toshimi; Trice, Jennifer L.

    2000-01-01

    An in-situ thermal management system for an energy storage device. The energy storage device includes a plurality of energy storage cells each being coupled in parallel to common positive and negative connections. Each of the energy storage cells, in accordance with the cell's technology, dimensions, and thermal/electrical properties, is configured to have a ratio of energy content-to-contact surface area such that thermal energy produced by a short-circuit in a particular cell is conducted to a cell adjacent the particular cell so as to prevent the temperature of the particular cell from exceeding a breakdown temperature. In one embodiment, a fuse is coupled in series with each of a number of energy storage cells. The fuses are activated by a current spike capacitively produced by a cell upon occurrence of a short-circuit in the cell, thereby electrically isolating the short-circuited cell from the common positive and negative connections.

  6. High-temperature sensor

    DOEpatents

    Not Available

    1981-01-29

    A high temperature sensor is described which 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 (1000 to 2000/sup 0/K). When required, the sensor can be encased within a ceramic protective coating.

  7. Mineral Carbonation in Wet Supercritical CO2: An in situ High-Pressure Magic Angle Spinning Nuclear Magnetic Resonance Study

    NASA Astrophysics Data System (ADS)

    Turcu, R. V.; Hoyt, D. H.; Sears, J. A.; Rosso, K. M.; Felmy, A. R.; Hu, J. Z.

    2011-12-01

    Understanding the mechanisms and kinetics of mineral carbonation reactions relevant to sequestering carbon dioxide as a supercritical fluid (scCO2) in geologic formations is crucial for accurately predicting long-term storage risks. In situ probes that provide molecular-level information at geologically relevant temperatures and pressures are highly desirable and challenging to develop. Magic angle spinning nuclear magnetic resonance (MAS NMR) is a powerful tool for obtaining detailed molecular structure and dynamics information of a system regardless whether the system is in a solid, a liquid, a gaseous, a supercritical state, or a mixture thereof. However, MAS NMR under scCO2 conditions has never been realized due to the tremendous technical difficulties of achieving and maintaining high pressure within a fast spinning MAS sample rotor. In this work, we report development of a unique high pressure MAS NMR capability capable of handling fluid pressure exceeding 170 bars and temperatures up to 80°C, and its application to mineral carbonation in scCO2 under geologically relevant temperatures and pressures. Mineral carbonation reactions of the magnesium silicate mineral forsterite and the magnesium hydroxide brucite reacted with scCO2 (up to 170 bar) and containing variable content of H2O (at, below, and above saturation in scCO2) were investigated at 50 to 70°C. In situ 13C MAS NMR spectra show peaks corresponding to the reactants, intermediates, and the magnesium carbonation products in a single spectrum. For example, Figure 1 shows the reaction dynamics, i.e., the formation and conversion of reaction intermediates, i.e., HCO3- and nesquehonite, to magnesite as a function of time at 70°C. This capability offers a significant advantage over traditional ex situ 13C MAS experiments on similar systems, where, for example, CO2 and HCO3- are not directly observable.

  8. New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

    SciTech Connect

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; Boehler, Reinhard; Shen, Guoyin

    2015-07-17

    An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in research areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.

  9. New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

    DOE PAGES

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; ...

    2015-07-17

    An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. Furthermore, the new capabilities have demonstrated clear benefits and provide new opportunities in researchmore » areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.« less

  10. New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team

    SciTech Connect

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; Shen, Guoyin; Boehler, Reinhard

    2015-07-15

    An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.

  11. New developments in laser-heated diamond anvil cell with in situ synchrotron x-ray diffraction at High Pressure Collaborative Access Team.

    PubMed

    Meng, Yue; Hrubiak, Rostislav; Rod, Eric; Boehler, Reinhard; Shen, Guoyin

    2015-07-01

    An overview of the in situ laser heating system at the High Pressure Collaborative Access Team, with emphasis on newly developed capabilities, is presented. Since its establishment at the beamline 16-ID-B a decade ago, laser-heated diamond anvil cell coupled with in situ synchrotron x-ray diffraction has been widely used for studying the structural properties of materials under simultaneous high pressure and high temperature conditions. Recent developments in both continuous-wave and modulated heating techniques have been focusing on resolving technical issues of the most challenging research areas. The new capabilities have demonstrated clear benefits and provide new opportunities in research areas including high-pressure melting, pressure-temperature-volume equations of state, chemical reaction, and time resolved studies.

  12. In situ phase separation following dehydration in bimetallic sulfates: a variable-temperature X-ray diffraction study.

    PubMed

    Swain, Diptikanta; Guru Row, Tayur N

    2009-08-03

    Phase separation resulting in a single-crystal-single-crystal transition accompanied by a polycrystalline phase following the dehydration of hydrated bimetallic sulfates [Na(2)Mn(1.167)(SO(4))(2)S(0.33)O(1.167) x 2 H(2)O and K(4)Cd(3)(SO(4))(5) x 3 H(2)O] has been investigated by in situ variable-temperature single-crystal X-ray diffraction. With two examples, we illustrate the possibility of generating structural frameworks following dehydration in bimetallic sulfates, which refer to the possible precursor phases at that temperature leading to the mineral formation. The room-temperature structure of Na(2)Mn(1.167)(SO(4))(2)S(0.33)O(1.167) x 2 H(2)O is trigonal, space group R3. On heating the crystal in situ on the diffractometer, the diffraction images display spherical spots and concentric rings suggesting phase separation, with the spherical spots getting indexed in a monoclinic space group, C2/c. The structure determination based on this data suggests the formation of Na(2)Mn(SO(4))(2). However, the diffraction images from concentric rings could not be indexed. In the second example, the room-temperature structure is determined to be K(4)Cd(3)(SO(4))(5) x 3 H(2)O, crystallizing in a monoclinic space group, P2(1)/n. On heating the crystal in situ, the diffraction images collected also have both spherical spots and diffuse rings. The spherical spots could be indexed to a cubic crystal system, space group P2(1)3, and the structure is K(2)Cd(2)(SO(4))(3). The possible mechanism for the phase transition in the dehydration regime resulting in this remarkable single-crystal to single-crystal transition with the appearance of a surrogate polycrystalline phase is proposed.

  13. In situ supported MnO(x)-CeO(x) on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3.

    PubMed

    Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

    2013-02-07

    The MnO(x) and CeO(x) were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH(3). X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H(2) temperature-programmed reduction (H(2)-TPR) and NH(3) temperature-programmed desorption (NH(3)-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H(2)-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH(3)-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO(2)-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.

  14. In situ subterranean determination of actinides by high-resolution gamma-ray spectrometry

    SciTech Connect

    Brodzinski, R. L.

    1981-04-01

    A system utilizing high resolution germanium diode gamma-ray spectroscopy for the simple, safe, and economical in situ determination of actinides is described. Six isotopes, /sup 235/U, /sup 238/U, /sup 237/Np, /sup 239/Pu, /sup 241/Pu, and /sup 241/Am, can be simultaneously measured at the 10 nCi g/sup -1/ level in less than 7 minutes. Collimators provide for measurement of horizontal strata as thin as 1 cm or solid angles as small as 0.1 steradians. Information obtainable with the system is discussed and compared to that obtainable with neutron activation/detection systems.

  15. In-situ temperature-controllable shear flow device for neutron scattering measurement—An example of aligned bicellar mixtures

    SciTech Connect

    Xia, Yan; Li, Ming; Kučerka, Norbert; Li, Shutao; Nieh, Mu-Ping

    2015-02-15

    We have designed and constructed a temperature-controllable shear flow cell for in-situ study on flow alignable systems. The device has been tested in the neutron diffraction and has the potential to be applied in the small angle neutron scattering configuration to characterize the nanostructures of the materials under flow. The required sample amount is as small as 1 ml. The shear rate on the sample is controlled by the flow rate produced by an external pump and can potentially vary from 0.11 to 3.8 × 10{sup 5} s{sup −1}. Both unidirectional and oscillational flows are achievable by the setting of the pump. The instrument is validated by using a lipid bicellar mixture, which yields non-alignable nanodisc-like bicelles at low T and shear-alignable membranes at high T. Using the shear cell, the bicellar membranes can be aligned at 31 °C under the flow with a shear rate of 11.11 s{sup −1}. Multiple high-order Bragg peaks are observed and the full width at half maximum of the “rocking curve” around the Bragg’s condition is found to be 3.5°–4.1°. It is noteworthy that a portion of the membranes remains aligned even after the flow stops. Detailed and comprehensive intensity correction for the rocking curve has been derived based on the finite rectangular sample geometry and the absorption of the neutrons as a function of sample angle [See supplementary material at http://dx.doi.org/10.1063/1.4908165 for the detailed derivation of the absorption correction]. The device offers a new capability to study the conformational or orientational anisotropy of the solvated macromolecules or aggregates induced by the hydrodynamic interaction in a flow field.

  16. In-situ temperature-controllable shear flow device for neutron scattering measurement—An example of aligned bicellar mixtures

    NASA Astrophysics Data System (ADS)

    Xia, Yan; Li, Ming; Kučerka, Norbert; Li, Shutao; Nieh, Mu-Ping

    2015-02-01

    We have designed and constructed a temperature-controllable shear flow cell for in-situ study on flow alignable systems. The device has been tested in the neutron diffraction and has the potential to be applied in the small angle neutron scattering configuration to characterize the nanostructures of the materials under flow. The required sample amount is as small as 1 ml. The shear rate on the sample is controlled by the flow rate produced by an external pump and can potentially vary from 0.11 to 3.8 × 105 s-1. Both unidirectional and oscillational flows are achievable by the setting of the pump. The instrument is validated by using a lipid bicellar mixture, which yields non-alignable nanodisc-like bicelles at low T and shear-alignable membranes at high T. Using the shear cell, the bicellar membranes can be aligned at 31 °C under the flow with a shear rate of 11.11 s-1. Multiple high-order Bragg peaks are observed and the full width at half maximum of the "rocking curve" around the Bragg's condition is found to be 3.5°-4.1°. It is noteworthy that a portion of the membranes remains aligned even after the flow stops. Detailed and comprehensive intensity correction for the rocking curve has been derived based on the finite rectangular sample geometry and the absorption of the neutrons as a function of sample angle [See supplementary material at http://dx.doi.org/10.1063/1.4908165 for the detailed derivation of the absorption correction]. The device offers a new capability to study the conformational or orientational anisotropy of the solvated macromolecules or aggregates induced by the hydrodynamic interaction in a flow field.

  17. Calcium Pyroxenes at Mercurian Surface Temperatures: Investigation of In-Situ Emissivity Spectra.

    NASA Astrophysics Data System (ADS)

    Ferrari, Sabrina; Maturilli, Alessandro; Helbert, Jörn; Rossi, Manuela; Nestola, Fabrizio; D'Amore, Mario; Hiesinger, Harald

    2014-05-01

    Several observations point to the possibility that Ca-rich (and low-Fe) clinopyroxenes could be common constituent minerals of the surface of Mercury. The upcoming ESA-JAXA BepiColombo mission to Mercury will carry on board the Mercury Radiometer and Thermal Infrared Spectrometer (MERTIS) that will provide surface emissivity spectra in the wavelength range from 7-14 μm. This spectral range is very useful to identify the fine-scale structural properties of several silicates including pyroxenes. The extreme daily surface temperature range of Mercury (70 to 725 K) that significantly affects the spectral signature of minerals will make the interpretation of MERTIS observations challenging. It has been shown that spectra of clinopyroxenes with similar calcium content display a deepening of the main absorption bands, and a shift of the band minima toward higher wavelengths with increasing temperatures. Similar shifts can also be observed at constant temperature with increasing iron content in the M2 site. Therefore, the thermal expansion induced by the increasing temperature simulates the presence of a larger cation (e.g., iron vs. magnesium) within the mineral structure. Interestingly, each band shifts by a different amount, representing a marker for the real chemistry of the sample. A detailed study of the described mineral behavior is fundamental to localize those spectral bands sensitive to the daily temperature range of the Mercury surface. In combination with the temperature measurements obtained independently by the radiometer channel of MERTIS this will help to further constrain the mineralogical interpretation of the MERTIS spectral data. Here we present high-temperature (up to 750 K) laboratory emissivity spectra of several augitic pyroxenes with different calcium contents and very different magnesium to iron ratios. The spectra were derived from individual well-preserved natural crystals of several pyroxenes of less than 125 ?m in size, which approaches the

  18. High Temperature Semiconductor Process

    NASA Technical Reports Server (NTRS)

    1998-01-01

    A sputtering deposition system capable of depositing large areas of high temperature superconducting materials was developed by CVC Products, Inc. with the support of the Jet Propulsion Laboratory SBIR (Small Business Innovative Research) program. The system was devleoped for NASA to produce high quality films of high temperature superconducting material for microwave communication system components. The system is also being used to deposit ferroelectric material for capacitors and the development of new electro-optical materials.2002103899

  19. Taking the temperature of the world's lakes: Decadal variability and long-term trends in lake surface temperature from in situ and satellite observations

    NASA Astrophysics Data System (ADS)

    Lenters, John; Hook, Simon; Read, Jordan; Gray, Derek; Hampton, Stephanie; McIntyre, Peter; O'Reilly, Catherine; Schneider, Philipp; Sharma, Sapna; Contributors, Gltc

    2016-04-01

    Recent studies have shown significant warming of inland water bodies throughout the world. To better understand the patterns, mechanisms, and ecological implications of global lake warming, an initiative known as the "Global Lake Temperature Collaboration" (GLTC) was started in 2010, with the objective of compiling and analyzing lake temperature data from numerous satellite and in situ records dating back at least 20-30 years. The GLTC project has now assembled data from over 250 lakes, with some in situ records dating back more than 100 years. Here, we present an analysis of the long-term warming trends, decadal variability, and a direct comparison between in situ and remotely sensed summer lake surface temperatures from 1895-2009. The results show consistent trends of increasing summer-mean lake surface temperature across most but not all sites. Lakes with especially long records show accelerated warming in the most recent two to three decades, with almost half of the lakes warming at rates in excess of 0.5 °C per decade during the period 1985-2009, and a few even exceeding 1.0 °C per decade.

  20. In Situ Eddy Analysis in a High-Resolution Ocean Climate Model.

    PubMed

    Woodring, Jonathan; Petersen, Mark; Schmeißer, Andre; Patchett, John; Ahrens, James; Hagen, Hans

    2016-01-01

    An eddy is a feature associated with a rotating body of fluid, surrounded by a ring of shearing fluid. In the ocean, eddies are 10 to 150 km in diameter, are spawned by boundary currents and baroclinic instabilities, may live for hundreds of days, and travel for hundreds of kilometers. Eddies are important in climate studies because they transport heat, salt, and nutrients through the world's oceans and are vessels of biological productivity. The study of eddies in global ocean-climate models requires large-scale, high-resolution simulations. This poses a problem for feasible (timely) eddy analysis, as ocean simulations generate massive amounts of data, causing a bottleneck for traditional analysis workflows. To enable eddy studies, we have developed an in situ workflow for the quantitative and qualitative analysis of MPAS-Ocean, a high-resolution ocean climate model, in collaboration with the ocean model research and development process. Planned eddy analysis at high spatial and temporal resolutions will not be possible with a postprocessing workflow due to various constraints, such as storage size and I/O time, but the in situ workflow enables it and scales well to ten-thousand processing elements.

  1. In Situ Biodiesel Production from Fast-Growing and High Oil Content Chlorella pyrenoidosa in Rice Straw Hydrolysate

    PubMed Central

    Li, Penglin; Miao, Xiaoling; Li, Rongxiu; Zhong, Jianjiang

    2011-01-01

    Rice straw hydrolysate was used as lignocellulose-based carbon source for Chlorella pyrenoidosa cultivation and the feasibility of in situ biodiesel production was investigated. 13.7 g/L sugar was obtained by enzymatic hydrolyzation of rice straw. Chlorella pyrenoidosa showed a rapid growth in the rice straw hydrolysate medium, the maximum biomass concentration of 2.83 g/L was obtained in only 48 hours. The lipid content of the cells reached as high as 56.3%. In situ transesterification was performed for biodiesel production. The optimized condition was 1 g algal powder, 6 mL n-hexane, and 4 mL methanol with 0.5 M sulfuric acid at the temperature of 90°C in 2-hour reaction time, under which over 99% methyl ester content and about 95% biodiesel yield were obtained. The results suggested that the method has great potential in the production of biofuels with lignocellulose as an alternative carbon source for microalgae cultivation. PMID:21318171

  2. Sustained ocular drug delivery from a temperature and pH triggered novel in situ gel system.

    PubMed

    Gupta, Himanshu; Jain, Sanyog; Mathur, Rashi; Mishra, Pushpa; Mishra, Anil K; Velpandian, T

    2007-11-01

    Various ocular diseases like glaucoma, conjunctivitis, and dry eye syndrome require frequent drug administration. Poor ocular bioavailability of drugs (< 1%) from conventional eye drops is due mainly to the precorneal loss factors that include rapid tear turnover, nonproductive absorption, transient residence time in the cul-de-sac, and the relative impermeability of the drugs to corneal epithelial membrane. These problems may be overcome by the use of in situ gel-forming systems that are instilled as drops into the eye and undergo a sol-gel transition in the cul-de-sac. Our present work describes the formulation and evaluation of an ocular delivery system of timolol maleate based on the concept of both temperature and pH-triggered in situ gelation. Pluronic F-127 (a thermosensitive polymer) in combination with chitosan (pH-sensitive polymer also acts as permeation enhancer) was used as gelling agent. The developed formulation was characterized for various in vitro parameters e.g., clarity, gelation temperature and pH, isotonicity, sterility, rheological behavior, drug release profile, transcorneal permeation profile, and ocular irritation. Developed formulation was clear, isotonic solution, that converted into gel at temperatures above 35 degrees C and pH 6.9-7.0. A significant higher drug transport across corneal membrane and increased ocular retention time was observed using the developed formulation. The developed system is a viable alternative to conventional eye drops for the treatment of glaucoma and various other ocular diseases.

  3. In Situ, High-Resolution Profiles of Labile Metals in Sediments of Lake Taihu

    PubMed Central

    Wang, Dan; Gong, Mengdan; Li, Yangyang; Xu, Lv; Wang, Yan; Jing, Rui; Ding, Shiming; Zhang, Chaosheng

    2016-01-01

    Characterizing labile metal distribution and biogeochemical behavior in sediments is crucial for understanding their contamination characteristics in lakes, for which in situ, high-resolution data is scare. The diffusive gradient in thin films (DGT) technique was used in-situ at five sites across Lake Taihu in the Yangtze River delta in China to characterize the distribution and mobility of eight labile metals (Fe, Mn, Zn, Ni, Cu, Pb, Co and Cd) in sediments at a 3 mm spatial resolution. The results showed a great spatial heterogeneity in the distributions of redox-sensitive labile Fe, Mn and Co in sediments, while other metals had much less marked structure, except for downward decreases of labile Pb, Ni, Zn and Cu in the surface sediment layers. Similar distributions were found between labile Mn and Co and among labile Ni, Cu and Zn, reflecting a close link between their geochemical behaviors. The relative mobility, defined as the ratio of metals accumulated by DGT to the total contents in a volume of sediments with a thickness of 10 mm close to the surface of DGT probe, was the greatest for Mn and Cd, followed by Zn, Ni, Cu and Co, while Pb and Fe had the lowest mobility; this order generally agreed with that defined by the modified BCR approach. Further analyses showed that the downward increases of pH values in surface sediment layer may decrease the lability of Pb, Ni, Zn and Cu as detected by DGT, while the remobilization of redox-insensitive metals in deep sediment layer may relate to Mn cycling through sulphide coprecipitation, reflected by several corresponding minima between these metals and Mn. These in situ data provided the possibility for a deep insight into the mechanisms involved in the remobilization of metals in freshwater sediments. PMID:27608033

  4. Comparisons of the in-situ measurements from the rocket Nimbus satellite comparison series II. [atmospheric temperature

    NASA Technical Reports Server (NTRS)

    Olsen, R. O.; Schmidlin, F. J.; Wright, D. U.; Luers, J. R.

