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Sample records for in-situ high temperature

  1. 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

  2. In Situ Observation of High Temperature Creep Behavior During Annealing of Steel

    NASA Astrophysics Data System (ADS)

    Zhang, X. F.; Terasaki, H.; Komizo, Y.; Murakami, Y.; Yasuda, K.

    2012-12-01

    Previous studies on creep suggested a close relationship between polycrystal grain size, substructure, and creep rate. At present, however, our understanding of the influence of polycrystal grain size, substructure, and thermal stress on creep deformation behavior seems rather insufficient, especially as there is a general lack of in situ data on structural changes during creep. In this study, the effects of thermal stress, austenite grain size, and cooling rate on slip deformations in C-Mn-Al steel during annealing were investigated systematically on the basis of in situ observations using high temperature laser scanning confocal microscopy. Finally, a kinetics model based on thermal expansion anisotropy and temperature difference was developed to explain these interesting experimental results. The in situ investigation of slip deformation during annealing greatly contributes to the understanding of high temperature creep behavior.

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

    DOE PAGESBeta

    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,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

  4. 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.

  5. 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.

  6. 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.

  7. In situ proton irradiation-induced creep at very high temperature

    NASA Astrophysics Data System (ADS)

    Campbell, Anne A.; Was, Gary S.

    2013-02-01

    This objective of this work was to develop an experimental facility that can perform in situ high temperature proton irradiation-induced creep experiments on a range of materials. This was achieved by designing an irradiation chamber and stage that allows for load application and removal, provides a method for controlling and monitoring temperature and proton flux, and a means to make in situ measurement of dimensional change of the samples during the experiment. Initial experiments on POCO Graphite Inc. ZXF-5Q grade ultra-fine grain samples irradiated at 1000 °C at a damage rate of 1.15 × 10-6 dpa/s exhibited a linear dependence of measured creep rate on applied stress over a range of stresses from 10 MPa to 40 MPa.

  8. High-voltage electron microscope high-temperature in situ straining experiments to study dislocation dynamics in intermetallics and quasicrystals.

    PubMed

    Messerschmidt, U

    2001-07-01

    The dynamic behaviour of dislocations in several intermetallic alloys, studied by in situ straining experiments in a high-voltage electron microscope, is compared at room temperature and at high temperatures. In contrast to room temperature, the dislocations move viscously at high temperatures, which is explained by diffusion processes in the dislocation cores. In quasicrystals, the viscous dislocation motion can be interpreted by models on the cluster scale. PMID:11454156

  9. 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.

  10. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-06-01

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

  12. 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. PMID:26578758

  13. 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

  14. Continuous high temperature gradient solidification of in situ Cu-Nb alloys for large scale development

    SciTech Connect

    LeHuy, H.; Fihey, J.L.; Foner, S.; Roberge, R.

    1982-01-01

    Several research groups are evaluating various scale-up approaches for the in situ technique of preparing multiply-connected Nb/sub 3/Sn composite superconducting wire. Previously, the authors developed an arrangement for continuous high temperature gradient solidification, and now have upgraded the process to permit the solidification of larger diameter (9.5 mm) rods in virtually unlimited lengths. The preparation, the microstructure, and the characteristics (solidification rate, dendrite branching, and dendrite size) are given for three directionally solidified in situ materials with a nominal composition of Cu-30 wt% Nb. Micrographs of variously extracted Nb filaments and various-order dendrites are provided. The HTGS technique offers several advantages over other scale-up production methods, such as the control over the microstructure, form, and size of the Nb dendrites. A critical current density of 10 kA/cm/sup 2/ at roughly 16.5 T has been measured for the fine dendrite materials.

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

    PubMed

    Nonnenmann, Stephen S

    2016-02-14

    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. PMID:26795921

  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 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.

  18. 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.

  19. In-Situ Transmission Electron Microscope High Temperature Behavior in Nanocrystalline Platinum Thin Films

    NASA Astrophysics Data System (ADS)

    Garcia, Davil; Leon, Alexander; Kumar, Sandeep

    2016-01-01

    In this work, we present a micro electro-mechanical systems (MEMS)-based in situ transmission electron microscope (TEM) experimental setup for high-temperature uniaxial tensile behavior of nanocrystalline thin films. This setup utilizes self-heating (Ohmic) to raise the temperature of thin films while applying uniaxial tensile loading using electro-thermal actuators. Self-heating is achieved by passing a high-density direct current through the specimen. We carried out a qualitative uniaxial tensile experiment on a 75-nm platinum thin film at 360 K. Temperature is estimated using COMSOL modeling. In this qualitative experiment, we observed initial grain growth followed by formation of edge serrations. We propose that grain boundary sliding coupled with grain growth is the underlying mechanism responsible for the observed behavior.

  20. In-situ high temperature irradiation setup for temperature dependent structural studies of materials under swift heavy ion irradiation

    NASA Astrophysics Data System (ADS)

    Kulriya, P. K.; Kumari, Renu; Kumar, Rajesh; Grover, V.; Shukla, R.; Tyagi, A. K.; Avasthi, D. K.

    2015-01-01

    An in-situ high temperature (1000 K) setup is designed and installed in the materials science beam line of superconducting linear accelerator at the Inter-University Accelerator Centre (IUAC) for temperature dependent ion irradiation studies on the materials exposed with swift heavy ion (SHI) irradiation. The Gd2Ti2O7 pyrochlore is irradiated using 120 MeV Au ion at 1000 K using the high temperature irradiation facility and characterized by ex-situ X-ray diffraction (XRD). Another set of Gd2Ti2O7 samples are irradiated with the same ion beam parameter at 300 K and simultaneously characterized using in-situ XRD available in same beam line. The XRD studies along with the Raman spectroscopic investigations reveal that the structural modification induced by the ion irradiation is strongly dependent on the temperature of the sample. The Gd2Ti2O7 is readily amorphized at an ion fluence 6 × 1012 ions/cm2 on irradiation at 300 K, whereas it is transformed to a radiation-resistant anion-deficient fluorite structure on high temperature irradiation, that amorphized at ion fluence higher than 1 × 1013 ions/cm2. The temperature dependent ion irradiation studies showed that the ion fluence required to cause amorphization at 1000 K irradiation is significantly higher than that required at room temperature irradiation. In addition to testing the efficiency of the in-situ high temperature irradiation facility, the present study establishes that the radiation stability of the pyrochlore is enhanced at higher temperatures.