    1978-01-01

    Atmospheric measurements between 30 and 90 km using two rocket-borne techniques - the inflatable falling sphere and the acoustic grenade - are compared in order to determine temperature measurement compatibility. The falling sphere, deployed at 115 km, is tracked by precision radar to determine winds as well as accurate drag parameters needed to deduce density from which temperatures are derived. The acoustic grenade technique uses sound arrivals at the ground from grenades ejected at 2-km intervals to determine temperature and wind between 40 and 90 km. The available data were obtained during an in-situ techniques-comparison with the remote sounders aboard Nimbus 6 during the summer and winter of 1975.

  5. In situ flash x-ray high-speed computed tomography for the quantitative analysis of highly dynamic processes

    NASA Astrophysics Data System (ADS)

    Moser, Stefan; Nau, Siegfried; Salk, Manfred; Thoma, Klaus

    2014-02-01

    The in situ investigation of dynamic events, ranging from car crash to ballistics, often is key to the understanding of dynamic material behavior. In many cases the important processes and interactions happen on the scale of milli- to microseconds at speeds of 1000 m s-1 or more. Often, 3D information is necessary to fully capture and analyze all relevant effects. High-speed 3D-visualization techniques are thus required for the in situ analysis. 3D-capable optical high-speed methods often are impaired by luminous effects and dust, while flash x-ray based methods usually deliver only 2D data. In this paper, a novel 3D-capable flash x-ray based method, in situ flash x-ray high-speed computed tomography is presented. The method is capable of producing 3D reconstructions of high-speed processes based on an undersampled dataset consisting of only a few (typically 3 to 6) x-ray projections. The major challenges are identified, discussed and the chosen solution outlined. The application is illustrated with an exemplary application of a 1000 m s-1 high-speed impact event on the scale of microseconds. A quantitative analysis of the in situ measurement of the material fragments with a 3D reconstruction with 1 mm voxel size is presented and the results are discussed. The results show that the HSCT method allows gaining valuable visual and quantitative mechanical information for the understanding and interpretation of high-speed events.

  6. High-Temperature Superconductivity

    SciTech Connect

    Peter Johnson

    2008-11-05

    Like astronomers tweaking images to gain a more detailed glimpse of distant stars, physicists at Brookhaven National Laboratory have found ways to sharpen images of the energy spectra in high-temperature superconductors — materials that carry electrical c

  7. High Temperature Capacitor Development

    SciTech Connect

    John Kosek

    2009-06-30

    The absence of high-temperature electronics is an obstacle to the development of untapped energy resources (deep oil, gas and geothermal). US natural gas consumption is projected to grow from 22 trillion cubic feet per year (tcf) in 1999 to 34 tcf in 2020. Cumulatively this is 607 tcf of consumption by 2020, while recoverable reserves using current technology are 177 tcf. A significant portion of this shortfall may be met by tapping deep gas reservoirs. Tapping these reservoirs represents a significant technical challenge. At these depths, temperatures and pressures are very high and may require penetrating very hard rock. Logistics of supporting 6.1 km (20,000 ft) drill strings and the drilling processes are complex and expensive. At these depths up to 50% of the total drilling cost may be in the last 10% of the well depth. Thus, as wells go deeper it is increasingly important that drillers are able to monitor conditions down-hole such as temperature, pressure, heading, etc. Commercial off-the-shelf electronics are not specified to meet these operating conditions. This is due to problems associated with all aspects of the electronics including the resistors and capacitors. With respect to capacitors, increasing temperature often significantly changes capacitance because of the strong temperature dependence of the dielectric constant. Higher temperatures also affect the equivalent series resistance (ESR). High-temperature capacitors usually have low capacitance values because of these dielectric effects and because packages are kept small to prevent mechanical breakage caused by thermal stresses. Electrolytic capacitors do not operate at temperatures above 150oC due to dielectric breakdown. The development of high-temperature capacitors to be used in a high-pressure high-temperature (HPHT) drilling environment was investigated. These capacitors were based on a previously developed high-voltage hybridized capacitor developed at Giner, Inc. in conjunction with a

  8. High-temperature electronics

    NASA Technical Reports Server (NTRS)

    Matus, Lawrence G.; Seng, Gary T.

    1990-01-01

    To meet the needs of the aerospace propulsion and space power communities, the high temperature electronics program at the Lewis Research Center is developing silicon carbide (SiC) as a high temperature semiconductor material. This program supports a major element of the Center's mission - to perform basic and developmental research aimed at improving aerospace propulsion systems. Research is focused on developing the crystal growth, characterization, and device fabrication technologies necessary to produce a family of SiC devices.

  9. High temperature pressure gauge

    DOEpatents

    Echtler, J. Paul; Scandrol, Roy O.

    1981-01-01

    A high temperature pressure gauge comprising a pressure gauge positioned in fluid communication with one end of a conduit which has a diaphragm mounted in its other end. The conduit is filled with a low melting metal alloy above the diaphragm for a portion of its length with a high temperature fluid being positioned in the remaining length of the conduit and in the pressure gauge.

  10. In situ FT-IR study on the homogeneous nucleation of nanoparticles of titanium oxides from highly supersaturated vapor

    NASA Astrophysics Data System (ADS)

    Ishizuka, Shinnosuke; Kimura, Yuki; Yamazaki, Tomoya

    2016-09-01

    The formation of nanoparticles of titanium oxides by homogeneous nucleation from highly supersaturated vapors was investigated by in situ Fourier transform IR spectroscopy and by observation of the resulting nanoparticles by transmission electron microscopy (TEM). Titanium metal was thermally evaporated in a specially designed chamber under a gaseous atmosphere of oxygen and argon. Nanoparticles nucleated and subsequently grew as they flew freely through the oxidizing gas atmosphere. Nascent nanoparticles of titanium oxides showed a broad IR absorption band at 10-20 μm. Subsequently, the cooled nanoparticles showed a sharp crystalline anatase feature at 12.8 μm. TEM observations showed the formation of spherical anatase nanoparticles. The IR spectral evolution showed that the titanium oxides nucleated as metastable liquid droplets, and that crystallization proceeded through secondary nucleation from the supercooled liquid droplets. This suggests that history of the titanium oxide nanoparticles, such as the temperature and oxidation that they experience after nucleation, determines their polymorphic form.

  11. High temperature electronics

    NASA Astrophysics Data System (ADS)

    Seng, Gary T.

    1991-03-01

    In recent years, the aerospace propulsion and space power communities have acknowledged a growing need for electronic devices that are capable of sustained high-temperature operation. Aeropropulsion applications for high-temperature electronic devices include engine ground test instrumentation such as multiplexers, analog-to-digital converters, and telemetry systems capable of withstanding hot section engine temperatures in excess of 600 C. Uncooled operation of control and condition monitoring systems in advanced supersonic aircraft would subject the electronics to temperatures in excess of 300 C. Similarly, engine-mounted integrated electronic sensors could reach temperatures which exceed 500 C. In addition to aeronautics, there are many other areas that could benefit from the existence of high-temperature electronic devices. Space applications include power electronic devices for space platforms and satellites. Since power electronics require radiators to shed waste heat, electronic devices that operate at higher temperatures would allow a reduction in radiator size. Terrestrial applications include deep-well drilling instrumentation, high power electronics, and nuclear reactor instrumentation and control. To meet the needs of the applications mentioned previously, the high-temperature electronics (HTE) program at the Lewis Research Center is developing silicon carbide (SiC) as a high-temperature semiconductor material. Research is focused on developing the crystal growth, growth modeling, characterization, and device fabrication technologies necessary to produce a family of SiC devices. Interest in SiC has grown dramatically in recent years due to solid advances in the technology. Much research remains to be performed, but SiC appears ready to emerge as a useful semiconductor material.

  12. High Temperature ESP Monitoring

    SciTech Connect

    Jack Booker; Brindesh Dhruva

    2011-06-20

    The objective of the High Temperature ESP Monitoring project was to develop a downhole monitoring system to be used in wells with bottom hole well temperatures up to 300°C for measuring motor temperature, formation pressure, and formation temperature. These measurements are used to monitor the health of the ESP motor, to track the downhole operating conditions, and to optimize the pump operation. A 220 ºC based High Temperature ESP Monitoring system was commercially released for sale with Schlumberger ESP motors April of 2011 and a 250 ºC system with will be commercially released at the end of Q2 2011. The measurement system is now fully qualified, except for the sensor, at 300 °C.

  13. High temperature probe

    DOEpatents

    Swan, Raymond A.

    1994-01-01

    A high temperature probe for sampling, for example, smokestack fumes, and is able to withstand temperatures of 3000.degree. F. The probe is constructed so as to prevent leakage via the seal by placing the seal inside the water jacket whereby the seal is not exposed to high temperature, which destroys the seal. The sample inlet of the probe is also provided with cooling fins about the area of the seal to provide additional cooling to prevent the seal from being destroyed. Also, a heated jacket is provided for maintaining the temperature of the gas being tested as it passes through the probe. The probe includes pressure sensing means for determining the flow velocity of an efficient being sampled. In addition, thermocouples are located in various places on the probe to monitor the temperature of the gas passing there through.

  14. High temperature structural silicides

    SciTech Connect

    Petrovic, J.J.

    1997-03-01

    Structural silicides have important high temperature applications in oxidizing and aggressive environments. Most prominent are MoSi{sub 2}-based materials, which are borderline ceramic-intermetallic compounds. MoSi{sub 2} single crystals exhibit macroscopic compressive ductility at temperatures below room temperature in some orientations. Polycrystalline MoSi{sub 2} possesses elevated temperature creep behavior which is highly sensitive to grain size. MoSi{sub 2}-Si{sub 3}N{sub 4} composites show an important combination of oxidation resistance, creep resistance, and low temperature fracture toughness. Current potential applications of MoSi{sub 2}-based materials include furnace heating elements, molten metal lances, industrial gas burners, aerospace turbine engine components, diesel engine glow plugs, and materials for glass processing.

  15. Versatile variable temperature insert at the DEIMOS beamline for in situ electrical transport measurements.

    PubMed

    Joly, L; Muller, B; Sternitzky, E; Faullumel, J G; Boulard, A; Otero, E; Choueikani, F; Kappler, J P; Studniarek, M; Bowen, M; Ohresser, P

    2016-05-01

    The design and the first experiments are described of a versatile cryogenic insert used for its electrical transport capabilities. The insert is designed for the cryomagnet installed on the DEIMOS beamline at the SOLEIL synchrotron dedicated to magnetic characterizations through X-ray absorption spectroscopy (XAS) measurements. This development was spurred by the multifunctional properties of novel materials such as multiferroics, in which, for example, the magnetic and electrical orders are intertwined and may be probed using XAS. The insert thus enables XAS to in situ probe this interplay. The implementation of redundant wiring and careful shielding also enables studies on operating electronic devices. Measurements on magnetic tunnel junctions illustrate the potential of the equipment toward XAS studies of in operando electronic devices.

  16. Scaling an in situ network for high resolution modeling during SMAPVEX15

    NASA Astrophysics Data System (ADS)

    Coopersmith, E. J.; Cosh, M. H.; Jacobs, J. M.; Jackson, T. J.; Crow, W. T.; Holifield Collins, C.; Goodrich, D. C.; Colliander, A.

    2015-12-01

    Among the greatest challenges within the field of soil moisture estimation is that of scaling sparse point measurements within a network to produce higher resolution map products. Large-scale field experiments present an ideal opportunity to develop methodologies for this scaling, by coupling in situ networks, temporary networks, and aerial mapping of soil moisture. During the Soil Moisture Active Passive Validation Experiments in 2015 (SMAPVEX15) in and around the USDA-ARS Walnut Gulch Experimental Watershed and LTAR site in southeastern Arizona, USA, a high density network of soil moisture stations was deployed across a sparse, permanent in situ network in coordination with intensive soil moisture sampling and an aircraft campaign. This watershed is also densely instrumented with precipitation gages (one gauge/0.57 km2) to monitor the North American Monsoon System, which dominates the hydrologic cycle during the summer months in this region. Using the precipitation and soil moisture time series values provided, a physically-based model is calibrated that will provide estimates at the 3km, 9km, and 36km scales. The results from this model will be compared with the point-scale gravimetric samples, aircraft-based sensor, and the satellite-based products retrieved from NASA's Soil Moisture Active Passive mission.

  17. Microbial diversity in long-term water-flooded oil reservoirs with different in situ temperatures in China

    PubMed Central

    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. PMID:23094135

  18. Dynamic fuel retention in tokamak wall materials: An in situ laboratory study of deuterium release from polycrystalline tungsten at room temperature

    NASA Astrophysics Data System (ADS)

    Bisson, R.; Markelj, S.; Mourey, O.; Ghiorghiu, F.; Achkasov, K.; Layet, J.-M.; Roubin, P.; Cartry, G.; Grisolia, C.; Angot, T.

    2015-12-01

    Retention of deuterium ion implanted in polycrystalline tungsten samples is studied in situ in an ultra-high vacuum apparatus equipped with a low-flux ion source and a high sensitivity thermo-desorption setup. Retention as a function of ion fluence was measured in the 1017-1021 D+·m-2 range. By combining this new fluence range with the literature in situ experimental data, we evidence the existence of a retention ∝ fluence0.645±0.025 relationship which describes deuterium retention behavior on polycrystalline tungsten on 8 orders of magnitude of fluence. Evolution of deuterium retention as a function of the sample storage time in vacuum at room temperature was followed. A loss of 50% of the retained deuterium is observed when the storage time is increased from 2 h to 135 h. The role of the surface and of natural bulk defects on the deuterium retention/release in polycrystalline tungsten is discussed in light of the behavior of the single desorption peak obtained with Temperature Programmed Desorption.

  19. Sensor fabrication method for in situ temperature and humidity monitoring of light emitting diodes.

    PubMed

    Lee, Chi-Yuan; Su, Ay; Liu, Yin-Chieh; Chan, Pin-Cheng; Lin, Chia-Hung

    2010-01-01

    In this work micro temperature and humidity sensors are fabricated to measure the junction temperature and humidity of light emitting diodes (LED). The junction temperature is frequently measured using thermal resistance measurement technology. The weakness of this method is that the timing of data capture is not regulated by any standard. This investigation develops a device that can stably and continually measure temperature and humidity. The device is light-weight and can monitor junction temperature and humidity in real time. Using micro-electro-mechanical systems (MEMS), this study minimizes the size of the micro temperature and humidity sensors, which are constructed on a stainless steel foil substrate (40 μm-thick SS-304). The micro temperature and humidity sensors can be fixed between the LED chip and frame. The sensitivities of the micro temperature and humidity sensors are 0.06±0.005 (Ω/°C) and 0.033 pF/%RH, respectively.

  20. The 'Nuts and Bolts' of 13C NMR Spectroscopy at Elevated-Pressures and -Temperatures for Monitoring In Situ CO2 Conversion to Metal Carbonates

    NASA Astrophysics Data System (ADS)

    Moore, J. K.; Surface, J. A.; Skemer, P. A.; Conradi, M. S.; Hayes, S. E.

    2013-12-01

    characterization of multiple metastable mineral phases in pure forms and in mixtures. Notably, NMR spectroscopy is able to observe signals from amorphous materials, and mixtures of both crystalline and amorphous species can be analyzed. NMR results are verified through a combination of Raman spectroscopy and powder XRD (of crystalline species). Further, we have examined the effects on mineralization reactions of pH gradients in the sample--also monitored in situ by NMR--and these results will be presented. Reference: 'In Situ Measurement of Magnesium Carbonate Formation from CO2 Using Static High-Pressure and -Temperature 13C NMR' J. Andrew Surface, Philip Skemer, Sophia E. Hayes, and Mark S. Conradi, Environ. Sci. Technol. 2013, 47, 119-125. DOI: 10.1021/es301287n

  1. In situ high throughput method for H(2)S detection during micro-scale wine fermentation.

    PubMed

    Winter, Gal; Curtin, Chris

    2012-10-01

    An in situ high throughput method for the detection of H(2)S during fermentation was developed. The method utilizes a redox reaction in which sulfide ion reduces methylene blue, leading to its decolourisation. Incorporation of methylene blue into the fermentation media allows real-time detection of H(2)S during fermentation and the generation of an H(2)S production profile. Kinetic parameters extracted from the H(2)S production profile can be used to characterise genetic factors affecting H(2)S production and differentiate between environmental conditions affecting it. The method, validated here for Saccharomyces cerevisiae, is suited for high throughput screening purposes by virtue of its simplicity and the ability to detect H(2)S in micro-scale fermentations.

  2. High-Temperature Lubricants

    NASA Technical Reports Server (NTRS)

    1984-01-01

    In the early 1980's, Lewis Research Center began a program to develop high-temperature lubricants for use on future aircraft flying at three or more times the speed of sound, which can result in vehicle skin temperatures as high as 1,600 degrees Fahrenheit. A material that emerged from this research is a plasma-sprayed, self-lubricating metal- glass-fluoride coating able to reduce oxidation at very high temperatures. Technology is now in commercial use under the trade name Surf-Kote C-800, marketed by Hohman Plating and Manufacturing Inc. and manufactured under a patent license from NASA. Among its uses are lubrication for sliding contact bearings, shaft seals for turbopumps, piston rings for high performance compressors and hot glass processing machinery; it is also widely used in missile and space applications.

  3. Transmission electron microscopy study of cascade collapse in copper during in-situ ion-irradiation at elevated temperatures.

    SciTech Connect

    Daulton, T. L.; Kirk, M. A.; Rehn, L. E.

    1998-01-29

    The basic mechanisms driving the collapse of point defects produced in collision cascades are investigated by transmission electron microscope (TEM) characterization of defect microstructure produced in fcc-Cu irradiated with low-fluences of heavy (100 keV Kr) ions at elevated temperature (23--600 C). Areal defect yields are determined from direct TEM observation of the total defect production integrated over the duration of the in-situ ion-irradiation. They are unequivocally demonstrated to decrease with increasing lattice temperature. This decrease in defect yield indicates a proportional decrease in the probability of collapse of cascade regions into defects of size where visible contrast is produced in a TEM.

  4. Firsthand in situ observation of active fine laser tuning by combining a temperature gradient and a CLC wedge cell structure.

    PubMed

    Jeong, Mi-Yun; Cha, Jihun

    2015-08-10

    In situ direct observation of the lasing process in a cholesteric liquid crystal (CLC) laser array using a CMOS camera was used to investigate discontinuous laser tuning in a parallel CLC cell. In accordance with the discontinuous pitch change by thermal energy transfer, at the same time the laser wavelength undergoes an immediate and discontinuous shift. And we found out the reason why the CLC phase has domain textures. And this work develops a simple active tunable laser array by forming a spatial temperature gradient along a wedge CLC cell. With this new strategy, only just about 7 nm laser tuning range at room temperature is extremely widened over the 105 nm wavelength range with about 0.2 nm tuning resolution. Furthermore, there is no aging effect because the employed CLC array has only one chiral molecular concentration. This strategy could be used in a practical CLC laser device application.