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

    PubMed

    Li, Li; Weidner, Donald J

    2015-12-01

    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%. PMID:26724072

  2. 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%.

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

    NASA Astrophysics Data System (ADS)

    Li, Li; Weidner, Donald J.

    2015-12-01

    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%.

  4. 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

  5. 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.

  6. In-Situ Ultrafast 3D Imaging of Magma Vesiculation at High Temperature

    NASA Astrophysics Data System (ADS)

    Ulmer, P.; Pistone, M.; Caricchi, L.; Fife, J.; Marone, F.; Benson, P. M.; Almqvist, B.; Reusser, E.; Rust, A.; Burlini, L.

    2011-12-01

    We present new experimental results on magma vesiculation at high temperature. We investigated the processes of volatile exsolution (nucleation, growth and coalescence of gas bubbles) in magmas by performing in-situ high-temperature and ambient pressure experiments. Samples were heated with a newly-commissioned class 4 laser system and manual control. Simultaneously, the evolving 3D structure was captured by ultrafast synchrotron based X-ray tomographic microscopy (pixel size of 2.9 microns; 1 complete tomographic dataset acquired in 1 s), performed at the TOMCAT beam-line at Swiss Light Source (PSI, Villigen, Switzerland). Hydrous crystal- and bubble-free magmatic glasses liable to vesiculate at high temperature (400-1100 °C) were employed for the experiments. The samples used were cylindrical cores (2 mm in diameter and 2 mm in length), drilled from natural samples of obsidian (from: Lipari Island, Italy; Mayor Island, New Zealand; Tenerife Island, Spain; Little Glass Mountain, USA), containing different amounts of water (less than 1 wt%). These were chosen to represent a range of different physical properties (i.e., viscosity) as function of increasing temperature, due to their specific chemical compositions and, in particular, water content in the starting glass (measured via Karl Fischer titration). We observed the development of four different kinds of 3D microstructures during in-situ high-temperature experiments, depending on the starting material employed: (1) low vesicularity (40 vol%) with a narrow range in size of bubbles, which are generally spherical; (2) high vesicularity (80 vol%), showing a range of bubble sizes, shapes and extent of coalescence; (3) high vesicularity (85 vol%) and a polyhedral cell network (similar to reticulites); (4) a single expanding bubble. No magma fragmentation occurred in any of the experiments performed; we noticed different degrees of vertical thermal expansion, mainly depending on the amount of bubbles generated during

  7. 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

    2016-05-01

    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.

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

    NASA Astrophysics Data System (ADS)

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

    2016-03-01

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

  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. Sealed Rotors for In Situ High Temperature High Pressure MAS NMR†

    PubMed Central

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

    2015-01-01

    Here we present the design of reusable and perfectly-sealed all-zircornia MAS rotors. The rotors are used to study AlPO4-5 molecular sieve crystallization under hydrothermal conditions, high temperature high pressure cyclohexanol dehydration reaction, and low temperature metabolomics of intact biological tissue. PMID:26171928

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

    PubMed

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

    2015-09-11

    Here we present the design of reusable and perfectly sealed all-zirconia MAS rotors. The rotors are used to study AlPO4-5 molecular sieve crystallization under hydrothermal conditions, high temperature high pressure cyclohexanol dehydration reaction, and low temperature metabolomics of intact biological tissue. PMID:26171928

  12. Additive Manufacturing of Reactive In Situ Zr Based Ultra-High Temperature Ceramic Composites

    NASA Astrophysics Data System (ADS)

    Sahasrabudhe, Himanshu; Bandyopadhyay, Amit

    2016-03-01

    Reactive in situ multi-material additive manufacturing of ZrB2-based ultra-high-temperature ceramics in a Zr metal matrix was demonstrated using LENS™. Sound metallurgical bonding was achieved between the Zr metal and Zr-BN composites with Ti6Al4V substrate. Though the feedstock Zr power had α phase, LENS™ processing of the Zr powder and Zr-BN premix powder mixture led to the formation of some β phase of Zr. Microstructure of the Zr-BN composite showed primary grains of zirconium diboride phase in zirconium metal matrix. The presence of ZrB2 ceramic phase was confirmed by X-ray diffraction (XRD) analysis. Hardness of pure Zr was measured as 280 ± 12 HV and, by increasing the BN content in the feedstock, the hardness was found to increase. In Zr-5%BN composite, the hardness was 421 ± 10 HV and the same for Zr-10%BN composite was 562 ± 10 HV. It is envisioned that such multi-materials additive manufacturing will enable products in the future that cannot be manufactured using traditional approaches particularly in the areas of high-temperature metal-ceramic composites with compositional and functional gradation.

  13. 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

  14. 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

  15. In situ measurements of high temperature growth of correlated systems: a materials by design scheme

    NASA Astrophysics Data System (ADS)

    He, Hua

    There is great interest in developing new ways to use predictive theory to accelerate materials synthesis. We have previously shown that DFT +DMFT electronic structure calculations are successful at predicting gaps and ordered moments, even when correlations are very strong.[ 1 , 2 ] Building on these results, we set out to explore an even closer integration of theory and synthesis, aiming to discover new routes for doping Mott insulators and producing new superconductors. In situ high temperature high energy X-ray diffraction is used to determine the crystal structures of compounds just as they form from the growths, and the structural information is used as input for DFT +DMFT calculations that predict functionality, closing the synthesis loop by suggesting productive new directions. Using this approach, we have investigated the transition metal oxysulfide system Ba-Co-S-O and successfully discovered the new compound BaCoSO, and identified it as an interesting small gap Mott insulator by DFT +DMFT calculations even before any traditional crystal growth is attempted in the lab We acknowledge the Office of Assistant Secretary of Defense for Research and Engineering for providing the NSSEFF funds that supported this research.

  16. 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.

  17. 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.

  18. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-04-01

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

  20. 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.

  1. In situ X-ray ptychography imaging of high-temperature CO{sub 2} acceptor particle agglomerates

    SciTech Connect

    Høydalsvik, Kristin; Bø Fløystad, Jostein; Esmaeili, Morteza; Mathiesen, Ragnvald H.; Breiby, Dag W.; Zhao, Tiejun; Rønning, Magnus; Diaz, Ana; Andreasen, Jens W.

    2014-06-16

    Imaging nanoparticles under relevant reaction conditions of high temperature and gas pressure is difficult because conventional imaging techniques, like transmission electron microscopy, cannot be used. Here we demonstrate that the coherent diffractive imaging technique of X-ray ptychography can be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO{sub 2} capture material, was studied at a pressure of one atmosphere in air and in CO{sub 2}, at temperatures exceeding 600 °C. Images with a spatial resolution better than 200 nm were retrieved, and possibilities for improving the experiment are described.

  2. High temperature in-situ observations of multi-segmented metal nanowires encapsulated within carbon nanotubes by in-situ filling technique

    PubMed Central

    2012-01-01

    Multi-segmented one-dimensional metal nanowires were encapsulated within carbon nanotubes (CNTs) through in-situ filling technique during plasma-enhanced chemical vapor deposition process. Transmission electron microscopy (TEM) and environmental TEM were employed to characterize the as-prepared sample at room temperature and high temperature. The selected area electron diffractions revealed that the Pd4Si nanowire and face-centered-cubic Co nanowire on top of the Pd nanowire were encapsulated within the bottom and tip parts of the multiwall CNT, respectively. Although the strain-induced deformation of graphite walls was observed, the solid-state phases of Pd4Si and Co-Pd remain even at above their expected melting temperatures and up to 1,550 ± 50°C. Finally, the encapsulated metals were melted and flowed out from the tip of the CNT after 2 h at the same temperature due to the increase of internal pressure of the CNT. PMID:22873841

  3. In-situ electrochemical study of Zr1nb alloy corrosion in high temperature Li+ containing water

    NASA Astrophysics Data System (ADS)

    Krausová, Aneta; Macák, Jan; Sajdl, Petr; Novotný, Radek; Renčiuková, Veronika; Vrtílková, Věra

    2015-12-01

    Long-term in-situ corrosion tests were performed in order to evaluate the influence of lithium ions on the corrosion of zirconium alloy. Experiments were carried out in a high-pressure high-temperature loop (280 °C, 8 MPa) in a high concentration water solution of LiOH (70 and 200 ppm Li+) and in a simulated WWER primary coolant environment. The kinetic parameters characterising the oxidation process have been explored using in-situ electrochemical impedance spectroscopy and slow potentiodynamic polarization. Also, a suitable equivalent circuit was suggested, which would approximate the impedance characteristics of the corrosion of Zr-1Nb alloy. The Mott-Schottky approach was used to determine the semiconducting character of the passive film.

  4. In situ high-temperature infrared emissivity spectroscopy of silicate glasses and glass-ceramics

    NASA Astrophysics Data System (ADS)

    Santos, Cristiane N.; de Sousa Meneses, Domingos; Montouillout, Valerie; Echegut, Patrick

    2011-03-01

    Glasses and glass-ceramics are materials of widespread application in industry, building, photonics, microelectronics and medicine. Glass-ceramics are obtained by controlled glass crystallization, and many efforts have been done in the last years to better understand the structural changes occurring in this process. Here we show that in situ infrared emissivity spectroscopy is also a suitable technique for this purpose and a wide spectral and temperature range could be accessed (25-16000 cm-1 and 400-1700 K, respectively). We use a home-made instrument composed of two spectrometers, and a CO2 laser for locally heat the glass samples up to the melt. A dielectric function model was applied to fit the experimental data and compute the materials optical properties. We show that using new decomposition procedure quantitative information on the distribution of the Qn tetrahedral units (n being the number of bridging oxygen) can be obtained. The results at room temperature are in good agreement with recent molecular dynamics simulations. The major changes occur during quartz crystallization, with a remarkable increase of Q4 units. Supported by ANR Postre.

  5. 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.

  6. Crystal structure of a high-pressure/high-temperature phase of alumina by in situ X-ray diffraction.

    PubMed

    Lin, Jung-Fu; Degtyareva, Olga; Prewitt, Charles T; Dera, Przemyslaw; Sata, Nagayoshi; Gregoryanz, Eugene; Mao, Ho-Kwang; Hemley, Russell J

    2004-06-01

    Alumina (alpha-Al(2)O(3)) has been widely used as a pressure calibrant in static high-pressure experiments and as a window material in dynamic shock-wave experiments; it is also a model material in ceramic science. So understanding its high-pressure stability and physical properties is crucial for interpreting such experimental data, and for testing theoretical calculations. Here we report an in situ X-ray diffraction study of alumina (doped with Cr(3+)) up to 136 GPa and 2,350 K. We observe a phase transformation that occurs above 96 GPa and at high temperatures. Rietveld full-profile refinements show that the high-pressure phase has the Rh(2)O(3) (II) (Pbcn) structure, consistent with theoretical predictions. This phase is structurally related to corundum, but the AlO(6) polyhedra are highly distorted, with the interatomic bond lengths ranging from 1.690 to 1.847 A at 113 GPa. Ruby luminescence spectra from Cr(3+) impurities within the quenched samples under ambient conditions show significant red shifts and broadening, consistent with the different local environments of chromium atoms in the high-pressure structure inferred from diffraction. Our results suggest that the ruby pressure scale needs to be re-examined in the high-pressure phase, and that shock-wave experiments using sapphire windows need to be re-evaluated. PMID:15146173

  7. 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

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

    NASA Astrophysics Data System (ADS)

    Ohuchi, Tomohiro; Nishihara, Yu; Seto, Yusuke; Kawazoe, Takaaki; Nishi, Masayuki; Maruyama, Genta; Hashimoto, Mika; Higo, Yuji; Funakoshi, Ken-ichi; Suzuki, Akio; Kikegawa, Takumi; Irifune, Tetsuo