  5. High-resolution Fiber-optic Microendoscopy for in situ Cellular Imaging

    PubMed Central

    Pierce, Mark; Yu, Dihua; Richards-Kortum, Rebecca

    2011-01-01

    Many biological and clinical studies require the longitudinal study and analysis of morphology and function with cellular level resolution. Traditionally, multiple experiments are run in parallel, with individual samples removed from the study at sequential time points for evaluation by light microscopy. Several intravital techniques have been developed, with confocal, multiphoton, and second harmonic microscopy all demonstrating their ability to be used for imaging in situ 1. With these systems, however, the required infrastructure is complex and expensive, involving scanning laser systems and complex light sources. Here we present a protocol for the design and assembly of a high-resolution microendoscope which can be built in a day using off-the-shelf components for under US$5,000. The platform offers flexibility in terms of image resolution, field-of-view, and operating wavelength, and we describe how these parameters can be easily modified to meet the specific needs of the end user. We and others have explored the use of the high-resolution microendoscope (HRME) in in vitro cell culture 2-5, in excised 6 and living animal tissues 2,5, and in human tissues in vivo 2,7. Users have reported the use of several different fluorescent contrast agents, including proflavine 2-4, benzoporphyrin-derivative monoacid ring A (BPD-MA) 5, and fluoroscein 6,7, all of which have received full, or investigational approval from the FDA for use in human subjects. High-resolution microendoscopy, in the form described here, may appeal to a wide range of researchers working in the basic and clinical sciences. The technique offers an effective and economical approach which complements traditional benchtop microscopy, by enabling the user to perform high-resolution, longitudinal imaging in situ. PMID:21248707

  6. Copper phosphonatoethanesulfonates: temperature dependent in situ energy dispersive X-ray diffraction study and influence of the pH on the crystal structures.

    PubMed

    Feyand, Mark; Hübner, Annika; Rothkirch, André; Wragg, David S; Stock, Norbert

    2012-11-19

    The system Cu(2+)/H2O3P-C2H4-SO3H/NaOH was investigated using in situ energy dispersive X-ray diffraction (EDXRD) to study the formation and temperature induced phase transformation of previously described copper phosphonosulfonates. Thus, the formation of [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·3H2O (4) at 90 °C is shown to proceed via a previously unknown intermediate [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·4H2O (6), which could be structurally characterized from high resolution powder diffraction data. Increase of the reaction temperature to 150 °C led to a rapid phase transformation to [Cu2(O3P-C2H4-SO3)(OH)(H2O)]·H2O (1), which was also studied by in situ EDXRD. The comparison of the structures of 1, 4, and 6 allowed us to establish a possible reaction mechanism. In addition to the in situ crystallization studies, microwave assisted heating for the synthesis of the copper phosphonosulfonates was employed, which allowed the growth of larger crystals of [NaCu(O3P-C2H4-SO3)(H2O)2] (5) suitable for single crystal X-ray diffraction. Through the combination of force field calculations and Rietveld refinement we were able to determine the crystal structure of [Cu1.5(O3P-C2H4-SO3)] 2H2O (3) and thus structurally characterize all compounds known up to now in this well investigated system. With the additional structural data we are now able to describe the influence of the pH on the structure formation.

  7. Structural characterizaiton and gas reactions of small metal particles by high-resolution, in-situ TEM and TED

    NASA Technical Reports Server (NTRS)

    1984-01-01

    The existing in-situ transmission electron microscopy (TEM) facility was improved by adding a separately pumped mini-specimen chamber. The chamber contains wire-evaporation sources for three metals and a specimen heater for moderate substrate temperatures. A sample introduction device was constructed, installed, and tested, facilitating rapid introduction of a specimen into the mini-chamber while maintaining the background pressure in that chamber in the 10(-9) millibar range. Small particles and clusters of Pd, grown by deposition from the vapor phase in an in-situ TEM facility on amorphous and crystalline support films of alumina and on ultra-thin carbon films, were analyzed by conventional high-resolution TEM and image analysis in terms of detectability, number density, and size distribution. The smallest particles that could be detected and counted contained no more than 6 atoms; size determinations could be made for particles 1 nm in diameter. The influence of various oxygen plasma treatments, annealing treatments, and of increasing the substrate temperature during deposition was investigated. The TEM technique was employed to demonstrate that under otherwise identica l conditions the lattice parameter of Pd particles in the 1 to 2 nm size range and supported in random orientation on ex-situ prepared mica films is expanded by some 3% when compared to 5 nm size particles. It is believed that this expansion is neither a small-particle diffraction effect nor due to pseudomorphism, but that it is due to a annealing-induced transformation of the small as-deposited particles with predominantly composite crystal structures into larger particles with true f.c.c. structure and thus inherently smaller lattice parameter.

  8. Validation of Land Surface Temperature from multiple satellite instruments using worldwide in situ datasets and sensor inter-comparisons

    NASA Astrophysics Data System (ADS)

    Schneider, Philipp; Martins, Joao; Trigo, Isabel; Pires, Ana; Jimenez, Carlos; Prigent, Catherine; Prata, Fred; Goettsche, Frank; Hook, Simon

    2014-05-01

    Land surface temperature (LST) is an important parameter for a wide variety of earth surface processes and in particular for evapotranspiration. The ESA-funded project WACMOS-ET aims at advancing the development of evapotranspiration estimates at global and regional scales using various earth observations products. As part of this project, LST is computed globally using satellite data from both low-earth orbit and geostationary instruments. More specifically, observations from the Advanced Along-Track Scanning Radiometer (AATSR), the Spinning Enhanced Visible and Infrared Imager (SEVIRI), the Geostationary Operational Environmental Satellite (GOES), and the Multi-functional Transport Satellite (MTSAT) have been used to generate LST for a three year period ranging from 2005 through 2007. Here we present the first validation results of the project's LST component. The validation was performed by comparing satellite-derived LST a) against in situ observations acquired at stations located in various land cover types and b) against the independent observations of the well-validated MOD11 LST product which is generated from data of the Moderate Resolution Imaging Spectroradiometer (MODIS) satellite instrument onboard of the Terra platform. More specifically, in situ observations of LST were obtained from stations located in Gobabeb (Namibia), Evora (Portugal), Lake Tahoe (Unites States), as well as multiple sites of the Surface Radiation (SURFRAD) and Atmospheric Radiation Measurement (ARM) station networks. The initial results overall indicate good correspondence with the in situ datasets and with the independent satellite observations. As would be expected the LST error increases with the spatial heterogeneity of the validation site and the resulting uncertainty in the emissivity estimates. Furthermore the relationship between LST error and land cover is studied and the impact of different algorithms is investigated.

  9. Assessing microbial processes in deep-sea hydrothermal systems by incubation at in situ temperature and pressure

    NASA Astrophysics Data System (ADS)

    McNichol, Jesse; Sylva, Sean P.; Thomas, François; Taylor, Craig D.; Sievert, Stefan M.; Seewald, Jeffrey S.

    2016-09-01

    At deep-sea hydrothermal vents, a large source of potential chemical energy is created when reducing vent fluid and oxidizing seawater mix. In this environment, chemolithoautotrophic microbes catalyze exergonic redox reactions which in turn provide the energy needed to fuel their growth and the fixation of CO2 into biomass. In addition to producing new organic matter, this process also consumes compounds contained both in vent fluid and entrained seawater (e.g. H2, NO3-). Despite their biogeochemical importance, such reactions have remained difficult to quantify due to methodological limitations. To address this knowledge gap, this study reports a novel application of isobaric gas-tight fluid samplers for conducting incubations of hydrothermal vent fluids at in situ temperature and pressure. Eighteen 24 h incubations were carried out, representing seven distinct conditions that examine amendments consisting of different electron donors and acceptors. Microbial activity was observed in all treatments, and time series chemical measurements showed that activity was limited by electron acceptor supply, confirming predictions based on geochemical data. Also consistent with these predictions, the presence of nitrate increased rates of hydrogen consumption and yielded ammonium as a product of nitrate respiration. The stoichiometry of predicted redox reactions was also determined, revealing that the sulfur and nitrogen cycles are incompletely understood at deep-sea vents, and likely involve unknown intermediate redox species. Finally, the measured rates of redox processes were either equal to or far greater than what has been reported in previous studies where in situ conditions were not maintained. In addition to providing insights into deep-sea hydrothermal vent biogeochemistry, the methods described herein also offer a practical approach for the incubation of any deep-sea pelagic sample under in situ conditions.

  10. Trends in Mars Thermospheric Density and Temperature Structure Obtained from MAVEN In-situ Datasets: Interpretation Using Global Models

    NASA Astrophysics Data System (ADS)

    Bougher, Stephen W.; Tolson, Robert H.; Mahaffy, Paul R.; Johnston, Timothy E.; Olsen, Kirk; Bell, Jared M.

    2015-04-01

    The Mars thermosphere-ionosphere-exosphere (TIE) system constitutes the atmospheric reservoir (i.e. available cold and hot planetary neutral and thermal ion species) that regulates present day escape processes from the planet. Without knowledge of the physics and chemistry creating this TIE region and driving its variations (e.g., solar cycle, seasonal), it is not possible to constrain either the short-term or long-term histories of atmosphere escape. The characterization of this upper atmosphere reservoir is one of the major science objectives of the MAVEN mission.We investigate both in-situ Neutral Gas and Ion Mass Spectrometer (NGIMS) neutral densities/temperatures and Accelerometer Experiment (ACC) reaction wheel (RW) derived mass densities/temperatures obtained over the first ~400 orbits. This sampling occurs when periapsis latitudes ranged from about 32° to 74°N periapsis local mean solar times (LMST) ranged from about 15:00 to 06:00; and corresponding periapsis altitudes ranged from ~200 km down to ~150 km. This dayside in-situ sampling lasted until about 17-December-2014, after which the periapsis began moving Southward toward nightside Northern mid-latitudes. During this dayside period, monthly mean solar EUV-UV fluxes corresponded to F10.7 ~ 150-160 at Earth (solar moderate conditions) and the Martian season was approaching perihelion (Ls ~ 205 to 254°).Thermospheric trends (e.g. latitude, local time, diurnal) of extracted densities and inferred temperatures will be compared with corresponding 3-D Mars Global Ionosphere-Thermosphere Model (M-GITM) simulated outputs in order to understand the variations observed, and probe the underlying physical processes responsible. Solar rotation variations in EUV fluxes and their impacts on dayside temperatures will also be examined.

  11. Temperature Assisted in-Situ Small Angle X-ray Scattering Analysis of Ph-POSS/PC Polymer Nanocomposite

    NASA Astrophysics Data System (ADS)

    Yadav, Ramdayal; Naebe, Minoo; Wang, Xungai; Kandasubramanian, Balasubramanian

    2016-07-01

    Inorganic/organic nanofillers have been extensively exploited to impart thermal stability to polymer nanocomposite via various strategies that can endure structural changes when exposed a wide range of thermal environment during their application. In this abstraction, we have utilized temperature assisted in-situ small angle X-ray scattering (SAXS) to examine the structural orientation distribution of inorganic/organic nanofiller octa phenyl substituted polyhedral oligomeric silsesquioxane (Ph-POSS) in Polycarbonate (PC) matrix from ambient temperature to 180 °C. A constant interval of 30 °C with the heating rate of 3 °C/min was utilized to guise the temperature below and above the glass transition temperature of PC followed by thermal gravimetric, HRTEM, FESEM and hydrophobic analysis at ambient temperature. The HRTEM images of Ph-POSS nano unit demonstrated hyperrectangular structure, while FESEM image of the developed nano composite rendered separated phase containing flocculated and overlapped stacking of POSS units in the PC matrix. The phase separation in polymer nanocomposite was further substantiated by thermodynamic interaction parameter (χ) and mixing energy (Emix) gleaned via Accelrys Materials studio. The SAXS spectra has demonstrated duplex peak at higher scattering vector region, postulated as a primary and secondary segregated POSS domain and followed by abundance of secondary peak with temperature augmentation.

  12. Temperature Assisted in-Situ Small Angle X-ray Scattering Analysis of Ph-POSS/PC Polymer Nanocomposite

    PubMed Central

    Yadav, Ramdayal; Naebe, Minoo; Wang, Xungai; Kandasubramanian, Balasubramanian

    2016-01-01

    Inorganic/organic nanofillers have been extensively exploited to impart thermal stability to polymer nanocomposite via various strategies that can endure structural changes when exposed a wide range of thermal environment during their application. In this abstraction, we have utilized temperature assisted in-situ small angle X-ray scattering (SAXS) to examine the structural orientation distribution of inorganic/organic nanofiller octa phenyl substituted polyhedral oligomeric silsesquioxane (Ph-POSS) in Polycarbonate (PC) matrix from ambient temperature to 180 °C. A constant interval of 30 °C with the heating rate of 3 °C/min was utilized to guise the temperature below and above the glass transition temperature of PC followed by thermal gravimetric, HRTEM, FESEM and hydrophobic analysis at ambient temperature. The HRTEM images of Ph-POSS nano unit demonstrated hyperrectangular structure, while FESEM image of the developed nano composite rendered separated phase containing flocculated and overlapped stacking of POSS units in the PC matrix. The phase separation in polymer nanocomposite was further substantiated by thermodynamic interaction parameter (χ) and mixing energy (Emix) gleaned via Accelrys Materials studio. The SAXS spectra has demonstrated duplex peak at higher scattering vector region, postulated as a primary and secondary segregated POSS domain and followed by abundance of secondary peak with temperature augmentation. PMID:27436152

  13. Dynamic in situ observation of voltage-driven repeatable magnetization reversal at room temperature.

    PubMed

    Gao, Ya; Hu, Jia-Mian; Nelson, C T; Yang, T N; Shen, Y; Chen, L Q; Ramesh, R; Nan, C W

    2016-03-31

    Purely voltage-driven, repeatable magnetization reversal provides a tantalizing potential for the development of spintronic devices with a minimum amount of power consumption. Substantial progress has been made in this subject especially on magnetic/ferroelectric heterostructures. Here, we report the in situ observation of such phenomenon in a NiFe thin film grown directly on a rhombohedral Pb(Mg1/3Nb2/3)0.7Ti0.3O3(PMN-PT) ferroelectric crystal. Under a cyclic voltage applied perpendicular to the PMN-PT without a magnetic field, the local magnetization of NiFe can be repetitively reversed through an out-of-plane excursion and then back into the plane. Using phase field simulations we interpret magnetization reversal as a synergistic effect of the metastable ferroelastic switching in the PMN-PT and an electrically rotatable local exchange bias field arising from the heterogeneously distributed NiO clusters at the interface.

  14. Dynamic in situ observation of voltage-driven repeatable magnetization reversal at room temperature

    NASA Astrophysics Data System (ADS)

    Gao, Ya; Hu, Jia-Mian; Nelson, C. T.; Yang, T. N.; Shen, Y.; Chen, L. Q.; Ramesh, R.; Nan, C. W.

    2016-03-01

    Purely voltage-driven, repeatable magnetization reversal provides a tantalizing potential for the development of spintronic devices with a minimum amount of power consumption. Substantial progress has been made in this subject especially on magnetic/ferroelectric heterostructures. Here, we report the in situ observation of such phenomenon in a NiFe thin film grown directly on a rhombohedral Pb(Mg1/3Nb2/3)0.7Ti0.3O3(PMN-PT) ferroelectric crystal. Under a cyclic voltage applied perpendicular to the PMN-PT without a magnetic field, the local magnetization of NiFe can be repetitively reversed through an out-of-plane excursion and then back into the plane. Using phase field simulations we interpret magnetization reversal as a synergistic effect of the metastable ferroelastic switching in the PMN-PT and an electrically rotatable local exchange bias field arising from the heterogeneously distributed NiO clusters at the interface.

  15. Dynamic in situ observation of voltage-driven repeatable magnetization reversal at room temperature

    PubMed Central

    Gao, Ya; Hu, Jia-Mian; Nelson, C. T.; Yang, T. N.; Shen, Y.; Chen, L. Q.; Ramesh, R.; Nan, C. W.

    2016-01-01

    Purely voltage-driven, repeatable magnetization reversal provides a tantalizing potential for the development of spintronic devices with a minimum amount of power consumption. Substantial progress has been made in this subject especially on magnetic/ferroelectric heterostructures. Here, we report the in situ observation of such phenomenon in a NiFe thin film grown directly on a rhombohedral Pb(Mg1/3Nb2/3)0.7Ti0.3O3(PMN-PT) ferroelectric crystal. Under a cyclic voltage applied perpendicular to the PMN-PT without a magnetic field, the local magnetization of NiFe can be repetitively reversed through an out-of-plane excursion and then back into the plane. Using phase field simulations we interpret magnetization reversal as a synergistic effect of the metastable ferroelastic switching in the PMN-PT and an electrically rotatable local exchange bias field arising from the heterogeneously distributed NiO clusters at the interface. PMID:27029464

  16. Synthesis and characterization of an in situ forming hydrogel using tyramine conjugated high methoxyl gum tragacanth.

    PubMed

    Tavakol, Moslem; Vasheghani-Farahani, Ebrahim; Mohammadifar, Mohammad Amin; Soleimani, Masoud; Hashemi-Najafabadi, Sameereh

    2016-02-01

    In this study, an enzyme catalyzed in situ forming hydrogel based on tyramine conjugated high methoxyl content gum tragacanth (TA-HMGT) was prepared and characterized. TA-HMGT was synthesized via heterogeneous ammonolysis of methyl ester groups of HMGT. Then, the hydrogel was prepared via horseradish peroxidase catalyzed coupling reaction in the presence of hydrogen peroxide. Hydrogel properties, such as gelation time, swelling/degradation behavior and rheological properties could be adjusted by tuning the gelation parameters and extent of tyramine conjugation. This system was a soft elastic hydrogel with appropriate biocompatibility. The fast gelation of the hydrogel is desirable for clinical applications. Also, in vitro bovine serum albumin release from the synthesized hydrogel showed good release profile with limited burst release.

  17. In situ laser-induced synthesis of copper microstructures with high catalytic properties and sensory characteristics

    NASA Astrophysics Data System (ADS)

    Tumkin, Ilya I.; Panov, Maxim S.; Khairullina, Evgenia; Gordeychuk, Dmitry; Ermakov, Sergey S.; Kochemirovsky, Vladimir A.

    2016-11-01

    The continuous in situ laser-induced catalysis proceeding via generation and growth of nano-sized copper particles was discussed. Also, the simple and lost-cost method for manufacturing of microstructural copper electrodes was proposed. The electrochemical properties of these electrodes were studied by cyclic voltammetry and impedance spectroscopy. The surface of the deposited copper structures (electrodes) was investigated by X-ray photoelectron spectroscopy and atomic force microscopy. These microstructures are highly conductive and porous with a dispersion of pore size ranging from 50 nm to 50 μm. An analytical response of the fabricated copper electrode is 30 times higher than those observed for a pure bulk copper with similar geometric parameters. A study of sensory characteristics for hydrogen peroxide determination showed that the value of Faraday current at the fabricated copper electrode is 2-2.5 orders of magnitude higher than for etalon one.