    2015-06-01

    Simple-shear deformation experiments on polycrystalline olivine and olivine single-crystal were conducted at pressures of 1.3-3.8 GPa and temperatures of 1223-1573 K to understand the achievement of steady-state fabric strength and the process of dynamic recrystallization. Development of crystallographic preferred orientation (CPO) of olivine was evaluated from two-dimensional X-ray diffraction patterns, and shear strain was measured from X-ray radiographs. 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 [0 1 0] 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 (70 vol.% olivine + 30 vol.% minor phases) 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 fabric. Experimental results on the deformation of single-crystal olivine showed that the CPO of olivine is influenced by the initial orientation of the starting single crystal because strain is concentrated in the recrystallized areas and the relic of the starting single crystal remains. In the upper mantle, the old CPO of olivine developed in the past may affect the olivine CPO developed in the present.

  9. Injection well with high-pressure, high-temperature in situ down-hole steam formation

    SciTech Connect

    Marr, A.W.

    1981-12-01

    A portion of an injection well adjacent an oil-bearing earth formation is sealed off by spaced-apart high-pressure-resistant plugs, and water is charged into the bore-hole space between the plugs at a sufficient rate to effect sustained water pressure in the range of from 400 to 25,000 psi. Under such pressure sufficient current is passed between two electrodes in the water to convert from 10 to 33 barrels of water per hour into steam.

  10. Fracture Evaluation of In-Situ Sensors for High Temperature Applications

    NASA Technical Reports Server (NTRS)

    Forth, Scott C.; Staroselsky, Alexander

    2003-01-01

    The feasibility of fabricating an in-situ crack sensor for real-time detection of surface cracks propagating in engine components was evaluated using a computational fracture mechanics model. The in-situ sensor system would be required to: (1) Be capable of sustaining normal function in a severe environment; (2) Transmit a signal if a detected crack in the component was above a predetermined length, but below a critical length that would lead to failure; (3) Act neutrally upon the overall performance of the engine system and not interfere with the engine maintenance operations. In this work, fracture mechanics methodologies are used to identify the requirements for an in-situ sensor system that could withstand the engine operating environment, foreign object damage, and minimally degrade engine performance. A computational fracture mechanics model was developed to evaluate the feasibility of fabricating an in-situ crack sensor for real-time damage propagation detection in engine components.

  11. In situ observation of low temperature growth of Ge on Si(1 1 1) by reflection high energy electron diffraction

    NASA Astrophysics Data System (ADS)

    Grimm, Andreas; Fissel, Andreas; Bugiel, Eberhard; Wietler, Tobias F.

    2016-05-01

    In this paper we investigate the initial stages of epitaxial growth of Ge on Si(1 1 1) and the impact of growth temperature on strain evolution in situ by reflection high energy electron diffraction (RHEED) for temperatures between 200 °C and 400 °C. The change in surface morphology from a flat wetting layer to subsequent islanding that is characteristic for Stranski-Krastanov growth is monitored by spot intensity analysis. The corresponding critical layer thickness is determined to 3.1 < dc < 3.4 ML. In situ monitoring of the strain relaxation process reveals a contribution of the Si(1 1 1) 7 × 7-surface reconstruction to the strain relaxation process. High resolution transmission electron microscopy confirms that the Ge islands exhibit a high degree of structural perfection and an ordered interfacial misfit dislocation network already at a growth temperature of 200 °C is established. The temperature dependency of island shape, density and height is characterized by atomic force microscopy and compared to the RHEED investigations.

  12. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2014-12-01

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

  14. In situ biaxial rotation at low-temperatures in high magnetic fields.

    PubMed

    Selby, N S; Crawford, M; Tracy, L; Tracey, L; Reno, J L; Pan, W

    2014-09-01

    We report the design, construction, and characterization of a biaxial sample rotation stage for use in a cryogenic system for orientation-dependent studies of anisotropic electronic transport phenomena at low temperatures and high magnetic fields. Our apparatus allows for continuous rotation of a sample about two axes, both independently and simultaneously. PMID:25273781

  15. In situ biaxial rotation at low-temperatures in high magnetic fields

    SciTech Connect

    Selby, N. S.; Crawford, M.; Tracy, L.; Reno, J. L.; Pan, W.

    2014-09-15

    We report the design, construction, and characterization of a biaxial sample rotation stage for use in a cryogenic system for orientation-dependent studies of anisotropic electronic transport phenomena at low temperatures and high magnetic fields. Our apparatus allows for continuous rotation of a sample about two axes, both independently and simultaneously.

  16. 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.

  17. Deformation of olivine under mantle conditions: An in situ high-pressure, high-temperature study using monochromatic synchrotron radiation

    SciTech Connect

    Hilairet, Nadège; Wang, Yanbin; Sanehira, Takeshi; Merkel, Sébastien; Mei, Shenghua

    2012-03-15

    Polycrystalline samples of San Carlos olivine were deformed at high-pressure (2.8-7.8 GPa), high-temperature (1153 to 1670 K), and strain rates between 7.10{sup -6} and 3.10{sup -5} s{sup -1}, using the D-DIA apparatus. Stress and strain were measured in situ using monochromatic X-rays diffraction and imaging, respectively. Based on the evolution of lattice strains with total bulk strain and texture development, we identified three deformation regimes, one at confining pressures below 3-4 GPa, one above 4 GPa, both below 1600 K, and one involving growth of diffracting domains associated with mechanical softening above {approx}1600 K. The softening is interpreted as enhanced grain boundary migration and recovery. Below 1600 K, elasto-plastic self-consistent analysis suggests that below 3-4 GPa, deformation in olivine occurs with large contribution from the so-called 'a-slip' system [100](010). Above {approx}4 GPa, the contribution of the a-slip decreases relative to that of the 'c-slip' [001](010). This conclusion is further supported by texture refinements. Thus for polycrystalline olivine, the evolution in slip systems found by previous studies may be progressive, starting from as low as 3-4 GPa and up to 8 GPa. During such a gradual change, activation volumes measured on polycrystalline olivine cannot be linked to a particular slip system straightforwardly. The quest for 'the' activation volume of olivine at high pressure should cease at the expense of detailed work on the flow mechanisms implied. Such evolution in slip systems should also affect the interpretation of seismic anisotropy data in terms of upper mantle flow between 120 and 300 km depth.

  18. 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

    2016-04-01

    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.

  19. 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.

  20. Lubricous Deposit Formed In Situ Between Wearing Surfaces at High Temperatures

    NASA Technical Reports Server (NTRS)

    1996-01-01

    Many components of future aircraft will be constructed from novel high-temperature materials, such as superalloys and ceramic composites, to meet expected operating temperatures in excess of 300 C. There are no known liquid lubricants that can lubricate above 300 C without significant decomposition. Solid lubricants could be considered, but problems caused by the higher friction coefficients and wear rates of the solid lubricant film make this an undesirable approach. An alternative method of lubrication is currently being investigated: vapor phase lubrication. In vapor phase lubrication, an organic liquid (in our studies a thioether was used) is vaporized into a flowing air stream that is directed to sliding surfaces where lubrication is needed. The organic vapor reacts at the concentrated contact sliding area generating a lubricous deposit. This deposit has been characterized as a thin polymeric film that can provide effective lubrication at temperatures greater than 400 C. Initial tribological studies were conducted at the NASA Lewis Research Center and Cleveland State University with a high-temperature friction and wear tribometer. A cast iron rod was loaded (a 4-kg mass was used to generate a contact pressure of 1.2 MPa) against a reciprocating, cast iron plate at 500 C. This system was then lubricated with the vapor phase of thioether.

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

    NASA Technical Reports Server (NTRS)

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

    2013-01-01

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

  2. 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.

  3. High-temperature dehydration of talc: a kinetics study using in situ X-ray powder diffraction

    NASA Astrophysics Data System (ADS)

    Wang, Duojun; Yi, Li; Huang, Bojin; Liu, Chuanjiang

    2015-06-01

    High-temperature in situ X-ray powder diffraction patterns were used to study the dehydration kinetics of natural talc with a size of 10-15 µm. The talc was annealed from 1073 to 1223 K, and the variations in the characteristic peaks corresponding to talc with the time were recorded to determine the reaction progress. The decomposition of talc occurred, and peaks corresponding to talc and peaks corresponding to enstatite and quartz were observed. The enstatite and talc exhibited a topotactic relationship. The dehydration kinetics of talc was studied as a function of temperature between 1073 and 1223 K. The kinetics data could be modeled using an Avrami equation that considers nucleation and growth processes ? where n varies from 0.4 to 0.8. The rate constant (k) equation for the natural talc is ? The reaction mechanism for the dehydration of talc is a heterogeneous nucleation and growth mechanism.

  4. In situ high temperature oxidation analysis of Zircaloy-4 using acoustic emission coupled with thermogravimetry

    NASA Astrophysics Data System (ADS)

    Omar, Al Haj; Véronique, Peres; Eric, Serris; François, Grosjean; Jean, Kittel; François, Ropital; Michel, Cournil

    2015-06-01

    Zircaloy-4 oxidation behavior at high temperature (900 °C), which can be reached in case of severe accidental situations in nuclear pressurised water reactor, was studied using acoustic emission analysis coupled with thermogravimetry. Two different atmospheres were used to study the oxidation of Zircaloy-4: (a) helium and pure oxygen, (b) helium and oxygen combined with slight addition of air. The experiments with 20% of oxygen confirm the dependence on oxygen anions diffusion in the oxide scale. Under a mixture of oxygen and air in helium, an acceleration of the corrosion was observed due to the detrimental effect of nitrogen. The kinetic rate increased significantly after a kinetic transition (breakaway). This acceleration was accompanied by an acoustic emission activity. Most of the acoustic emission bursts were recorded after the kinetic transition (post-transition) or during the cooling of the sample. The characteristic features of the acoustic emission signals appear to be correlated with the different populations of cracks and their occurrence in the ZrO2 layer or in the α-Zr(O) layer. Acoustic events were recorded during the isothermal dwell time at high temperature under air. They were associated with large cracks in the zirconia porous layer. Acoustic events were also recorded during cooling after oxidation tests both under air or oxygen. For the latter, cracks were observed in the oxygen enriched zirconium metal phase and not in the dense zirconia layer after 5 h of oxidation.

  5. 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.

  6. Reactions Between Silicon and Graphite Substrates at High Temperature: In Situ Observations

    NASA Astrophysics Data System (ADS)

    White, Jesse F.; Ma, Luyao; Forwald, Karl; Sichen, Du

    2013-09-01

    Graphite as a refractory material has found wide application in many process steps to produce photovoltaic silicon. In the current study, the melting behavior of silicon in contact with different grades of graphite was investigated. The infiltration of silicon into graphite was found to be highly dependent on the internal structure of the graphite substrate. It was confirmed that the heating history of silicon in contact with a graphite substrate strongly influences the melting behavior, which is likely attributed to a gas-solid reaction that forms SiC at less than the liquidus temperature of silicon and alters the surface properties of the graphite. It was also observed that a concentration of CO greater than 5 pct in the inlet gas leads to SiC formation on the surface of the silicon and severely hinders melting.

  7. In situ temperature jump high-frequency dynamic nuclear polarization experiments: enhanced sensitivity in liquid-state NMR spectroscopy.