  18. In-Situ Observation of Horizontal Centrifugal Casting using a High-Speed Camera

    NASA Astrophysics Data System (ADS)

    Esaka, Hisao; Kawai, Kohsuke; Kaneko, Hiroshi; Shinozuka, Kei

    2012-07-01

    In order to understand the solidification process of horizontal centrifugal casting, experimental equipment for in-situ observation using transparent organic substance has been constructed. Succinonitrile-1 mass% water alloy was filled in the round glass cell and the glass cell was completely sealed. To observe the movement of equiaxed grains more clearly and to understand the effect of movement of free surface, a high-speed camera has been installed on the equipment. The most advantageous point of this equipment is that the camera rotates with mold, so that one can observe the same location of the glass cell. Because the recording rate could be increased up to 250 frames per second, the quality of movie was dramatically modified and this made easier and more precise to pursue the certain equiaxed grain. The amplitude of oscillation of equiaxed grain ( = At) decreased as the solidification proceeded.

  19. In situ imaging and proteome profiling indicate andrographolide is a highly promiscuous compound

    PubMed Central

    Li, Lin; Wijaya, Hadhi; Samanta, Sanjay; Lam, Yulin; Yao, Shao Q.

    2015-01-01

    Natural products represent an enormous source of pharmacologically useful compounds, and are often used as the starting point in modern drug discovery. Many biologically interesting natural products are however not being pursued as potential drug candidates, partly due to a lack of well-defined mechanism-of-action. Traditional in vitro methods for target identification of natural products based on affinity protein enrichment from crude cellular lysates cannot faithfully recapitulate protein-drug interactions in living cells. Reported herein are dual-purpose probes inspired by the natural product andrographolide, capable of both reaction-based, real-time bioimaging and in situ proteome profiling/target identification in live mammalian cells. Our results confirm that andrographolide is a highly promiscuous compound and engaged in covalent interactions with numerous previously unknown cellular targets in cell type-specific manner. We caution its potential therapeutic effects should be further investigated in detail. PMID:26105662

  20. Low toxicity high temperature PMR polyimide

    NASA Technical Reports Server (NTRS)

    Pater, Ruth H. (Inventor)

    1992-01-01

    In-situ polymerization of monomer reactants (PMR) type polyimides constitute an important class of ultra high performance composite matrix resins. PMR-15 is the best known and most widely used PMR polyimide. An object of the present invention is to provide a substantially improved high temperature PMR-15 system that exhibits better processability, toughness, and thermo-oxidative stability than PMR-15, as well as having a low toxicity. Another object is to provide new PMR polyimides that are useful as adhesives, moldings, and composite matrices. By the present invention, a new PMR polyimide comprises a mixture of the following compounds: 3,4'-oxydianiline (3,4'-ODA), NE, and BTDE which are then treated with heat. This PMR was designated LaRC-RP46 and has a broader processing window, better reproducibility of high quality composite parts, better elevated temperature mechanical properties, and higher retention of mechanical properties at an elevated temperature, particularly, at 371 C.

  1. EXPERIMENTAL INVESTIGATION AND HIGH RESOLUTION SIMULATOR OF IN-SITU COMBUSTION PROCESSES

    SciTech Connect

    Margot Gerritsen; Anthony R. Kovscek

    2005-02-01

    Accurate simulation of in-situ combustion processes is computationally very challenging because the spatial and temporal scales over which the combustion process takes place are very small. In this fifth quarterly report of our DoE funded research, we continue the discussion of the design of a new simulation tool based on an efficient Cartesian Adaptive Mesh Refinement technique that allows much higher grid densities to be used near typical fronts than current simulators. We have now developed an appropriate upscaling technique for our grids, based on the local-global upscaling approach. We show preliminary results on two-dimensional test cases. On the experimental side, we continued experiments to measure the rates and kinetics of combustion in the presence and absence of metallic additives. In this quarter, we developed a better understanding of the cation replacing power of the various additives that affect combustion performance positively, and obtained a preliminary reactivity series. We also resumed our experimental investigation into the cyclic solvent-combustion process using crude oil from the Hamaca Region of Venezuela. Various measurements were made including oxygen consumption as a function of temperature. Preliminary results show that the temperatures for the onset of combustion are a function of the solvent injected.

  2. Preparation of high temperature gas-cooled reactor fuel element

    DOEpatents

    Bradley, Ronnie A.; Sease, John D.

    1976-01-01

    This invention relates to a method for the preparation of high temperature gas-cooled reactor (HTGR) fuel elements wherein uncarbonized fuel rods are inserted in appropriate channels of an HTGR fuel element block and the entire block is inserted in an autoclave for in situ carbonization under high pressure. The method is particularly applicable to remote handling techniques.

  3. In-situ microfluidic controlled, low temperature hydrothermal growth of nanoflakes for dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Zhao, Chao; Zhang, Jia; Hu, Yue; Robertson, Neil; Hu, Ping An; Child, David; Gibson, Desmond; Fu, Yong Qing

    2015-12-01

    In this paper, an in-situ microfluidic control unit (MCU) was designed and applied in a hydrothermal synthesis process, which provides an easy way to localize liquid-phase reaction and realize selective synthesis and direct growth of nanostructures as well as their morphology, all in a low-temperature and atmospheric environment. The morphology was controlled through controlling the amount of additivities using the MCU. This achieved a facile fabrication of Al doped ZnO (AZO) nanoflakes vertically grown on flexible polymer substrates with enhanced light scattering and dye loading capabilities. Flexible DSSCs with a significant enhancement (410% compare to ZnO NRs based devices) in power conversion efficiency were obtained using AZO nanoflake photoanodes of 6 μm thick, due to the enhancement in electron mobility and reduction in recombination. This hydrothermal synthesis using the in-situ MCU provides an efficient and scalable technique to synthesize controllable nanostructures with characteristics of easy set-up, low energy consumption and low cost.

  4. In-situ microfluidic controlled, low temperature hydrothermal growth of nanoflakes for dye-sensitized solar cells

    PubMed Central

    Zhao, Chao; Zhang, Jia; Hu, Yue; Robertson, Neil; Hu, Ping An; Child, David; Gibson, Desmond; Fu, Yong Qing

    2015-01-01

    In this paper, an in-situ microfluidic control unit (MCU) was designed and applied in a hydrothermal synthesis process, which provides an easy way to localize liquid-phase reaction and realize selective synthesis and direct growth of nanostructures as well as their morphology, all in a low-temperature and atmospheric environment. The morphology was controlled through controlling the amount of additivities using the MCU. This achieved a facile fabrication of Al doped ZnO (AZO) nanoflakes vertically grown on flexible polymer substrates with enhanced light scattering and dye loading capabilities. Flexible DSSCs with a significant enhancement (410% compare to ZnO NRs based devices) in power conversion efficiency were obtained using AZO nanoflake photoanodes of 6 μm thick, due to the enhancement in electron mobility and reduction in recombination. This hydrothermal synthesis using the in-situ MCU provides an efficient and scalable technique to synthesize controllable nanostructures with characteristics of easy set-up, low energy consumption and low cost. PMID:26631685

  5. Stimulating in situ denitrification in an aerobic, highly permeable municipal drinking water aquifer.

    PubMed

    Critchley, K; Rudolph, D L; Devlin, J F; Schillig, P C

    2014-12-15

    A preliminary trial of a cross-injection system (CIS) was designed to stimulate in situ denitrification in an aquifer servicing an urban community in southern Ontario. It was hypothesized that this remedial strategy could be used to reduce groundwater nitrate in the aquifer such that it could remain in use as a municipal supply until the beneficial effects of local reduced nutrient loadings lead to long-term water quality improvement at the wellfield. The CIS application involved injecting a carbon source (acetate) into the subsurface using an injection-extraction well pair positioned perpendicular to the regional flow direction, up-gradient of the water supply wells, with the objective of stimulating native denitrifying bacteria. The pilot remedial strategy was targeted in a high nitrate flux zone within an aerobic and heterogeneous section of the glacial sand and gravel aquifer. Acetate injections were performed at intervals ranging from daily to bi-daily. The carbon additions led to general declines in dissolved oxygen concentrations; decreases in nitrate concentration were localized in aquifer layers where velocities were estimated to be less than 0.5m/day. NO3-(15)N and NO3-(18)O isotope data indicated the nitrate losses were due to denitrification. Relatively little nitrate was removed from groundwater in the more permeable strata, where velocities were estimated to be on the order of 18 m/day or greater. Overall, about 11 percent of the nitrate mass passing through the treatment zone was removed. This work demonstrates that stimulating in situ denitrification in an aerobic, highly conductive aquifer is challenging but achievable. Further work is needed to increase rates of denitrification in the most permeable units of the aquifer.

  6. In vivo and in situ tracking cancer chemotherapy by highly photostable NIR fluorescent theranostic prodrug.

    PubMed

    Wu, Xumeng; Sun, Xuanrong; Guo, Zhiqian; Tang, Jianbin; Shen, Youqing; James, Tony D; Tian, He; Zhu, Weihong

    2014-03-05

    In vivo monitoring of the biodistribution and activation of prodrugs is urgently required. Near infrared (NIR) fluorescence-active fluorophores with excellent photostability are preferable for tracking drug release in vivo. Herein, we describe a NIR prodrug DCM-S-CPT and its polyethylene glycol-polylactic acid (PEG-PLA) loaded nanoparticles as a potent cancer therapy. We have conjugated a dicyanomethylene-4H-pyran derivative as the NIR fluorophore with camptothecin (CPT) as the anticancer drug using a disulfide linker. In vitro experiments verify that the high intracellular glutathione (GSH) concentrations in tumor cells cause cleavage of the disulfide linker, resulting in concomitantly the active drug CPT release and significant NIR fluorescence turn-on with large Stokes shift (200 nm). The NIR fluorescence of DCM-S-CPT at 665 nm with fast response to GSH can act as a direct off-on signal reporter for the GSH-activatable prodrug. Particularly, DCM-S-CPT possesses much better photostability than ICG, which is highly desirable for in situ fluorescence-tracking of cancer chemotherapy. DCM-S-CPT has been successfully utilized for in vivo and in situ tracking of drug release and cancer therapeutic efficacy in living animals by NIR fluorescence. DCM-S-CPT exhibits excellent tumor-activatable performance when intravenously injected into tumor-bearing nude mice, as well as specific cancer therapy with few side effects. DCM-S-CPT loaded in PEG-PLA nanoparticles shows even higher antitumor activity than free CPT, and is also retained longer in the plasma. The tumor-targeting ability and the specific drug release in tumors make DCM-S-CPT as a promising prodrug, providing significant advances toward deeper understanding and exploration of theranostic drug-delivery systems.

  7. Real time, in-situ temperature monitoring using diffuse reflectance spectroscopy

    SciTech Connect

    Booth, J.L.; Beard, B.T.; Pearsall, T.P.; Wang, Z.Z.; Stevens, J.E.; Blain, M.G.; Meisenheimer, T.L.

    1996-11-01

    Real time temperature measurements have been performed on both GaAs and silicon substrates during wafer processing using a technique based upon diffuse reflectance spectroscopy (DRS). Good temperature resolution ({+-}O.4 {degrees}C) and rapid updates have enabled the process control potential of the device to be demonstrated.

  8. High temperature storage loop :

    SciTech Connect

    Gill, David Dennis; Kolb, William J.

    2013-07-01

    A three year plan for thermal energy storage (TES) research was created at Sandia National Laboratories in the spring of 2012. This plan included a strategic goal of providing test capability for Sandia and for the nation in which to evaluate high temperature storage (>650ÀC) technology. The plan was to scope, design, and build a flow loop that would be compatible with a multitude of high temperature heat transfer/storage fluids. The High Temperature Storage Loop (HTSL) would be reconfigurable so that it was useful for not only storage testing, but also for high temperature receiver testing and high efficiency power cycle testing as well. In that way, HTSL was part of a much larger strategy for Sandia to provide a research and testing platform that would be integral for the evaluation of individual technologies funded under the SunShot program. DOEs SunShot program seeks to reduce the price of solar technologies to 6/kWhr to be cost competitive with carbon-based fuels. The HTSL project sought to provide evaluation capability for these SunShot supported technologies. This report includes the scoping, design, and budgetary costing aspects of this effort

  9. Seeing the light: the effects of particles, dissolved materials, and temperature on in situ measurements of DOM fluorescence in rivers and streams

    USGS Publications Warehouse

    Downing, Bryan D.; Pellerin, Brian A.; Bergamaschi, Brian A.; Saraceno, John Franco; Kraus, Tamara E.C.

    2012-01-01

    Field-deployable sensors designed to continuously measure the fluorescence of colored dissolved organic matter (FDOM) in situ are of growing interest. However, the ability to make FDOM measurements that are comparable across sites and over time requires a clear understanding of how instrument characteristics and environmental conditions affect the measurements. In particular, the effects of water temperature and light attenuation by both colored dissolved material and suspended particles may be significant in settings such as rivers and streams. Using natural standard reference materials, we characterized the performance of four commercially-available FDOM sensors under controlled laboratory conditions over ranges of temperature, dissolved organic matter (DOM) concentrations, and turbidity that spanned typical environmental ranges. We also examined field data from several major rivers to assess how often attenuation artifacts or temperature effects might be important. We found that raw (uncorrected) FDOM values were strongly affected by the light attenuation that results from dissolved substances and suspended particles as well as by water temperature. Observed effects of light attenuation and temperature agreed well with theory. Our results show that correction of measured FDOM values to account for these effects is necessary and feasible over much of the range of temperature, DOM concentration, and turbidity commonly encountered in surface waters. In most cases, collecting high-quality FDOM measurements that are comparable through time and between sites will require concurrent measurements of temperature and turbidity, and periodic discrete sample collection for laboratory measurement of DOM.

  10. Setting up of a low temperature in-situ ion implantation and channeling facility at Kalpakkam

    SciTech Connect

    Sundaravel, B.; Saravanan, K.; Panigrahi, B. K.; Nair, K. G. M.

    2011-07-15

    A simple low temperature ion implantation and ion channeling facility has been set up. Low temperatures upto 70 K has been obtained on a goniometer sample holder by connecting to a continuous flow Helium cryostat with a copper braid. Charge integration is carried out with a transmission Faraday cup with 10 mm diameter aperture and four Faraday cups for performing ion implantation and an electron suppressed 1.5 mm aperture with a TEM grid of 60% beam transmission for ion beam analysis. Typical low temperature ion implantation and channeling experiments have been carried out. Stabilization at intermediate temperatures by controlling the heater at the sample holder and improvement of the achievable lowest temperature by having liquid nitrogen cooled heat shield are in progress.

  11. In Situ Polymerization and Characterization of Highly Conducting Polypyrrole Fish Scales for High-Frequency Applications

    NASA Astrophysics Data System (ADS)

    Velhal, Ninad B.; Patil, Narayan D.; Puri, Vijaya R.

    2015-12-01

    Polypyrrole (Ppy) thin films on alumina were synthesized by an in situ chemical oxidative polymerization method at 300 K with equal monomer-to-oxidant ratio. Fourier transform infrared spectroscopy (FTIR) and FT-Raman spectroscopy confirmed the formation of Ppy. A thickness-dependent change from cauliflower to fish-scale morphology was observed. Microwave properties such as transmission, reflection, shielding effectiveness, permittivity, and microwave conductivity are reported in the frequency range from 8 GHz to 12 GHz. The direct-current (DC) conductivity varied from 9.45 × 10-3 S/cm to 17.29 × 10-3 S/cm, whereas the microwave conductivity varied from 63.07 S/cm to 349.08 S/cm. The shielding effectiveness varied between 6.18 dB and 10.39 dB.

  12. EQUILGAS: Program to estimate temperatures and in situ two-phase conditions in geothermal reservoirs using three combined FT-HSH gas equilibria models

    NASA Astrophysics Data System (ADS)

    Barragán, Rosa María; Núñez, José; Arellano, Víctor Manuel; Nieva, David

    2016-03-01

    Exploration and exploitation of geothermal resources require the estimation of important physical characteristics of reservoirs including temperatures, pressures and in situ two-phase conditions, in order to evaluate possible uses and/or investigate changes due to exploitation. As at relatively high temperatures (>150 °C) reservoir fluids usually attain chemical equilibrium in contact with hot rocks, different models based on the chemistry of fluids have been developed that allow deep conditions to be estimated. Currently either in water-dominated or steam-dominated reservoirs the chemistry of steam has been useful for working out reservoir conditions. In this context, three methods based on the Fischer-Tropsch (FT) and combined H2S-H2 (HSH) mineral-gas reactions have been developed for estimating temperatures and the quality of the in situ two-phase mixture prevailing in the reservoir. For these methods the mineral buffers considered to be controlling H2S-H2 composition of fluids are as follows. The pyrite-magnetite buffer (FT-HSH1); the pyrite-hematite buffer (FT-HSH2) and the pyrite-pyrrhotite buffer (FT-HSH3). Currently from such models the estimations of both, temperature and steam fraction in the two-phase fluid are obtained graphically by using a blank diagram with a background theoretical solution as reference. Thus large errors are involved since the isotherms are highly nonlinear functions while reservoir steam fractions are taken from a logarithmic scale. In order to facilitate the use of the three FT-HSH methods and minimize visual interpolation errors, the EQUILGAS program that numerically solves the equations of the FT-HSH methods was developed. In this work the FT-HSH methods and the EQUILGAS program are described. Illustrative examples for Mexican fields are also given in order to help the users in deciding which method could be more suitable for every specific data set.

  13. In-situ ellipsometric studies of optical and surface properties of GaAs(100) at elevated temperatures

    NASA Technical Reports Server (NTRS)

    Yao, Huade; Snyder, Paul G.

    1991-01-01

    A rotating-polarizer ellipsometer was attached to an ultrahigh vacuum (UHV) chamber. A GaAs(100) sample was introduced into the UHV chamber and heated at anumber of fixed elevated temperatures, without arsenic overpressure. In-situ spectroscopic ellipsometric (SE) measurements were taken, through a pair of low-strain quartz windows, to monitor the surface changes and measure the pseudodielectric functions at elevated temperatures. Real-time data from GaAs surface covered with native oxide showed clearly the evolution of oxide desorption at approximately 580 C. In addition, surface degradation was found before and after the oxide desorption. An oxide free and smooth GaAs surface was obtained by depositing an arsenic protective coating onto a molecular beam epitaxy grown GaAs surface. The arsenic coating was evaporated immediately prior to SE measurements. A comparison showed that our room temperature data from this GaAs surface, measured in the UHV, are in good agreement with those in the literature obtained by wet-chemical etching. The surface also remained clean and smooth at higher temperatures, so that reliable temperature-dependent dielectric functions were obtained.

  14. Highly textured fresnoite thin films synthesized in situ by pulsed laser deposition with CO2 laser direct heating

    NASA Astrophysics Data System (ADS)

    Lorenz, Michael; de Pablos-Martin, Araceli; Patzig, Christian; Stölzel, Marko; Brachwitz, Kerstin; Hochmuth, Holger; Grundmann, Marius; Höche, Thomas

    2014-01-01

    Fresnoite Ba2TiSi2O8 (BTS) thin films were grown and crystallized in situ using pulsed laser deposition (PLD) with CO2 laser direct heating of the a-plane sapphire (1 1 0) substrates up to 1250 °C. Starting with 775 °C growth temperature, (0 0 1)- and (1 1 0)-textured BTS and BaTiO3 phases, respectively, could be assigned in the films, and the typical fern-like BTS crystallization patterns appear. For higher process temperatures of 1100 to 1250 °C, atomically smooth, terraced surface of the films was found, accompanied by crystalline high-temperature phases of Ba-Ti-Si oxides. HAADF micrographs taken in both scanning transmission electron microscopy and energy-dispersive x-ray spectrometry mode show details of morphology and elemental distribution inside the films and at the interface. To balance the inherent Si deficiency of the BTS films, growth from glassy BTS × 2 SiO2 and BTS × 2.5 SiO2 targets was considered as well. The latter targets are ideal for PLD since the employed glasses possess 100% of the theoretical density and are homogeneous at the atomic scale.