    PubMed

    Joo, Chan-Gyu; Hu, Kan-Nian; Bryant, Jeffrey A; Griffin, Robert G

    2006-07-26

    We describe an experiment, in situ temperature jump dynamic nuclear polarization (TJ-DNP), that is demonstrated to enhance sensitivity in liquid-state NMR experiments of low-gamma spins--13C, 15N, etc. The approach consists of polarizing a sample at low temperature using high-frequency (140 GHz) microwaves and a biradical polarizing agent and then melting it rapidly with a pulse of 10.6 microm infrared radiation, followed by observation of the NMR signal in the presence of decoupling. In the absence of polarization losses due to relaxation, the enhancement should be epsilon+ = epsilon(T(obs)/T(mu)(wave)), where epsilon+ is the observed enhancement, epsilon is the enhancement obtained at the temperature where the polarization process occurs, and T(mu)(wave) and T(obs) are the polarization and observation temperatures, respectively. In a single experimental cycle, we observe room-temperature enhancements, epsilon(dagger), of 13C signals in the range 120-400 when using a 140 GHz gyrotron microwave source, T(mu)(wave) = 90 K, and T(obs) = 300 K. In addition, we demonstrate that the experiment can be recycled to perform signal averaging that is customary in contemporary NMR spectroscopy. Presently, the experiment is applicable to samples that can be repeatedly frozen and thawed. TJ-DNP could also serve as the initial polarization step in experiments designed for rapid acquisition of multidimensional spectra. PMID:16848479

  8. 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

    2015-04-01

    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. PMID:25815414

  9. 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.

  10. In Situ Neutron and Synchrotron X-ray Diffraction Studies of Jarosite at High-Temperature High-Pressure Conditions

    NASA Astrophysics Data System (ADS)

    Xu, H.; Zhao, Y.; Hickmott, D.; Zhang, J.; Vogel, S.; Daemen, L.; Hartl, M.

    2011-03-01

    Jarosite (KFe 3 (SO4)2 (OH)6) occurs in acid mine drainage and epithermal environments and hot springs associated with volcanic activity. Jarosite is also of industrial interest as an iron-impurity extractor from zinc sulfide ores. In 2004, jarosite was detected by the Mars Exploration Rover Mössbauer spectrometer, which has been interpreted as a strong evidence for the existence of water (and possibly life) on ancient Mars. This discovery has spurred considerable interests in stability and structural behavior of jarosite and related phases at various temperature, pressure, and aqueous conditions. In this work, we have investigated the crystal structure and phase stability of jarosite at temperatures up to 900 K and/or pressures up to 9 GPa using in situ neutron and synchrotron X-ray diffraction. To avoid the large incoherent scattering of neutrons by hydrogen, a deuterated sample was synthesized and characterized. Rietveld analysis of the obtained diffraction data allowed determination of unit-cell parameters, atomic positions and atomic displacement parameters as a function of temperature and pressure. In addition, the coefficients of thermal expansion, bulk moduli and pressure-temperature stability regions of jarosite were determined.

  11. In-situ, in air, high-temperature phase transformations in rare-earth niobates and titanium oxides (dysprosium and yttrium) using a thermal-image furnace

    NASA Astrophysics Data System (ADS)

    Siah, Lay Foong

    Thermal-image furnaces afford two major advantages over the conventional resistance heating systems for high-temperature studies of oxides in air, namely: (i) the highly localized heating allows temperatures in excess of 2500°C to be reached in air or in an oxidizing atmosphere, and (ii) no sample contamination from volatile furnace components since the sample is heated by absorption of a focused, high intensity light beam. In this work, we developed a compact furnace powered by four halogen infrared reflector lamps (150 W each), for in-situ high-temperature studies using synchrotron radiation. The primary objective was to evaluate the feasibility of the thermal-image technique for in-situ, in air, studies of high-temperature phase transformations in oxide ceramics. Specifically, the issues of temperature measurement and reliability of results obtained in comparison with published literature were addressed. The use of a co-existent "in-situ thermometer" was found to be a viable method to monitor the sample temperature in the image "hot-spot". Studies of YNbO4 and DyNbO4 revealed the existence of a new cubic phase at elevated temperatures beyond the commonly known ferroelastic monoclinic-to-paraelastic tetragonal transformations. A series of high-temperature powder patterns of the pure hexagonal phase of DY2TiO5 was also collected in-situ, in air.

  12. 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

  13. 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.

  14. In-situ X-ray diffraction analysis of zirconia layer formed on zirconium alloys oxidized at high temperature

    NASA Astrophysics Data System (ADS)

    Gosset, D.; Le Saux, M.

    2015-03-01

    In the case of a hypothetical loss of primary coolant accident (LOCA) in a light water reactor, the zirconium alloys fuel cladding would be oxidized in steam at high temperature, typically in the range 800-1200 °C. The monoclinic to tetragonal phase martensitic transition of zirconia occurs within this temperature range and complex phenomena possibly having an impact on the oxidation kinetics are then to be expected. In order to provide an accurate description of the structure and microstructure of the oxide layers, systematic X-ray diffraction analyses have been performed in-situ under oxidizing atmosphere at high temperature (between 800 and 1100 °C) on Zircaloy-4 and M5™ sheet samples. It was confirmed that the volume fraction of the tetragonal and monoclinic zirconia phases formed during oxide growth drastically depends on the oxidation temperature. For example, the few outer microns of the oxide are fully tetragonal above 1050 °C and contain only 20% of tetragonal phase at 800 °C. It was also shown that cooling after oxidation induces irreversible phase transitions within the oxide. As a consequence, both the structure and the microstructure of the growing oxide cannot be observed post-facto, neither at room temperature nor after reheating at the prior oxidation temperature. It has been deduced from microstructural analyses that the grain size of the tetragonal zirconia phase is nanometric, about 100 nm during oxidation at 1100 °C down to 20 nm after cooling down to room temperature. This small grain size allows the stabilization of the tetragonal phase. The lattice parameters of the monoclinic and tetragonal zirconia phases have been analyzed, during both high temperature oxidation and cooling. In both cases, it appears the 'a' and 'b' cell parameters of the monoclinic phase are strongly constrained by the tetragonal 'a' one. The structural characteristics of the oxide formed at high temperature on Zircaloy-4 and M5™ are quite similar. All those

  15. 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. PMID:25284768

  16. 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

  17. 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. PMID:27475566

  18. 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.

  19. 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. PMID:26914998

  20. 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.

  1. 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

  2. In-Situ Study of Gaseous Reduction of Magnetite Doped with Alumina Using High-Temperature XRD Analysis

    NASA Astrophysics Data System (ADS)

    Kapelyushin, Yury; Sasaki, Yasushi; Zhang, Jianqiang; Jeong, Sunkwang; Ostrovski, Oleg

    2015-12-01

    The reduction of magnetite of technical grade and magnetite doped with 3 mass pct Al2O3 was studied in situ using high-temperature XRD (HT-XRD) analysis. Magnetite was reduced by CO-CO2 gas (80 vol pct CO) at 1023 K (750 °C). Reduction of magnetite doped with alumina occurred from the Fe3O4-FeAl2O4 solid solution which has a miscibility gap with critical temperature of 1133 K (860 °C). The degree of reduction of magnetite was derived using Rietveld refinement of the HT-XRD spectra; the compositions of the Fe3O4-FeAl2O4 solid solution and the concentrations of carbon in γ-iron were determined from the lattice constants of the solutions. The reduction of magnetite progressed topochemically with the formation of a dense iron shell. The reduction of alumina-containing magnetite started along certain lattice planes with the formation of a network-like structure. Reduction of alumina-containing magnetite was faster than that of un-doped magnetite; this difference was attributed to the formation of the network-like structure. Hercynite content in the Fe3O4-FeAl2O4 solid solution in the process of reduction of magnetite doped with 3 mass pct Al2O3 increased from 5.11 to 20 mass pct, which is close to the miscibility gap at 1023 K (750 °C). The concentration of carbon in γ-Fe (0.76 mass pct) formed in the reduced sample of magnetite doped with 3 mass pct Al2O3 was close to the equilibrium value with 80 vol pct CO to 20 vol pct CO2 gas used in the HT-XRD experiments.

  3. 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.

  4. In situ high-temperature scanning tunneling microscopy studies of early stage growth kinetics during titanium nitride epitaxy

    NASA Astrophysics Data System (ADS)

    Kodambaka, Suneel Kumar

    NaCl-structure TiN is widely used as a hard wear-resistant coating on cutting tools, as a diffusion-barrier layer in microelectronic devices, as a corrosion-resistant coating on mechanical components, and as an abrasion-resistant layer on optics and architectural glass. Even though its diffusion barrier and elastic properties are known to be anisotropic, and hence depend upon grain orientation, little is known regarding the mechanisms and reaction paths leading to the development of preferred orientation in polycrystalline TiN layers deposited by reactive evaporation and sputter deposition. Efforts to model polycrystalline growth as a function of deposition conditions is a complex problem. As a minimum set, one requires adatom transport parameters---activation barriers for surface diffusion step edge attachment/detachment, the adatom formation energy, the step edge Ehrlich barrier, and the step formation energy---all as a function of orientation. Unfortunately, very little data, either experimental or theoretical, is available concerning these parameters for TiN. During the course of my research, I have developed methods to grow atomically-smooth TiN(001) and (111) single-crystal layers with simple well-defined single-atom-high 2D island configurations on large atomically-smooth terraces. I used in situ scanning tunneling microscopy to study time- and temperature-dependent 2D island coarsening/decay kinetics, obtain 2D equilibrium island shapes, and follow temporal fluctuations of island shapes on both TiN(001) and (111) surfaces. I have developed a combination of experimental and theoretical techniques to analyze the surface dynamics measurements and determined adatom surface transport parameters, step energies, step stiffnesses, and kink formation energies on TiN(001) and TiN(111) surfaces.

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

    PubMed

    Liu, Chuan-jiang; Zheng, Hai-fei

    2012-02-01

    The phase transitions of calcite at high temperature and high pressure were investigated by using hydrothermal diamond anvil cell combined with Raman spectroscopy. The result showed that the Raman peak of 155 cm(-1) disappeared, the peak of 1 087 cm(-1) splited into 1083 and 1 090 cm(-1) peaks and the peak of 282 cm(-1) abruptly reduced to 231 cm(-1) at ambient temperature when the system pressure increased to 1 666 and 2 127 MPa respectively, which proved that calcite transformed to calcite-II and calcite-III. In the heating process at the initial pressure of 2 761 MPa and below 171 degrees C, there was no change in Raman characteristic peaks of calcite-III. As the temperature increased to 171 degrees C, the color of calcite crystal became opaque completely and the symmetric stretching vibration peak of 1 087 cm(-1), in-plane bending vibration peak of 713 cm(-1) and lattice vibration peaks of 155 and 282 cm(-1) began to mutate, showing that the calcite-III transformed to a new phase of calcium carbonate at the moment. When the temperature dropped to room temperature, this new phase remained stable all along. It also indicated that the process of phase transformation from calcite to the new phase of calcium carbonate was irreversible. The equation of phase transition between calcite-III and new phase of calcium carbonate can be determined by P(MPa) = 9.09T x (degrees C) +1 880. The slopes of the Raman peak (v1 087) of symmetrical stretching vibration depending on pressure and temperature are dv/dP = 5.1 (cm(-1) x GPa(-1)) and dv/dT = -0.055 3(cm(-1) x degrees C(-1)), respectively. PMID:22512172

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

    PubMed

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

    2014-05-27

    High-temperature in situ electron microscopy and X-ray diffraction have revealed that Au and Fe2O3 particles fuse in a fluid fashion at temperatures far below their size-reduced melting points. With increasing temperature, the fused particles undergo a sequence of complex structural transformations from surface alloy to phase segregated and ultimately core-shell structures. The combination of in situ electron microscopy and spectroscopy provides insights into fundamental thermodynamic and kinetic aspects governing the formation of heterogeneous nanostructures. The observed structural transformations present an interesting analogy to thin film growth on the curved surface of a nanoparticle. Using single-particle observations, we constructed a phase diagram illustrating the complex relationships among composition, morphology, temperature, and particle size. PMID:24758698

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

    NASA Astrophysics Data System (ADS)

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

    2015-11-01

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

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

    DOE PAGESBeta

    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 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

  9. 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.

  10. 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.

  11. 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.