  15. A Versatile System for High-Throughput In Situ X-ray Screening and Data Collection of Soluble and Membrane-Protein Crystals

    PubMed Central

    2016-01-01

    In recent years, in situ data collection has been a major focus of progress in protein crystallography. Here, we introduce the Mylar in situ method using Mylar-based sandwich plates that are inexpensive, easy to make and handle, and show significantly less background scattering than other setups. A variety of cognate holders for patches of Mylar in situ sandwich films corresponding to one or more wells makes the method robust and versatile, allows for storage and shipping of entire wells, and enables automated crystal imaging, screening, and goniometer-based X-ray diffraction data-collection at room temperature and under cryogenic conditions for soluble and membrane-protein crystals grown in or transferred to these plates. We validated the Mylar in situ method using crystals of the water-soluble proteins hen egg-white lysozyme and sperm whale myoglobin as well as the 7-transmembrane protein bacteriorhodopsin from Haloquadratum walsbyi. In conjunction with current developments at synchrotrons, this approach promises high-resolution structural studies of membrane proteins to become faster and more routine. PMID:28261000

  16. High-pressure behavior and thermoelastic properties of niobium studied by in situ x-ray diffraction

    SciTech Connect

    Zou, Yongtao E-mail: yongtaozou6@gmail.com; Li, Baosheng; Qi, Xintong; Wang, Xuebing; Chen, Ting; Li, Xuefei; Welch, David

    2014-07-07

    In situ synchrotron energy dispersive x-ray diffraction (XRD) experiments on Nb have been conducted at pressures up to 6.4 GPa and temperatures up to 1073 K. From the pressure-volume-temperature measurements, thermoelastic parameters were derived for the first time for Nb based on the thermal pressure (ΔP{sub th}) equation of state (EOS), modified high-T Birch-Murnaghan EOS, and Mie-Grüneisen-Debye EOS. With the pressure derivative of the bulk modulus K{sub T}{sup ´} fixed at 4.0, we obtained the ambient isothermal bulk modulus K{sub T0}=174(5) GPa, the temperature derivative of bulk modulus at constant pressure (∂K{sub T}/∂T){sub P}=-0.060(8) GPa K⁻¹ and at constant volume (∂K{sub T}/∂T){sub V}=-0.046(8) GPa K⁻¹, the volumetric thermal expansivity α{sub T}(T)=2.3(3)×10⁻⁵+0.3(2)×10⁻⁸T (K⁻¹), as well as the pressure dependence of thermal expansion (∂α/∂P){sub T}=(₋2.0±0.4)×10⁻⁶ K⁻¹ GPa⁻¹. Fitting the present data to the Mie-Grüneisen-Debye EOS with Debye temperature Θ₀=276.6 K gives γ₀=1.27(8) and K{sub T0}=171(3) GPa at a fixed value of q=3.0. The ambient isothermal bulk modulus and Grüneisen parameter derived from this work are comparable to previously reported values from both experimental and theoretical studies. An in situ high-resolution, angle dispersive XRD study on Nb did not indicate any anomalous behavior related to pressure-induced electronic topological transitions at ~5 GPa as has been reported previously.

  17. Satellite-derived surface temperature and in situ measurement at Solfatara of Pozzuoli (Naples, Italy)

    NASA Astrophysics Data System (ADS)

    Silvestri, M.; Cardellini, C.; Chiodini, G.; Buongiorno, M. F.

    2016-06-01

    Ground thermal anomalies in volcanic-hydrothermal systems, where the outflow of hot fluids gives rise to fumarolic fields, soil degassing, and hot soils, have, up to now, rarely been investigated by using satellite. Here we report a comparison between surface temperature derived by satellite data and a large data set of measured soil temperatures and CO2 fluxes for a volcanic-hydrothermal system, the Solfatara of Pozzuoli (Campi Flegrei, Italy). Surface temperatures derived from ASTER (Advanced Spaceborne Thermal Emission and Reflection Radiometer) data are compared with soil temperatures and CO2 fluxes from four surveys performed in 2003, 2010, and in 2014. The good match between the spatial distributions of computed and measured temperatures suggests the adequacy of satellite data to describe the Solfatara thermal anomaly, while the correspondence between temperatures and CO2 fluxes, evidences the link between degassing and heating processes. The ASTER derived surface temperatures (14-37°C) are coherent with those measured in the soil (10-97°C at 10 cm depth), considering the effect of the thermal gradients which characterize the degassing area of Solfatara. This study shows that satellite data can be a very powerful tool with which to study surface thermal anomalies, and can provide a supplementary tool to monitor thermal evolution of restless volcanoes.

  18. High Temperature Structural Foam

    NASA Technical Reports Server (NTRS)

    Weiser, Erik S.; Baillif, Faye F.; Grimsley, Brian W.; Marchello, Joseph M.

    1997-01-01

    The Aerospace Industry is experiencing growing demand for high performance polymer foam. The X-33 program needs structural foam insulation capable of retaining its strength over a wide range of environmental conditions. The High Speed Research Program has a need for low density core splice and potting materials. This paper reviews the state of the art in foam materials and describes experimental work to fabricate low density, high shear strength foam which can withstand temperatures from -220 C to 220 C. Commercially available polymer foams exhibit a wide range of physical properties. Some with densities as low as 0.066 g/cc are capable of co-curing at temperatures as high as 182 C. Rohacell foams can be resin transfer molded at temperatures up to 180 C. They have moduli of elasticity of 0.19 MPa, tensile strengths of 3.7 Mpa and compressive strengths of 3.6 MPa. The Rohacell foams cannot withstand liquid hydrogen temperatures, however Imi-Tech markets Solimide (trademark) foams which withstand temperatures from -250 C to 200 C, but they do not have the required structural integrity. The research activity at NASA Langley Research Center focuses on using chemical blowing agents to produce polyimide thermoplastic foams capable of meeting the above performance requirements. The combination of blowing agents that decompose at the minimum melt viscosity temperature together with plasticizers to lower the viscosity has been used to produce foams by both extrusion and oven heating. The foams produced exhibit good environmental stability while maintaining structural properties.

  19. In-Situ Acoustic Measurements of Temperature Profile in Extreme Environments

    SciTech Connect

    Skliar, Mikhail

    2015-03-31

    A gasifier’s temperature is the primary characteristic that must be monitored to ensure its performance and the longevity of its refractory. One of the key technological challenges impacting the reliability and economics of coal and biomass gasification is the lack of temperature sensors that are capable of providing accurate, reliable, and long-life performance in an extreme gasification environment. This research has proposed, demonstrated, and validated a novel approach that uses a noninvasive ultrasound method that provides real-time temperature distribution monitoring across the refractory, especially the hot face temperature of the refractory. The essential idea of the ultrasound measurements of segmental temperature distribution is to use an ultrasound propagation waveguide across a refractory that has been engineered to contain multiple internal partial reflectors at known locations. When an ultrasound excitation pulse is introduced on the cold side of the refractory, it will be partially reflected from each scatterer in the US propagation path in the refractory wall and returned to the receiver as a train of partial echoes. The temperature in the corresponding segment can be determined based on recorded ultrasonic waveform and experimentally defined relationship between the speed of sound and temperature. The ultrasound measurement method offers a powerful solution to provide continuous real time temperature monitoring for the occasions that conventional thermal, optical and other sensors are infeasible, such as the impossibility of insertion of temperature sensor, harsh environment, unavailable optical path, and more. Our developed ultrasound system consists of an ultrasound engineered waveguide, ultrasound transducer/receiver, and data acquisition, logging, interpretation, and online display system, which is simple to install on the existing units with minimal modification on the gasifier or use with new units. This system has been successfully tested

  20. High-Temperature Superconductivity

    ScienceCinema

    Peter Johnson

    2016-07-12

    Like astronomers tweaking images to gain a more detailed glimpse of distant stars, physicists at Brookhaven National Laboratory have found ways to sharpen images of the energy spectra in high-temperature superconductors — materials that carry electrical c

  1. HIGH TEMPERATURE THERMOCOUPLE

    DOEpatents

    Eshayu, A.M.

    1963-02-12

    This invention contemplates a high temperature thermocouple for use in an inert or a reducing atmosphere. The thermocouple limbs are made of rhenium and graphite and these limbs are connected at their hot ends in compressed removable contact. The rhenium and graphite are of high purity and are substantially stable and free from diffusion into each other even without shielding. Also, the graphite may be thick enough to support the thermocouple in a gas stream. (AEC)

  2. A simple method for in situ monitoring of water temperature in substrates used by spawning salmonids

    USGS Publications Warehouse

    Zimmerman, Christian E.; Finn, James E.

    2012-01-01

    Interstitial water temperature within spawning habitats of salmonids may differ from surface-water temperature depending on intragravel flow paths, geomorphic setting, or presence of groundwater. Because survival and developmental timing of salmon are partly controlled by temperature, monitoring temperature within gravels used by spawning salmonids is required to adequately describe the environment experienced by incubating eggs and embryos. Here we describe a simple method of deploying electronic data loggers within gravel substrates with minimal alteration of the natural gravel structure and composition. Using data collected in spawning sites used by summer and fall chum salmon Oncorhynchus keta from two streams within the Yukon River watershed, we compare contrasting thermal regimes to demonstrate the utility of this method.

  3. Low temperature engineering applied to lunar in-situ resource utilization

    NASA Technical Reports Server (NTRS)

    Zhang, Burt; Chui, Talso; Croonquist, Arvid

    2005-01-01

    In support of NASA's Exploration Mission low-temperature scientists and engineers have investigated the process of extracting volatile materials from the lunar regolith, their purification/liquefaction, and storage.

  4. Real-time monitoring of high-gravity corn mash fermentation using in situ raman spectroscopy.

    PubMed

    Gray, Steven R; Peretti, Steven W; Lamb, H Henry

    2013-06-01

    In situ Raman spectroscopy was employed for real-time monitoring of simultaneous saccharification and fermentation (SSF) of corn mash by an industrial strain of Saccharomyces cerevisiae. An accurate univariate calibration model for ethanol was developed based on the very strong 883 cm(-1) C-C stretching band. Multivariate partial least squares (PLS) calibration models for total starch, dextrins, maltotriose, maltose, glucose, and ethanol were developed using data from eight batch fermentations and validated using predictions for a separate batch. The starch, ethanol, and dextrins models showed significant prediction improvement when the calibration data were divided into separate high- and low-concentration sets. Collinearity between the ethanol and starch models was avoided by excluding regions containing strong ethanol peaks from the starch model and, conversely, excluding regions containing strong saccharide peaks from the ethanol model. The two-set calibration models for starch (R(2)  = 0.998, percent error = 2.5%) and ethanol (R(2)  = 0.999, percent error = 2.1%) provide more accurate predictions than any previously published spectroscopic models. Glucose, maltose, and maltotriose are modeled to accuracy comparable to previous work on less complex fermentation processes. Our results demonstrate that Raman spectroscopy is capable of real time in situ monitoring of a complex industrial biomass fermentation. To our knowledge, this is the first PLS-based chemometric modeling of corn mash fermentation under typical industrial conditions, and the first Raman-based monitoring of a fermentation process with glucose, oligosaccharides and polysaccharides present.

  5. Validating Satellite-Derived Land Surface Temperature with in Situ Measurements: A Public Health Perspective

    PubMed Central

    Brines, Shannon J.; Brown, Daniel G.; Dvonch, J. Timothy; Gronlund, Carina J.; Zhang, Kai; Oswald, Evan M.; O’Neill, Marie S.

    2013-01-01

    Background: Land surface temperature (LST) and percent surface imperviousness (SI), both derived from satellite imagery, have been used to characterize the urban heat island effect, a phenomenon in which urban areas are warmer than non-urban areas. Objectives: We aimed to assess the correlations between LSTs and SI images with actual temperature readings from a ground-based network of outdoor monitors. Methods: We evaluated the relationships among a) LST calculated from a 2009 summertime satellite image of the Detroit metropolitan region, Michigan; b) SI from the 2006 National Land Cover Data Set; and c) ground-based temperature measurements monitored during the same time period at 19 residences throughout the Detroit metropolitan region. Associations between these ground-based temperatures and the average LSTs and SI at different radii around the point of the ground-based temperature measurement were evaluated at different time intervals. Spearman correlation coefficients and corresponding p-values were calculated. Results: Satellite-derived LST and SI values were significantly correlated with 24-hr average and August monthly average ground temperatures at all but two of the radii examined (100 m for LST and 0 m for SI). Correlations were also significant for temperatures measured between 0400 and 0500 hours for SI, except at 0 m, but not LST. Statistically significant correlations ranging from 0.49 to 0.91 were observed between LST and SI. Conclusions: Both SI and LST could be used to better understand spatial variation in heat exposures over longer time frames but are less useful for estimating shorter-term, actual temperature exposures, which can be useful for public health preparedness during extreme heat events. PMID:23777856

  6. High temperature thermometric phosphors

    DOEpatents

    Allison, S.W.; Cates, M.R.; Boatner, L.A.; Gillies, G.T.

    1999-03-23

    A high temperature phosphor consists essentially of a material having the general formula LuPO{sub 4}:Dy{sub x},Eu{sub y} wherein: 0.1 wt % {<=} x {<=} 20 wt % and 0.1 wt % {<=} y {<=} 20 wt %. The high temperature phosphor is in contact with an article whose temperature is to be determined. The article having the phosphor in contact with it is placed in the environment for which the temperature of the article is to be determined. The phosphor is excited by a laser causing the phosphor to fluoresce. The emission from the phosphor is optically focused into a beam-splitting mirror which separates the emission into two separate emissions, the emission caused by the dysprosium dopant and the emission caused by the europium dopant. The separated emissions are optically filtered and the intensities of the emission are detected and measured. The ratio of the intensity of each emission is determined and the temperature of the article is calculated from the ratio of the intensities of the separate emissions. 2 figs.

  7. High temperature thermometric phosphors

    DOEpatents

    Allison, Stephen W.; Cates, Michael R.; Boatner, Lynn A.; Gillies, George T.

    1999-03-23

    A high temperature phosphor consists essentially of a material having the general formula LuPO.sub.4 :Dy.sub.(x),Eu.sub.y) wherein: 0.1 wt %.ltoreq.x.ltoreq.20 wt % and 0.1 wt %.ltoreq.y.ltoreq.20 wt %. The high temperature phosphor is in contact with an article whose temperature is to be determined. The article having the phosphor in contact with it is placed in the environment for which the temperature of the article is to be determined. The phosphor is excited by a laser causing the phosphor to fluoresce. The emission from the phosphor is optically focused into a beam-splitting mirror which separates the emission into two separate emissions, the emission caused by the dysprosium dopant and the emission caused by the europium dopent. The separated emissions are optically filtered and the intensities of the emission are detected and measured. The ratio of the intensity of each emission is determined and the temperature of the article is calculated from the ratio of the intensities of the separate emissions.

  8. Low-temperature atomic layer epitaxy of AlN ultrathin films by layer-by-layer, in-situ atomic layer annealing

    PubMed Central

    Shih, Huan-Yu; Lee, Wei-Hao; Kao, Wei-Chung; Chuang, Yung-Chuan; Lin, Ray-Ming; Lin, Hsin-Chih; Shiojiri, Makoto; Chen, Miin-Jang

    2017-01-01

    Low-temperature epitaxial growth of AlN ultrathin films was realized by atomic layer deposition (ALD) together with the layer-by-layer, in-situ atomic layer annealing (ALA), instead of a high growth temperature which is needed in conventional epitaxial growth techniques. By applying the ALA with the Ar plasma treatment in each ALD cycle, the AlN thin film was converted dramatically from the amorphous phase to a single-crystalline epitaxial layer, at a low deposition temperature of 300 °C. The energy transferred from plasma not only provides the crystallization energy but also enhances the migration of adatoms and the removal of ligands, which significantly improve the crystallinity of the epitaxial layer. The X-ray diffraction reveals that the full width at half-maximum of the AlN (0002) rocking curve is only 144 arcsec in the AlN ultrathin epilayer with a thickness of only a few tens of nm. The high-resolution transmission electron microscopy also indicates the high-quality single-crystal hexagonal phase of the AlN epitaxial layer on the sapphire substrate. The result opens a window for further extension of the ALD applications from amorphous thin films to the high-quality low-temperature atomic layer epitaxy, which can be exploited in a variety of fields and applications in the near future. PMID:28045075

  9. Low-temperature atomic layer epitaxy of AlN ultrathin films by layer-by-layer, in-situ atomic layer annealing

    NASA Astrophysics Data System (ADS)

    Shih, Huan-Yu; Lee, Wei-Hao; Kao, Wei-Chung; Chuang, Yung-Chuan; Lin, Ray-Ming; Lin, Hsin-Chih; Shiojiri, Makoto; Chen, Miin-Jang

    2017-01-01

    Low-temperature epitaxial growth of AlN ultrathin films was realized by atomic layer deposition (ALD) together with the layer-by-layer, in-situ atomic layer annealing (ALA), instead of a high growth temperature which is needed in conventional epitaxial growth techniques. By applying the ALA with the Ar plasma treatment in each ALD cycle, the AlN thin film was converted dramatically from the amorphous phase to a single-crystalline epitaxial layer, at a low deposition temperature of 300 °C. The energy transferred from plasma not only provides the crystallization energy but also enhances the migration of adatoms and the removal of ligands, which significantly improve the crystallinity of the epitaxial layer. The X-ray diffraction reveals that the full width at half-maximum of the AlN (0002) rocking curve is only 144 arcsec in the AlN ultrathin epilayer with a thickness of only a few tens of nm. The high-resolution transmission electron microscopy also indicates the high-quality single-crystal hexagonal phase of the AlN epitaxial layer on the sapphire substrate. The result opens a window for further extension of the ALD applications from amorphous thin films to the high-quality low-temperature atomic layer epitaxy, which can be exploited in a variety of fields and applications in the near future.

  10. In situ supported MnOx-CeOx on carbon nanotubes for the low-temperature selective catalytic reduction of NO with NH3

    NASA Astrophysics Data System (ADS)

    Zhang, Dengsong; Zhang, Lei; Shi, Liyi; Fang, Cheng; Li, Hongrui; Gao, Ruihua; Huang, Lei; Zhang, Jianping

    2013-01-01

    The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ prepared catalyst exhibited the highest activity and the most extensive operating-temperature window, compared to the catalysts prepared by impregnation or mechanically mixed methods. The XRD and TEM results indicated that the manganese oxide and cerium oxide species had a good dispersion on the CNT surface. The XPS results demonstrated that the higher atomic concentration of Mn existed on the surface of CNTs and the more chemisorbed oxygen species exist. The H2-TPR results suggested that there was a strong interaction between the manganese oxide and cerium oxide on the surface of CNTs. The NH3-TPD results demonstrated that the catalysts presented a larger acid amount and stronger acid strength. In addition, the obtained catalysts exhibited much higher SO2-tolerance and improved the water-resistance as compared to that prepared by impregnation or mechanically mixed methods.The MnOx and CeOx were in situ supported on carbon nanotubes (CNTs) by a poly(sodium 4-styrenesulfonate) assisted reflux route for the low-temperature selective catalytic reduction (SCR) of NO with NH3. X-Ray diffraction (XRD), transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray photoelectron spectroscopy (XPS), H2 temperature-programmed reduction (H2-TPR) and NH3 temperature-programmed desorption (NH3-TPD) have been used to elucidate the structure and surface properties of the obtained catalysts. It was found that the in situ

  11. In-Situ Formed Type I Nanocrystalline Perovskite Film for Highly Efficient Light-Emitting Diode.

    PubMed

    Lee, Jin-Wook; Choi, Yung Ji; Yang, June-Mo; Ham, Sujin; Jeon, Sang Kyu; Lee, Jun Yeob; Song, Young-Hyun; Ji, Eun Kyung; Yoon, Dae-Ho; Seo, Seongrok; Shin, Hyunjung; Han, Gil Sang; Jung, Hyun Suk; Kim, Dongho; Park, Nam-Gyu

    2017-03-28

    Excellent color purity with a tunable band gap renders organic-inorganic halide perovskite highly capable of performing as light-emitting diodes (LEDs). Perovskite nanocrystals show a photoluminescence quantum yield exceeding 90%, which, however, decreases to lower than 20% upon formation of a thin film. The limited photoluminescence quantum yield of a perovskite thin film has been a formidable obstacle for development of highly efficient perovskite LEDs. Here, we report a method for highly luminescent MAPbBr3 (MA = CH3NH3) nanocrystals formed in situ in a thin film based on nonstoichiometric adduct and solvent-vacuum drying approaches. Excess MABr with respect to PbBr2 in precursor solution plays a critical role in inhibiting crystal growth of MAPbBr3, thereby forming nanocrystals and creating type I band alignment with core MAPbBr3 by embedding MAPbBr3 nanocrystals in the unreacted wider band gap MABr. A solvent-vacuum drying process was developed to preserve nanocrystals in the film, which realizes a fast photoluminescence lifetime of 3.9 ns along with negligible trapping processes. Based on a highly luminescent nanocrystalline MAPbBr3 thin film, a highly efficient green LED with a maximum external quantum efficiency of 8.21% and a current efficiency of 34.46 cd/A was demonstrated.

  12. Phenomenological in-situ TEM gas exposure studies of palladium particles on MgO at room temperature

    NASA Technical Reports Server (NTRS)

    Heinemann, K.; Poppa, H.; Osaka, T.

    1983-01-01

    It has been found that very small vapor-deposited catalytically active metal particles in the 1-2 nm size range on metal oxide substrates can undergo significant changes when they are exposed to gases such as oxygen or air, or even when allowed to 'anneal' at room temperature (RT) under vacuum conditions. The present investigation is concerned with continued in-situ gas exposures of as-deposited, 1 to 2 nm size palladium particles on MgO to air, oxygen, nitrogen, hydrogen, CO, and water vapor at RT. It is found that the low-pressure exposure to various gases at RT can significantly affect small palladium particles supported on MgO surfaces. Exposure to oxygen for 3 min at 0.0002 m bar produces a considerable amount of coalescence, flattening of the particles, and some distinct crystallographic particle shapes.

  13. Comparison of evaporative fluxes from porous surfaces resolved by remotely sensed and in-situ temperature and soil moisture data

    NASA Astrophysics Data System (ADS)

    Wallen, B.; Trautz, A.; Smits, K. M.

    2014-12-01

    The estimation of evaporation has important implications in modeling climate at the regional and global scale, the hydrological cycle and estimating environmental stress on agricultural systems. In field and laboratory studies, remote sensing and in-situ techniques are used to collect thermal and soil moisture data of the soil surface and subsurface which is then used to estimate evaporative fluxes, oftentimes using the sensible heat balance method. Nonetheless, few studies exist that compare the methods due to limited data availability and the complexity of many of the techniques, making it difficult to understand flux estimates. This work compares different methods used to quantify evaporative flux based on remotely sensed and in-situ temperature and soil moisture data. A series of four laboratory experiments were performed under ambient and elevated air temperature conditions with homogeneous and heterogeneous soil configurations in a small two-dimensional soil tank interfaced with a small wind tunnel apparatus. The soil tank and wind tunnel were outfitted with a suite of sensors that measured soil temperature (surface and subsurface), air temperature, soil moisture, and tank weight. Air and soil temperature measurements were obtained using infrared thermography, heat pulse sensors and thermistors. Spatial and temporal thermal data were numerically inverted to obtain the evaporative flux. These values were then compared with rates of mass loss from direct weighing of the samples. Results demonstrate the applicability of different methods under different surface boundary conditions; no one method was deemed most applicable under every condition. Infrared thermography combined with the sensible heat balance method was best able to determine evaporative fluxes under stage 1 conditions while distributed temperature sensing combined with the sensible heat balance method best determined stage 2 evaporation. The approaches that appear most promising for determining the

  14. Influence of temperature on layer growth as measured by in situ XRD observation of nitriding of austenitic stainless steel

    NASA Astrophysics Data System (ADS)

    Manova, D.; Günther, C.; Bergmann, A.; Mändl, S.; Neumann, H.; Rauschenbach, B.

    2013-07-01

    Investigating the formation of expanded austenite has resulted in several, different models trying to explain the particular diffusion and phase formation behaviour. However, only ex situ information, influenced by cooling and annealing processes of the samples after ion implantation has been available until now. Here, the time and temperature dependent layer growth is reported using in situ XRD measurements obtained from low energy broadbeam nitrogen ion implantation into polycrystalline austenitic stainless steel 304 in the temperature range from 300 to 500 °C for a process time of up to 1 h. Expanded austenite was observed at all temperatures without any CrN, in agreement with already published lifetime data for this metastable phase. The layer growth was derived from the time evolution of the substrate peak intensity. Using the temperature dependence of the layer growth, an activation energy of nearly 0.8 eV was estimated for the nitrogen diffusion. In contrast, a complex behaviour was observed for the lattice expansion and peak width of the expanded peak, indicating additional dynamic annealing during implantation.

  15. In situ investigation of aggregate sizes formed using thermo-responsive polymers: Effect of temperature and shear.

    PubMed

    Ng, Wei Sung; Connal, Luke A; Forbes, Elizaveta; Mohanarangam, Krishna; Franks, George V

    2017-05-15

    Temperature-responsive flocculants, such as poly(N-isopropylacrylamide) (PNIPAM), induce reversible particle aggregation upon heating above a lower critical solution temperature (LCST). The aim of this work is to investigate the aggregation of ground iron ore using PNIPAM and conventional polyacrylamide (PAM) flocculants in a continuously-sheared suspension, through in situ chord length measurements using Focused Beam Reflectance Measurement techniques and real-time imaging of the particle aggregates. In the presence of uncharged PNIPAM, particle aggregation occurs only upon heating to the LCST, and the aggregates continue to grow with further heating. Subsequent cooling re-disperses the aggregates, and repeated heating causes reformation. Unlike uncharged PNIPAM, anionic PNIPAM produces aggregates at temperatures below the LCST due to the polymer chains binding to two different particles via attractive interactions between the acrylic acid groups and the hematite surfaces, and can be added at temperatures above the LCST due to the formation of charge-stabilised micelles. Under continuous shear, the flocculant most able to resist aggregate size reduction was anionic PAM, followed by PAM, anionic PNIPAM, PNIPAM (6MDa), and PNIPAM (122kDa). Reversible aggregate breakage was found with all samples, except with PNIPAM (6MDa) after being subjected to shear rates above 550s(-1). Furthermore, heating of the PNIPAM-dosed suspensions at shear rates below 200s(-1) produced larger and more breakage-resistant aggregates.

  16. In Situ GISAXS investigation of low-temperature aging in oriented surfactant-mesostructured titania thin films

    DOE PAGES

    Nagpure, Suraj; Das, Saikat; Garlapalli, Ravinder K.; ...

    2015-09-11

    In this study, the mechanism of forming orthogonally oriented hexagonal close packed (o-HCP) mesostructures during aging of surfactant-templated titania thin films is elucidated using in situ grazing incidence small-angle x-ray scattering (GISAXS) in a controlled-environment chamber. To promote orthogonal orientation, glass slides are modified with crosslinked Pluronic P123, to provide surfaces chemically neutral towards both blocks of mesophase template P123. At 4 °C and 80% RH, the o-HCP mesophase emerges in thin (~60 nm) films by a direct disorder-to-order transition, with no intermediate ordered mesophase. The Pluronic/titania o-HCP GISAXS intensity emerges only after ~10-12 minutes, much slower than previously reportedmore » for smallmolecule surfactants. The Avrami model applied to the data suggests 2D growth with nucleation at the start of the process with a half-life of 39.7 minutes for the aging time just after the induction period of 7 minutes followed by a period consistent with 1D growth kinetics. Surprisingly, films that are thicker (~250 nm) or cast on unmodified slides form o-HCP mesophase domains, but by a different mechanism (2D growth with continuous nucleation) with faster and less complete orthogonal alignment. Thus, the o-HCP mesophase is favored not only 2 by modifying the substrate, but also by aging at 4 °C, which is below the lower consolute temperature (LCST) of the poly(propylene oxide) block of P123. Consistent with this, in situ GISAXS shows that films aged at room temperature (above the LCST of the PPO block) have randomly oriented HCP mesostructure.« less

  17. In-situ monitoring of internal local temperature and voltage of proton exchange membrane fuel cells.

    PubMed

    Lee, Chi-Yuan; Fan, Wei-Yuan; Hsieh, Wei-Jung

    2010-01-01

    The distribution of temperature and voltage of a fuel cell are key factors that influence performance. Conventional sensors are normally large, and are also useful only for making external measurements of fuel cells. Centimeter-scale sensors for making invasive measurements are frequently unable to accurately measure the interior changes of a fuel cell. This work focuses mainly on fabricating flexible multi-functional microsensors (for temperature and voltage) to measure variations in the local temperature and voltage of proton exchange membrane fuel cells (PEMFC) that are based on micro-electro-mechanical systems (MEMS). The power density at 0.5 V without a sensor is 450 mW/cm(2), and that with a sensor is 426 mW/cm(2). Since the reaction area of a fuel cell with a sensor is approximately 12% smaller than that without a sensor, but the performance of the former is only 5% worse.

  18. Analysis of continuous multi-seasonal in-situ subsurface temperature measurements on Mars

    NASA Astrophysics Data System (ADS)

    Paton, M. D.; Harri, A.-M.; Mäkinen, T.; Savijärvi, H.; Kemppinen, O.; Hagermann, A.

    2015-10-01

    Our investigations reveal the local thermal properties on the Martian surface at the Viking Lander 1 (VL-1) site. We achieved this by using the VL-1 footpad temperature sensor which was buried, and due to its location, was under shadow for extensive periods of time during each sol. Reconstruction of the surface and subsurface temperature history of the regolith in the vicinity of the temperature sensor was made using a 1-D atmospheric column model (UH-FMI) together with a thermal model of the lander. The results have implications for the interpretation of subsurface thermal measurements made close to a spacecraft or rock, interpretation of remote sensing measurements of thermal inertia and understanding the micro-scale behavior of the Martian atmosphere.

  19. High temperature adsorption measurements

    SciTech Connect

    Bertani, R.; Parisi, L.; Perini, R.; Tarquini, B.

    1996-12-31

    Adsorption phenomena are a rich and rather new field of study in geothermal research, in particular at very high temperature. ENEL is interested in the exploitation of geothermal regions with super-heated steam, and it is important to understand the behavior of water-rock interaction. We have analyzed in the 170-200{degrees}C temperature range four samples of Monteverdi cuttings; the next experimental effort will be at 220{degrees}C and over in 1996. The first results of the 1995 runs are collected in this paper. We can highlight four main items: (1) At relative pressures over 0.6 the capillarity forces are very important. (2) There is no significant temperature effect. (3) Adsorbed water can be present, and it is able to multiply by a factor of 15 the estimated reserve of super-heated steam only. (4) Pores smaller than 15 {Angstrom} do not contribute to the adsorbed mass.

  20. High temperature adsorption measurements

    SciTech Connect

    Bertani, R.; Parisi, L.; Perini, R.; Tarquini, B.

    1996-01-24

    Adsorption phenomena are a rich and rather new field of study in geothermal research, in particular at very high temperature. ENEL is interested in the exploitation of geothermal regions with superheated steam, and it is important to understand the behavior of water-rock interaction. We have analyzed in the 170-200 °C temperature range four samples of Monteverdi cuttings; the next experimental effort will be at 220 °C and over in 1996. The first results of the 1995 runs are collected in this paper. We can highlight four main items: 1. At relative pressures over 0.6 the capillarity forces are very important. 2. There is no significant temperature effect. 3. Adsorbed water can be present, and it is able to multiply by a factor of 15 the estimated reserve of super-heated steam only. 4. Pores smaller than 15 Å do not contribute to the adsorbed mass.

  1. In Situ Determination of Manganese(II) Speciation in Deinococcus radiodurans by High Magnetic Field EPR

    PubMed Central

    Tabares, Leandro C.; Un, Sun

    2013-01-01

    High magnetic field high frequency electron paramagnetic resonance techniques were used to measure in situ Mn(II) speciation in Deinococcus radiodurans, a radiation-resistant bacteria capable of accumulating high concentrations of Mn(II). It was possible to identify and quantify the evolution of Mn(II) species in intact cells at various stages of growth. Aside from water, 95-GHz high field electron nuclear double resonance showed that the Mn(II) ions are bound to histidines and phosphate groups, mostly from fructose-1,6-bisphosphate but also inorganic phosphates and nucleotides. During stationary growth phase, 285-GHz continuous wave EPR measurements showed that histidine is the most common ligand to Mn(II) and that significant amounts of cellular Mn(II) in D. radiodurans are bound to peptides and proteins. As much as 40% of the total Mn(II) was in manganese superoxide dismutase, and it is this protein and not smaller manganese complexes, as has been suggested recently, that is probably the primary defense against superoxide. PMID:23303180

  2. In Situ Visualization of Tears on Contact Lens Using Ultra High Resolution Optical Coherence Tomography

    PubMed Central

    Wang, Jianhua; Jiao, Shuliang; Ruggeri, Marco; Shousha, Mohammed Abou; Chen, Qi

    2012-01-01

    Objective To demonstrate the capability of directly visualizing the tear film on contact lenses using optical coherence tomography (OCT). Methods Six eyes of three healthy subjects wearing PureVision and ACUVUE Advance soft and Boston RGP hard contact lenses were imaged with a custom built, high speed, ultra-high resolution spectral domain optical coherence tomograph. Refresh Liquigel was used to demonstrate the effect of artificial tears on the tear film. Results Ultra high resolution images of the pre- and post-lens films were directly visualized when each lens was inserted onto the eye. After the instillation of artificial tears during lens wear, the tear film was thicker. The post-lens tear film underneath the lens edge was clearly shown. Interactions between the lens edges and the ocular surface were obtained for each of the lens types and base curves. With a contrast enhancement agent, tear menisci on the contact lenses around the upper and lower eyelids were highlighted. With hard contact lenses, the tear film was visualized clearly and changed after a blink when the lens was pulled up by the lid. Conclusions Ultra-high resolution OCT is a potentially promising technique for imaging tears around contact lenses. This successful demonstration of in situ post-lens tear film imaging suggests that OCT could open a new era in studying tear dynamics during contact lens wear. The novel method may lead to new ways of evaluating contact lens fitting. PMID:19265323

  3. An in situ high voltage electron microscopy technique for the study of deformation and fracture: In multilayered materials

    SciTech Connect

    Wall, M.A.; Barbee, T.W. Jr.; Weihs, T.P.

    1995-04-14

    A novel, in situ, high voltage electron microscopy technique for the direct observation of the micromechanisms of tensile deformation and fracture in nanostructured materials is detailed. This technique is particularly well suited for the dynamic observations of deformation and fracture in multilayered materials. The success of this type of in situ technique is highly dependent upon unique specimen preparation procedures and sample design, the importance thereof will be discussed. The initial observations discussed here are expected to aid in the understanding of the mechanical behavior of this new class of atomically engineered materials.

  4. In situ study of maize starch gelatinization under ultra-high hydrostatic pressure using X-ray diffraction.

    PubMed

    Yang, Zhi; Gu, Qinfen; Hemar, Yacine

    2013-08-14

    The gelatinization of waxy (very low amylose) and high-amylose maize starches by ultra-high hydrostatic pressure (up to 6 GPa) was investigated in situ using synchrotron X-ray powder diffraction on samples held in a diamond anvil cell (DAC). The starch pastes, made by mixing starch and water in a 1:1 ratio, were pressurized and measured at room temperature. X-ray diffraction pattern showed that at 2.7 GPa waxy starch, which displayed A-type XRD pattern at atmospheric pressure, exhibited a faint B-type-like pattern. The B-type crystalline structures of high-amylose starch were not affected even when 1.5 GPa pressure was applied. However, both waxy and high-amylose maize starches can be fully gelatinized at 5.9 GPa and 5.1 GPa, respectively. In the case of waxy maize starch, upon release of pressure (to atmospheric pressure) crystalline structure appeared as a result of amylopectin aggregation.

  5. 1 kW imaging furnace with in situ measurement of surface temperature

    NASA Astrophysics Data System (ADS)

    Guesdon, Christine; Alxneit, Ivo; Tschudi, Hans Rudolf; Wuillemin, Daniel; Sturzenegger, Marcel

    2006-03-01

    This article describes the development and characterization of a 1kW imaging furnace that allows to investigate materials such as sulfides at ultrahigh temperatures under controlled atmosphere. Peak flux densities up to (15.37±0.66)×106Wm-2 corresponding to a maximum stagnation temperature of 3090K can be reached in the center of the heating zone of 3mm diameter (full width at half height). Individual sample holders can be mounted on a generic sample stage that is aligned in three axes. Together they define an experiment. Experiments can thus be easily interchanged without requiring any realignment. The use of a specific sample holder is reported where the sample rests on a water-cooled tip to avoid contamination by crucible material and where a protective glass dome can be mounted to allow the study of samples releasing condensable or corrosive gases. With the dome in place the peak flux density decreases to a value of (13.59±0.45)×106Wm-2 (Tstag=2980K). The surface temperature of the sample and the average irradiance can be measured simultaneously by the pyrometric method flash assisted multiwavelength pyrometry. The irradiance on the sample and, thus, the temperature reached can be controlled by adjusting the position of the sample. This is effected by a computer controlled fork lift with a resolution of 0.05mm.

  6. Magic angle spinning nuclear magnetic resonance apparatus and process for high-resolution in situ investigations

    SciTech Connect

    Hu, Jian Zhi; Sears, Jr., Jesse A.; Hoyt, David W.; Mehta, Hardeep S.; Peden, Charles H. F.

    2015-11-24

    A continuous-flow (CF) magic angle sample spinning (CF-MAS) NMR rotor and probe are described for investigating reaction dynamics, stable intermediates/transition states, and mechanisms of catalytic reactions in situ. The rotor includes a sample chamber of a flow-through design with a large sample volume that delivers a flow of reactants through a catalyst bed contained within the sample cell allowing in-situ investigations of reactants and products. Flow through the sample chamber improves diffusion of reactants and products through the catalyst. The large volume of the sample chamber enhances sensitivity permitting in situ .sup.13C CF-MAS studies at natural abundance.

  7. Aerosol-Cloud Interaction Determined by Both in Situ and Satellite Data Over a Northern High-Latitude Site

    NASA Technical Reports Server (NTRS)

    Lihavainen, H.; Kerminen, V.-M.; Remer, L. A.

    2009-01-01

    The first aerosol indirect effect over a clean, northern high-latitude site was investigated by determining the aerosol cloud interaction (ACI) using three different approaches; ground-based in situ measurements, combined ground-based in situ measurements 5 and satellite retrievals and using only satellite retrievals. The obtained values of ACI were highest for in situ ground-based data, clearly lower for combined ground-based and satellite data, and lowest for data relying solely on satellite retrievals. One of the key findings of this study was the high sensitivity of ACI to the definition of the aerosol burden. We showed that at least a part of the variability in ACI can be explained by 10 how different investigators have related dierent cloud properties to "aerosol burden".

  8. High temperature materials characterization

    NASA Technical Reports Server (NTRS)

    Workman, Gary L.

    1990-01-01

    A lab facility for measuring elastic moduli up to 1700 C was constructed and delivered. It was shown that the ultrasonic method can be used to determine elastic constants of materials from room temperature to their melting points. The ease in coupling high frequency acoustic energy is still a difficult task. Even now, new coupling materials and higher power ultrasonic pulsers are being suggested. The surface was only scratched in terms of showing the full capabilities of either technique used, especially since there is such a large learning curve in developing proper methodologies to take measurements into the high temperature region. The laser acoustic system does not seem to have sufficient precision at this time to replace the normal buffer rod methodology.

  9. High temperature future

    SciTech Connect

    Sheinkopf, K.

    1994-09-01

    During the past few years, there have been dramatic accomplishments and success of high temperature solar thermal systems and significant development of these systems. High temperature technologies, about 500 F and higher, such as dish engines, troughs, central receiver power towers and solar process heat systems, have been tested, demonstrated and used in an array of applications, including many cost-effective utility bulk power production and demand side supply projects in the United States. Large systems provide power and hot water to prisons, schools, nursing homes and other institutions. Joint ventures with industry, utility projects, laboratory design assistance and other activities are building a solid industry of US solar thermal systems ready for use today.

  10. High Temperature Thermosets

    NASA Technical Reports Server (NTRS)

    Hergenrother, Paul M.

    1999-01-01

    A thermoset or network polymer is an organic material where the molecules are tied together through chemical bonds (crosslinks) and therefore they cannot move past one another. As a result, these materials exhibit a certain degree of dimensional stability. The chemical composition and the degree of crosslink density of the thermoset have a pronounced effect upon the properties. High temperature thermosets offer a favorable combination of properties that makes them attractive for many applications. Their most important features are the excellent processability particularly of the low molecular weight precusor forms, the chemical and solvent resistance and the dimensional stability. The market for high temperature thermosets will increase as new uses for them are uncovered and new thermosets with better combinations of properties are developed.

  11. High-k gadolinium scandate on Si obtained by high pressure sputtering from metal targets and in-situ plasma oxidation

    NASA Astrophysics Data System (ADS)

    Pampillón, M. A.; San Andrés, E.; Feijoo, P. C.; Fierro, J. L. G.

    2017-03-01

    This article studies the physical and electrical behavior of Gd2‑x Sc x O3 layers grown by high pressure sputtering from metallic Gd and Sc targets. The aim is to obtain a high permittivity dielectric for microelectronic applications. The films were obtained by the deposition of a metallic nanolaminate of Gd and Sc alternating layers, which is afterwards in-situ oxidized by plasma. The oxide films obtained were close to stoichiometry, amorphous and with minimal interfacial regrowth. By fabricating metal–insulator–semiconductor capacitors we found that a moderate temperature annealing is needed to enhance permittivity, which reaches a high value of 32 while keeping moderate leakage. Finally, the feasibility of interface scavenging in this material with Ti gate electrodes is also demonstrated.

  12. In situ monitoring of internal surface temperature of the historic building envelope

    NASA Astrophysics Data System (ADS)

    Labovská, Veronika; Katunský, Dušan

    2016-12-01

    This article deals with progressive glass unit in glazing systems of building facades. Main aim of this research is reduction of heat gain in interior achieved by water added into Basic Insulation Glass Unit (hereinafter as IGU) which thereby becomes a transparent collector. Concerning heat gain reduction, this system provides a variety of positive characteristics. In relation to outdoor conditions, however, the system has its limitations, due to which each glass unit needs to be designed with regard to the climate condition it is intended for. These special properties have been described in previous articles. Currently, the model in scale 1:1 is prepared and provided for measurements in test chamber. Observation of liquid-filled window in summer weather simulation has brought valuable results for temperature, radiation and humidity. Temperature has been observed on surfaces, and exterior and interior sides of cavities.

  13. In-situ coal seam and overburden permeability characterization combining downhole flow meter and temperature logs.

    NASA Astrophysics Data System (ADS)

    Busse, Julia; Scheuermann, Alexander; Bringemeier, Detlef; Hossack, Alex; Li, Ling

    2016-06-01

    The planning and design of any coal mine development requires among others a thorough investigation of the geological, geotechnical and hydrogeological subsurface conditions. As part of a coal mine exploration program we conducted heat pulse vertical flow meter testing. The flow data were combined with absolute and differential temperature logging data to gain information about the hydraulic characteristics of two different coal seams and their over- and interburden. For the strata that were localised based on geophysical logging data including density, gamma ray and resistivity hydraulic properties were quantified. We demonstrate that the temperature log response complements the flow meter log response. A coupling of both methods is therefore recommended to get an insight into the hydraulic conditions in a coal seam and its overburden.

  14. Transformation of Mo and W thiosalts into unsupported sulfide catalysts: A temperature dependent in-situ spectroscopic investigation

    SciTech Connect

    Yi, Yanjiao; Williams, Christopher T.; Glascock, Mary; Xiong, Guang; Lauterbach, Jochen; Liang, Changhai

    2014-08-15

    Highlights: • TPD–MS results suggest that the majority of S remains in the solid sample after decomposition. • Decomposition of the (CH{sub 3}){sub 4}N is not directly correlated with that of the MS{sub 4}{sup 2−} species. • Surface of materials does not track directly with the bulk at various treatment temperatures. • ATT-derived materials retained a significant amount of +6 state consistent with the precursor. - Abstract: The thermal decomposition of ammonium thiomolybdate (ATM), ammonium thiotungstate (ATT), tetramethylammonium thiomolybdate (TMATM) and tetramethylammonium thiotungstate (TMATT) are investigated as a function of temperature by using thermogravimetric analysis (TGA), temperature-programmed decomposition with mass spectroscopy (TPS–MS), in-situ Fourier transform infrared (FTIR) and Raman spectroscopies, and X-ray photoelectron spectroscopy (XPS). The results allow for correlations to be made between the changes in the bulk and surface structures of the materials, and the evolution of gas-phase decomposition products. The major difference between the ammonium and tetramethylammonium precursors is the complexity of the thermal decomposition profile, which is found to follow two steps over a wide temperature range for the former, but one step over a relatively narrow range for the latter materials. Raman and FTIR spectra reveal the decomposition of the ammonium and tetramethylammonium groups, along with the decomposition of the initial sulfide structures to metal disulfides. For both sets of precursors, XPS results show that the surface of the resulting materials at various temperatures of treatment does not track directly with the state of the bulk material. While the ATM, TMATM, and TMATT-derived material surfaces are reduced to the 4{sup +} state at the highest temperature, indicating disulfides, the ATT-derived materials still retained a significant amount of W{sup 6+} state consistent with the starting precursor.

  15. Laboratory evaluation of the Level TROLL 100 manufactured by In-Situ Inc.: results of pressure and temperature tests

    USGS Publications Warehouse

    Carnley, Mark V.; Fulford, Janice M.; Brooks, Myron H.

    2013-01-01

    The Level TROLL 100 manufactured by In-Situ Inc. was evaluated by the U.S. Geological Survey (USGS) Hydrologic Instrumentation Facility (HIF) for conformance to the manufacturer’s accuracy specifications for measuring pressure throughout the device’s operating temperature range. The Level TROLL 100 is a submersible, sealed, water-level sensing device with an operating pressure range equivalent to 0 to 30 feet of water over a temperature range of −20 to 50 degrees Celsius (°C). The device met the manufacturer’s stated accuracy specifications for pressure within its temperature-compensated operating range of 0 to 50 °C. The device’s accuracy specifications did not meet established USGS requirements for primary water-stage sensors used in the operation of streamgages, but the Level TROLL 100 may be suitable for other hydrologic data-collection applications. As a note, the Level TROLL 100 is not designed to meet USGS accuracy requirements. Manufacturer accuracy specifications were evaluated, and the procedures followed and the results obtained are described in this report. USGS accuracy requirements are routinely examined and reported when instruments are evaluated at the HIF.

  16. In situ gelling pH- and temperature-sensitive biodegradable block copolymer hydrogels for drug delivery.

    PubMed

    Singh, Narendra K; Lee, Doo Sung

    2014-11-10

    Stimuli-sensitive injectable polymeric hydrogels have been extensively investigated during the past decade as bioactive agent delivery vehicles and for tissue engineering applications. An aqueous solution of these polymers undergoes a sol-to-gel phase transition in response to external stimuli such as pH, temperature, salt, light, biomolecules, electromagnetic field, etc. Bioactive molecules or cells can be mixed into the low-viscosity state of the polymer solution and injected into the body at a target site, forming an in situ hydrogel depot, which can then serve as bioactive-molecule-releasing carriers or a cell-growing microenvironment. This review systematically summarizes the recent progress in biodegradable and injectable block copolymer hydrogels, giving special attention to the novel and promising pH- and temperature-sensitive injectable block copolymer hydrogels for biomedical applications. The gelation mechanism, formation of ionic complexes, and biodegradation are highlighted as key factors responsible for controlled protein/drug delivery. The advantages and perspectives of pH- and temperature-sensitive injectable block copolymer hydrogels are also highlighted.

  17. Toward Biocompatible Nuclear Hyperpolarization Using Signal Amplification by Reversible Exchange: Quantitative in Situ Spectroscopy and High-Field Imaging

    PubMed Central

    2014-01-01

    Signal amplification by reversible exchange (SABRE) of a substrate and parahydrogen at a catalytic center promises to overcome the inherent insensitivity of magnetic resonance. In order to apply the new approach to biomedical applications, there is a need to develop experimental equipment, in situ quantification methods, and a biocompatible solvent. We present results detailing a low-field SABRE polarizer which provides well-controlled experimental conditions, defined spins manipulations, and which allows in situ detection of thermally polarized and hyperpolarized samples. We introduce a method for absolute quantification of hyperpolarization yield in situ by means of a thermally polarized reference. A maximum signal-to-noise ratio of ∼103 for 148 μmol of substance, a signal enhancement of 106 with respect to polarization transfer field of SABRE, or an absolute 1H-polarization level of ≈10–2 is achieved. In an important step toward biomedical application, we demonstrate 1H in situ NMR as well as 1H and 13C high-field MRI using hyperpolarized pyridine (d3) and 13C nicotinamide in pure and 11% ethanol in aqueous solution. Further increase of hyperpolarization yield, implications of in situ detection, and in vivo application are discussed. PMID:24397559

  18. Highly Enhanced Fluorescence of CdSeTe Quantum Dots Coated with Polyanilines via In-Situ Polymerization and Cell Imaging Application.

    PubMed

    Xue, Jingjing; Chen, Xinyi; Liu, Shanglin; Zheng, Fenfen; He, Li; Li, Lingling; Zhu, Jun-Jie

    2015-09-02

    The polyaniline (PAN)-coated CdSeTe quantum dots (QDs) were prepared by in situ polymerization of aniline on the surface of CdSeTe QDs. The PAN-coated CdSeTe QDs has a tremendously enhanced fluorescence (∼40 times) and improved biocompatibility compared to the uncoated CdSeTe QDs. The fluorescence intensity of the PAN-coated CdSeTe QDs can be adjusted by controlling the construction parameters of the PAN shell. The kinetics of the in situ controllable polymerization process was studied by varying the temperature, and the apparent activation energy of polymerization was estimated. With the same method, a series of the PAN derivatives were also tested to coat the CdSeTe QDs in this study. All the QDs showed a significant enhancement of the fluorescence intensity and better biocompatibility. The significantly enhanced fluorescence can provide highly amplified signal for luminescence-based cell imaging.

  19. Highly indistinguishable photons from deterministic quantum-dot microlenses utilizing three-dimensional in situ electron-beam lithography

    PubMed Central

    Gschrey, M.; Thoma, A.; Schnauber, P.; Seifried, M.; Schmidt, R.; Wohlfeil, B.; Krüger, L.; Schulze, J. -H.; Heindel, T.; Burger, S.; Schmidt, F.; Strittmatter, A.; Rodt, S.; Reitzenstein, S.

    2015-01-01

    The success of advanced quantum communication relies crucially on non-classical light sources emitting single indistinguishable photons at high flux rates and purity. We report on deterministically fabricated microlenses with single quantum dots inside which fulfil these requirements in a flexible and robust quantum device approach. In our concept we combine cathodoluminescence spectroscopy with advanced in situ three-dimensional electron-beam lithography at cryogenic temperatures to pattern monolithic microlenses precisely aligned to pre-selected single quantum dots above a distributed Bragg reflector. We demonstrate that the resulting deterministic quantum-dot microlenses enhance the photon-extraction efficiency to (23±3)%. Furthermore we prove that such microlenses assure close to pure emission of triggered single photons with a high degree of photon indistinguishability up to (80±7)% at saturation. As a unique feature, both single-photon purity and photon indistinguishability are preserved at high excitation power and pulsed excitation, even above saturation of the quantum emitter. PMID:26179766

  20. High Performance Molecular Visualization: In-Situ and Parallel Rendering with EGL.

    PubMed

    Stone, John E; Messmer, Peter; Sisneros, Robert; Schulten, Klaus

    2016-05-01

    Large scale molecular dynamics simulations produce terabytes of data that is impractical to transfer to remote facilities. It is therefore necessary to perform visualization tasks in-situ as the data are generated, or by running interactive remote visualization sessions and batch analyses co-located with direct access to high performance storage systems. A significant challenge for deploying visualization software within clouds, clusters, and supercomputers involves the operating system software required to initialize and manage graphics acceleration hardware. Recently, it has become possible for applications to use the Embedded-system Graphics Library (EGL) to eliminate the requirement for windowing system software on compute nodes, thereby eliminating a significant obstacle to broader use of high performance visualization applications. We outline the potential benefits of this approach in the context of visualization applications used in the cloud, on commodity clusters, and supercomputers. We discuss the implementation of EGL support in VMD, a widely used molecular visualization application, and we outline benefits of the approach for molecular visualization tasks on petascale computers, clouds, and remote visualization servers. We then provide a brief evaluation of the use of EGL in VMD, with tests using developmental graphics drivers on conventional workstations and on Amazon EC2 G2 GPU-accelerated cloud instance types. We expect that the techniques described here will be of broad benefit to many other visualization applications.

  1. High-speed Optical Coherence Tomography for Management after Laser in Situ Keratomileusis

    PubMed Central

    Avila, Mariana; Li, Yan; Song, Jonathan C.; Huang, David

    2007-01-01

    PURPOSE: To report applications of optical coherence tomography (OCT) in the management of laser in situ keratomileusis (LASIK) related problems. SETTING: Doheny Eye Institute and Department of Ophthalmology, Keck School of Medicine of the University of Southern California, Los Angeles, California, USA. METHODS: Five patients referred for LASIK-related problems were enrolled in a prospective observational study. Clinical examination, ultrasound (US) pachymetry, Placido ring slit-scanning corneal topography (Orbscan II, Bausch & Lomb), and high-speed corneal OCT were performed. RESULTS: In cases of regression and keratectasia, OCT provided thickness measurements of the cornea, flap, and posterior stromal bed. Locations of tissue loss and flap interface planes were identified in a case with a recut enhancement complication. The information was used to determine whether further laser ablation was safe, confirm keratectasia, and manage complications. Optical coherence tomography measurements of central corneal thickness agreed well with US pachymetry measurements (difference 6.4 mm G 11.7 [SD]) (P Z .026), while Orbscan significantly underestimated corneal thickness (-67.5 ± 72.5 μm) (P = .17). CONCLUSIONS: High-speed OCT provided noncontact imaging and measurement of LASIK anatomy. It was useful in monitoring LASIK results and evaluating complications. PMID:17081866

  2. In situ inspection of inclusions in toughened glass panels of high-rise buildings

    NASA Astrophysics Data System (ADS)

    Li, Xiang; Fang, Zhong Ping; Reading, Ivan; Zhao, Liping; Chow, Siew Loong

    2005-04-01

    Transparent toughened glass panels are widely installed in high-rise buildings. There is a growing need for inspection to detect the presence of detrimental inclusions of Nickel Sulfide. These inclusions can cause toughened glass to shatter, possibly causing property damage or injury. Optical equipment has been developed which can detect the inclusions in-situ. Light is coupled into a glass panel and propagates along the glass by total internal reflection. An inclusion in the glass will cause the light to scatter. Once an inclusion is found, it will be observed at higher magnification and the detailed image will be processed. By the analysis of its key features, the inclusion type can be identified. The coupling medium is made of a transparent, soft and deformable material. The equipment can be attached to a glass panel by vacuum suction. The optical system can scan the whole glass panel with a constant force spring as anti-weight structure. The whole system is fast, convenient and highly effective. A patent has been filed for this apparatus.

  3. High lactose tolerance in North Europeans: a result of migration, not in situ milk consumption.

    PubMed

    Vuorisalo, Timo; Arjamaa, Olli; Vasemägi, Anti; Taavitsainen, Jussi-Pekka; Tourunen, Auli; Saloniemi, Irma

    2012-01-01

    The main carbohydrate in milk is lactose, which must be hydrolyzed to glucose and galactose before the sugars can be digested. While 65% or more of the total human population are lactose intolerant, in some human populations lactase activity commonly persists into adulthood. Lactose tolerance is exceptionally widespread in Northern European countries such as Sweden and Finland, with tolerance levels of 74% and 82%, respectively. Theoretically, this may result either from a strong local selection pressure for lactose tolerance, or from immigration of lactose tolerant people to Northern Europe. We provide several lines of archaeological and historical evidence suggesting that the high lactose tolerance in North Europeans cannot be explained by selection from in situ milk consumption. First, fresh cow milk has not belonged to the traditional diet of Swedes or Finns until recent times. Second, not enough milk has been available for adult consumption. Cattle herding has been neither widespread nor productive enough in Northern Europe to have provided constant access to fresh milk. We suggest that the high prevalence of lactose tolerance in Finland in particular may be explained by immigration of people representing so-called Corded Ware Culture, an early culture representing agricultural development in Europe.

  4. High Performance Molecular Visualization: In-Situ and Parallel Rendering with EGL

    PubMed Central

    Stone, John E.; Messmer, Peter; Sisneros, Robert; Schulten, Klaus

    2016-01-01

    Large scale molecular dynamics simulations produce terabytes of data that is impractical to transfer to remote facilities. It is therefore necessary to perform visualization tasks in-situ as the data are generated, or by running interactive remote visualization sessions and batch analyses co-located with direct access to high performance storage systems. A significant challenge for deploying visualization software within clouds, clusters, and supercomputers involves the operating system software required to initialize and manage graphics acceleration hardware. Recently, it has become possible for applications to use the Embedded-system Graphics Library (EGL) to eliminate the requirement for windowing system software on compute nodes, thereby eliminating a significant obstacle to broader use of high performance visualization applications. We outline the potential benefits of this approach in the context of visualization applications used in the cloud, on commodity clusters, and supercomputers. We discuss the implementation of EGL support in VMD, a widely used molecular visualization application, and we outline benefits of the approach for molecular visualization tasks on petascale computers, clouds, and remote visualization servers. We then provide a brief evaluation of the use of EGL in VMD, with tests using developmental graphics drivers on conventional workstations and on Amazon EC2 G2 GPU-accelerated cloud instance types. We expect that the techniques described here will be of broad benefit to many other visualization applications. PMID:27747137

  5. In situ study of photo- and thermo-induced color centers in photochromic rutile TiO2 in the temperature range 90-720 K.

    PubMed

    Kuznetsov, V N; Glazkova, N I; Mikhaylov, R V; Serpone, N

    2016-10-05

    This article reports an in situ UV-Vis-NIR diffuse reflectance (DR) spectroscopic and kinetic study of the photoformation and thermal annealing of light absorbing electronic point defects (color centers) in photochromic TiO2 in the temperature range 90-720 K using a simple laboratory-made cryostat-type accessory (for a Cary 5000 spectrophotometer equipped with an integrating sphere). The accessory also allowed for UV-Vis-NIR DR studies to be undertaken either in vacuum or in an oxygen atmosphere at significantly high temperatures (to 720 K) to assess dark chemical events occurring in photochromic titania with the participation of color centers. The DR spectral and kinetic measurements provided the opportunity to examine the separation of photoinduced charge carriers at traps and thermally stimulated carrier detrapping and recombination, as well as the response of color centers to oxidative/reductive treatments of photochromic TiO2. Kinetic results also demonstrate the applicability of the fabricated DR accessory as a high-temperature reaction cell in the systematic study of the principal regularities in the formation and destruction of color centers in titania at various temperatures and gaseous atmospheres.

  6. Apparatus for high-pressure and low-temperature experiments

    NASA Technical Reports Server (NTRS)

    Golopentia, D. A.; Ruoff, A. L.

    1981-01-01

    A new type of apparatus for high-pressure experiments at low temperature (1.5 K) is presented. It uses a flat diamond anvil with a spherical indentor. It utilizes a load ring placed under the sample, so that the load (and hence pressure) can be measured in situ at low temperature. The apparatus was successfully used to investigate the high-conductivity state of sulphur. It can be used to investigate other thin film samples.

  7. High-order harmonic generation in a plasma plume of in situ laser-produced silver nanoparticles

    SciTech Connect

    Singhal, H.; Naik, P. A.; Chakera, J. A.; Chakravarty, U.; Vora, H. S.; Srivastava, A. K.; Mukherjee, C.; Navathe, C. P.; Deb, S. K.; Gupta, P. D.; Ganeev, R. A.

    2010-10-15

    The results of the experimental study of high-order harmonic generation (HHG) from the interaction of 45-fs Ti:sapphire laser pulses with plasma plumes of Ag nanoparticles produced in situ are presented in this article. The nanoparticles were generated by the interaction of 300-ps, 20-mJ laser pulses with bulk silver targets at an intensity of {approx}1x10{sup 13} W/cm{sup 2}. The spectral characteristics of the HHG from nanoparticles produced in situ are compared with the HHG from monoparticle plasma plumes and with the HHG from preformed nanoparticle-containing plasma plumes. The cutoff harmonic order generated using the in situ silver nanoparticles is at the 21st harmonic order.

  8. High Temperature Piezoelectric Drill

    NASA Technical Reports Server (NTRS)

    Bao, Xiaoqi; Bar-Cohen, Yoseph; Sherrit, Stewart; Badescu, Mircea; Shrout, Tom

    2012-01-01

    Venus is one of the planets in the solar systems that are considered for potential future exploration missions. It has extreme environment where the average temperature is 460 deg C and its ambient pressure is about 90 atm. Since the existing actuation technology cannot maintain functionality under the harsh conditions of Venus, it is a challenge to perform sampling and other tasks that require the use of moving parts. Specifically, the currently available electromagnetic actuators are limited in their ability to produce sufficiently high stroke, torque, or force. In contrast, advances in developing electro-mechanical materials (such as piezoelectric and electrostrictive) have enabled potential actuation capabilities that can be used to support such missions. Taking advantage of these materials, we developed a piezoelectric actuated drill that operates at the temperature range up to 500 deg C and the mechanism is based on the Ultrasonic/Sonic Drill/Corer (USDC) configuration. The detailed results of our study are presented in this paper

  9. High temperature strain gages

    NASA Technical Reports Server (NTRS)

    Gregory, Otto J. (Inventor); You, Tao (Inventor)

    2011-01-01

    A ceramic strain gage based on reactively sputtered indium-tin-oxide (ITO) thin films is used to monitor the structural integrity of components employed in aerospace propulsion systems operating at temperatures in excess of 1500.degree. C. A scanning electron microscopy (SEM) of the thick ITO sensors reveals a partially sintered microstructure comprising a contiguous network of submicron ITO particles with well defined necks and isolated nanoporosity. Densification of the ITO particles was retarded during high temperature exposure with nitrogen thus stabilizing the nanoporosity. ITO strain sensors were prepared by reactive sputtering in various nitrogen/oxygen/argon partial pressures to incorporate more nitrogen into the films. Under these conditions, sintering and densification of the ITO particles containing these nitrogen rich grain boundaries was retarded and a contiguous network of nano-sized ITO particles was established.

  10. High temperature acoustic levitator

    NASA Technical Reports Server (NTRS)

    Barmatz, M. B. (Inventor)

    1984-01-01

    A system is described for acoustically levitating an object within a portion of a chamber that is heated to a high temperature, while a driver at the opposite end of the chamber is maintained at a relatively low temperature. The cold end of the chamber is constructed so it can be telescoped to vary the length (L sub 1) of the cold end portion and therefore of the entire chamber, so that the chamber remains resonant to a normal mode frequency, and so that the pressure at the hot end of the chamber is maximized. The precise length of the chamber at any given time, is maintained at an optimum resonant length by a feedback loop. The feedback loop includes an acoustic pressure sensor at the hot end of the chamber, which delivers its output to a control circuit which controls a motor that varies the length (L) of the chamber to a level where the sensed acoustic pressure is a maximum.

  11. In situ high pressure infrared study of the carbon environment in (Mg,Fe)CO3 carbonate

    NASA Astrophysics Data System (ADS)

    Boulard, E.; Pan, D.; Galli, G.; Mao, W. L.

    2013-12-01

    Carbonates are likely to be the main carbon-bearing phase in the Earth's mantle, and therefore knowledge of their mineral physics down to core mantle boundary conditions is critical for understanding the deep carbon cycle. (Mg,Fe)CO3 has been the focus of many recent high pressure studies which indicate several crystallographic changes. An electronic spin transition in the iron end-member has been reported at approximately 45 GPa. As a result, a change in the volume and the equation of state, and moreover a change in the rate of C-O bond distortion were described by X-ray diffraction (XRD) studies (B. Lavina et al., 2009; 2010). At higher pressures, above 80 GPa, we have observed the transformation of (Mg,Fe)CO3 carbonate into a new high-pressure high-temperature phase by in situ XRD (Boulard et al., 2011). Investigation of the carbon environment had previously been limited to ex situ studies at ambient conditions after releasing the pressure on the sample. Spectroscopy on the carbon C-k edge indicated a potential change in the carbon environment, and a transformation of the carbonate trigonal CO3 groups into CO4 tetrahedra had been proposed (Boulard et al., 2011). However this interpretation is still under debate. To follow the evolution of C-O bonds and clarify the existence of CO4 tetrahedra in high-pressure carbonate phases, we combined in-situ infrared spectroscopy with theoretical calculations. Mid-infrared spectroscopy, performed at high pressure before and after laser heating at U2A, NSLS, BNL show several changes in the (Mg,Fe)CO3 spectrum after laser heating at 103 GPa. We will discuss the interpretation of these new spectroscopic signatures and the possibility of a dramatic change in the carbon environment. References: Boulard, E. et al., (2011). New host for carbon in the deep Earth. PNAS, 108(13), 5184-5187. Lavina, B. et al., (2009). Siderite at lower mantle conditions and the effects of the pressure-induced spin-pairing transition. Geophysical

  12. High throughput and multiplex localization of proteins and cells for in situ micropatterning using pneumatic microfluidics.

    PubMed

    Wang, Jian-Chun; Liu, Wenming; Tu, Qin; Ma, Chao; Zhao, Lei; Wang, Yaolei; Ouyang, Jia; Pang, Long; Wang, Jinyi

    2015-02-07

    Micropatterning technologies are emerging as an enabling tool for various microfluidic-based applications in life sciences. However, the high throughput and multiplex localization of multiple bio-components in a microfluidic device has not yet been well established. In this paper, we describe a simple and in situ micropatterning method using an integrated microfluidic device with pneumatic microstructures (PμSs) for highly controllable immobilization of both proteins and cells in a high throughput, geometry-dynamic, and multi-patterning way. The precise Pluronic F127 passivation of a microchamber surface except the PμS-blocked regions was performed and characterized, and the spatial dynamics and consistency of both the PμSs and protein/cell micropatterning were optically evaluated and quantitatively demonstrated too. Furthermore, a systematic investigation of PμS-assisted micropatterning in microfluidics was carried out. The feature of high throughput and spatial control of micropatterning can be simply realized by using the well-designed PμS arrays. Meanwhile, the co-micropatterning of different proteins (bovine serum albumin and chicken egg albumin) and cells (human umbilical vein endothelial cells and human hepatocellular carcinoma cells) in a microfluidic device was successfully accomplished with the orderly serial manipulation of PμS groups. We demonstrate that PμS-assisted micropatterning can be applied as a convenient microfluidic component for large-scale and diversified protein/cell patterning and manipulation, which could be useful for cell-based tissue organization, high-throughput imaging, protein-related interactions and immunoassays.

  13. High yield of pure multiwalled carbon nanotubes from the catalytic decomposition of acetylene on in-situ formed cobalt nanoparticles.

    PubMed

    Delpeux, Sandrine; Szostak, Katarzyna; Frackowiak, Elzbieta; Bonnamy, Sylvie; Béguin, François

    2002-10-01

    For the first time, multiwalled carbon nanotubes (MWNTs) could be formed selectively in a high yield, free of any disordered carbon by-product, from the catalytic decomposition of acetylene at 600 degrees C on a CoxMg(1-x)O solid solution. Starting from 1 g of catalytic substrate, 4 g of pure MWNTs were obtained after its dissolution in boiling concentrated HCl, without any additional purification in strongly oxidizing medium, as is required for other methods of nanotube production. In situ reduction of CoO by dihydrogen liberated from acetylene decomposition allows highly divided metal particles to be continuously produced as synthesis proceeds. This is undoubtedly the reason for the good performance of the catalyst and for the ability to produce nanotubes in a narrow diameter range, namely from 10 to 15 nm. With the use of acetylene instead of methane, the synthesis proceeds at low temperature, which prevents the growth of carbon shells, in which the metal particles are generally embedded, decreasing their activity. Because of the very low specific surface area of the catalyst support, the amount of disordered carbon by-product formed is negligible.

  14. Application of in situ diffraction in high-throughput structure determination platforms.

    PubMed

    Aller, Pierre; Sanchez-Weatherby, Juan; Foadi, James; Winter, Graeme; Lobley, Carina M C; Axford, Danny; Ashton, Alun W; Bellini, Domenico; Brandao-Neto, Jose; Culurgioni, Simone; Douangamath, Alice; Duman, Ramona; Evans, Gwyndaf; Fisher, Stuart; Flaig, Ralf; Hall, David R; Lukacik, Petra; Mazzorana, Marco; McAuley, Katherine E; Mykhaylyk, Vitaliy; Owen, Robin L; Paterson, Neil G; Romano, Pierpaolo; Sandy, James; Sorensen, Thomas; von Delft, Frank; Wagner, Armin; Warren, Anna; Williams, Mark; Stuart, David I; Walsh, Martin A

    2015-01-01

    Macromolecular crystallography (MX) is the most powerful technique available to structural biologists to visualize in atomic detail the macromolecular machinery of the cell. Since the emergence of structural genomics initiatives, significant advances have been made in all key steps of the structure determination process. In particular, third-generation synchrotron sources and the application of highly automated approaches to data acquisition and analysis at these facilities have been the major factors in the rate of increase of macromolecular structures determined annually. A plethora of tools are now available to users of synchrotron beamlines to enable rapid and efficient evaluation of samples, collection of the best data, and in favorable cases structure solution in near real time. Here, we provide a short overview of the emerging use of collecting X-ray diffraction data directly from the crystallization experiment. These in situ experiments are now routinely available to users at a number of synchrotron MX beamlines. A practical guide to the use of the method on the MX suite of beamlines at Diamond Light Source is given.

  15. In situ measurement of low-Z material coating thickness on high Z substrate for tokamaks

    SciTech Connect

    Mueller, D. Roquemore, A. L.; Jaworski, M.; Skinner, C. H.; Miller, J.; Creely, A.; Raman, P.; Ruzic, D.

    2014-11-15

    Rutherford backscattering of energetic particles can be used to determine the thickness of a coating of a low-Z material over a heavier substrate. Simulations indicate that 5 MeV alpha particles from an {sup 241}Am source can be used to measure the thickness of a Li coating on Mo tiles between 0.5 and 15 μm thick. Using a 0.1 mCi source, a thickness measurement can be accomplished in 2 h of counting. This technique could be used to measure any thin, low-Z material coating (up to 1 mg/cm{sup 2} thick) on a high-Z substrate, such as Be on W, B on Mo, or Li on Mo. By inserting a source and detector on a moveable probe, this technique could be used to provide an in situ measurement of the thickness of Li coating on NSTX-U Mo tiles. A test stand with an alpha source and an annular solid-state detector was used to investigate the measurable range of low-Z material thicknesses on Mo tiles.

  16. Highly Sensitive Tunable Diode Laser Spectrometers for In Situ Planetary Exploration

    NASA Technical Reports Server (NTRS)

    Vasudev, Ram; Mansour, Kamjou; Webster, Christopher R.

    2013-01-01

    This paper describes highly sensitive tunable diode laser spectrometers suitable for in situ planetary exploration. The technology developed at JPL is based on wavelength modulated cavity enhanced absorption spectroscopy. It is capable of sensitively detecting chemical signatures of life through the abundance of biogenic molecules and their isotopic composition, and chemicals such as water necessary for habitats of life. The technology would be suitable for searching for biomarkers, extinct life, potential habitats of extant life, and signatures of ancient climates on Mars; and for detecting biomarkers, prebiotic chemicals and habitats of life in the outer Solar System. It would be useful for prospecting for water on the Moon and asteroids, and characterizing its isotopic composition. Deployment on the Moon could provide ground truth to the recent remote measurements and help to uncover precious records of the early bombardment history of the inner Solar System buried at the shadowed poles, and elucidate the mechanism for the generation of near-surface water in the illuminated regions. The technology would also be useful for detecting other volatile molecules in planetary atmospheres and subsurface reservoirs, isotopic characterization of planetary materials, and searching for signatures of extinct life preserved in solid matrices.

  17. In-Situ High-Resolution Transmission Electron Microscopy Investigation of Overheating of Cu Nanoparticles

    NASA Astrophysics Data System (ADS)

    Chen, Chunlin; Hu, Ziyu; Li, Yanfen; Liu, Limin; Mori, Hirotaro; Wang, Zhangchang

    2016-01-01

    Synthesizing and functionalizing metal nanoparticles supported on substrates is currently the subject of intensive study owing to their outstanding catalytic performances for heterogeneous catalysis. Revealing the fundamental effect of the substrates on metal nanoparticles represents a key step in clarifying mechanisms of stability and catalytic properties of these heterogeneous systems. However, direct identification of these effects still poses a significant challenge due to the complicacy of interactions between substrates and nanoparticles and also for the technical difficulty, restraining our understanding of these heterogeneous systems. Here, we combine in situ high-resolution transmission electron microscopy with molecular dynamics simulations to investigate Cu nanoparticles supported on graphite and Cu2O substrates, and demonstrate that melting behavior and thermal stability of Cu nanoparticles can be markedly influenced by substrates. The graphite-supported Cu nanoparticles do not melt during annealing at 1073 K until they vanish completely, i.e. only the sublimation occurs, while the Cu2O-supported Cu nanoparticles suffer melting during annealing at 973 K. Such selective superheating of the Cu nanoparticles can be attributed to the adsorption of a thin carbon layer on the surface of the Cu nanoparticles, which helps guide further stability enhancement of functional nanoparticles for realistic applications.

  18. Ni3Si2 nanowires grown in situ on Ni foam for high-performance supercapacitors

    NASA Astrophysics Data System (ADS)

    Jiang, Yizhe; Li, Zhihui; Li, Beibei; Zhang, Jinying; Niu, Chunming

    2016-07-01

    Ni3Si2 nanowires and nanoawls have grown in situ on the surface of Ni foams by a controlled low pressure chemical vapor deposition process. Structural characterization shows that the individual Ni3Si2 nanowire is single crystal covered with a thin layer (1-2 nm) of SiO2 with a diameter of ∼20-30 nm and length of ten's micrometers. Individual nanoawl with a circular cone shape is polycrystalline. Both Ni3Si2 nanowire and nanoawl samples are evaluated as potential electrode materials for supercapacitors. The nanowire electrode delivers a very high specific capacitance and excellent rate capability. A specific capacitance of 760 F g-1 is measured at current density of 0.5 A g-1, which decreases to 518 F g-1 when the current density increases to 10 A g-1. The capacitance is dominated by pseudocapacitance with a mechanism similar to that of NiO or Ni(OH)2 widely studied in the literature. An asymmetric supercapacitor fabricated by pairing Ni3Si2 nanowire electrode with an activated carbon electrode exhibits energy densities of 17.5 Wh kg-1 and 8.8 Wh kg-1 at power densites of 301 W kg-1 and 3000 W kg-1.

  19. High temperature detonator

    DOEpatents

    Johnson, James O.; Dinegar, Robert H.

    1988-01-01

    A detonator assembly is provided which is usable at high temperatures about 300.degree. C. A detonator body is provided with an internal volume defining an anvil surface. A first acceptor explosive is disposed on the anvil surface. A donor assembly having an ignition element, an explosive material, and a flying plate, are placed in the body effective to accelerate the flying plate to impact the first acceptor explosive on the anvil for detonating the first acceptor explosive. A second acceptor explosive is eccentrically located in detonation relationship with the first acceptor explosive to thereafter effect detonation of a main charge.

  20. High Temperature Superconducting Compounds

    DTIC Science & Technology

    1990-10-01

    usual substrates, SrTiO3 , YSZ, MgO, and LaA103, it has been possible to deposit films on Si substrates without any buffer layer. A bolometer has been...new opportunities for the study of superconductor-insulator transitions and the investigation of photo- doping with carriers of high temperature super... SrTiO3 (00), SrTiO3 (l 10), LaA103 (100), MgO(100), and yttria stabilized zirconia (YSZ). The surfaces of these films could be imaged with a scanning