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

    PubMed

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

    2015-01-01

    Pressure measurements in high-temperature applications, including compressors, turbines, and others, have become increasingly critical. This paper proposes an implantable passive LC pressure sensor based on an alumina ceramic material for in situ pressure sensing in high-temperature environments. The inductance and capacitance elements of the sensor were designed independently and separated by a thermally insulating material, which is conducive to reducing the influence of the temperature on the inductance element and improving the quality factor of the sensor. In addition, the sensor was fabricated using thick film integrated technology from high-temperature materials that ensure stable operation of the sensor in high-temperature environments. Experimental results showed that the sensor accurately monitored pressures from 0 bar to 2 bar at temperatures up to 800 °C. The sensitivity, linearity, repeatability error, and hysteretic error of the sensor were 0.225 MHz/bar, 95.3%, 5.5%, and 6.2%, respectively. PMID:26334279

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

    PubMed Central

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

    2015-01-01

    Pressure measurements in high-temperature applications, including compressors, turbines, and others, have become increasingly critical. This paper proposes an implantable passive LC pressure sensor based on an alumina ceramic material for in situ pressure sensing in high-temperature environments. The inductance and capacitance elements of the sensor were designed independently and separated by a thermally insulating material, which is conducive to reducing the influence of the temperature on the inductance element and improving the quality factor of the sensor. In addition, the sensor was fabricated using thick film integrated technology from high-temperature materials that ensure stable operation of the sensor in high-temperature environments. Experimental results showed that the sensor accurately monitored pressures from 0 bar to 2 bar at temperatures up to 800 °C. The sensitivity, linearity, repeatability error, and hysteretic error of the sensor were 0.225 MHz/bar, 95.3%, 5.5%, and 6.2%, respectively. PMID:26334279

  14. 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.

  15. In situ X-ray observations of the melting relations in the Fe-S-H system under high pressure and high temperature

    NASA Astrophysics Data System (ADS)

    Shibazaki, Y.; Stagno, V.; Higo, Y.; Fei, Y.

    2013-12-01

    Sulfur and hydrogen are two of the most plausible light elements in the planetary cores. Particularly the cores of icy satellites, such as Ganymede, are considered to contain a significant amount of those elements based on studies of meteorites. Therefore, it is essential to investigate the properties of iron alloyed with those light elements at high pressure and high temperature, in order to shed light on the composition and structure of the cores. To date, the Fe-FeS system has been extensively investigated at high pressure and temperature. Hydrogen is known to dissolve in interstitial sites of Fe and FeS lattices and strongly depresses the melting temperatures. However, it is still not clear how hydrogen affects the eutectic point (temperature and composition) of the Fe-FeS system. In order to understand the melting relations in the Fe-S-H system, we have performed in situ X-ray diffraction experiments at high pressure and high temperature. The experiments were carried out using the multi-anvil apparatus at the BL04B1 beamline of SPring-8, Japan, up to 10 GPa and 1700 K. Fe-FeS powder mixtures (15.5 wt% S and 30 wt %S) were packed into a NaCl capsule along with LiAlH4. Hydrogen was supplied to the Fe-FeS sample by a thermal decomposition of LiAlH4. The Fe-FeS sample was separated from LiAlH4 using a thin MgO disk to avoid the direct chemical reaction between the sample and LiAlH4. The NaCl capsule is able to seal hydrogen effectively at high pressure and high temperature. The diffraction patterns were collected for a period of 300 s at a temperature interval of 50-100 K. The collected diffraction data show that FeHx and FeSHx were synthesized at high temperature and then the sample was totally molten via a partial melting with increasing temperature. Since the atomic volumes of Fe and FeS expand due to the hydrogen dissolution (hydrogenation), the hydrogen concentrations in FeHx and FeSHx were estimated by comparing the volumes of between Fe and FeHx or between

  16. 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.

  17. Design and application of a high-temperature microfurnace for an in situ X-ray diffraction study of phase transformation.

    PubMed

    Eu, W S; Cheung, W H; Valix, M

    2009-11-01

    Thermal treatment of mineral ores such as ilmenite can initiate phase transformations that could affect their activation or deactivation, subsequently influencing their ability to dissolve in a leaching agent. Most laboratory-based X-ray diffraction (XRD) studies were carried out ex situ in which realistic diffraction patterns could not be obtained simultaneously with occurring reactions and were time-consuming. The availability of synchrotron-radiation-based XRD not only allows in situ analysis, but significantly shortens the data recording time. The present study details the design of a robust high-temperature microfurnace which allows thermal processing of mineral ore samples and the simultaneous collection of high-resolution synchrotron XRD data. In addition, the application of the manufactured microfurnace for in situ study of phase transformations of ilmenite ore under reducing conditions is demonstrated. PMID:19844022

  18. A high-temperature in situ cell with a large solid angle for fluorescence X-ray absorption fine structure measurement.

    PubMed

    Murata, Naoyoshi; Kobayashi, Makoto; Okada, Yukari; Suzuki, Takuya; Nitani, Hiroaki; Niwa, Yasuhiro; Abe, Hitoshi; Wada, Takahiro; Mukai, Shingo; Uehara, Hiromitsu; Ariga, Hiroko; Takakusagi, Satoru; Asakura, Kiyotaka

    2015-03-01

    We present the design and performance of a high-temperature in situ cell with a large solid angle for fluorescence X-ray absorption fine structure (XAFS) spectra. The cell has a large fluorescence XAFS window (116 mm(ϕ)) near the sample in the cell, realizing a large half-cone angle of 56°. We use a small heater (25 × 35 mm(2)) to heat the sample locally to 873 K. We measured a Pt-SnO2 thin layer on a Si substrate at reaction conditions having a high activity. In situ measurement enables the analysis of the difference XAFS spectra between before and during the reaction to reveal the structure change during the operation. PMID:25832248

  19. 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.

    2016-07-01

    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.

  20. 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.

  1. X ray attenuation measurements for high-temperature materials characterization and in-situ monitoring of damage accumulation. Ph.D. Thesis - Cleveland State Univ., 1991

    NASA Technical Reports Server (NTRS)

    Baaklini, George Y.

    1992-01-01

    The scope of this dissertation is to develop and apply 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. This dissertation results in the development of: (1) a point scan digital radiography system, and (2) an in-situ x ray material testing system. Radiographic evaluation before, during, and after loading shows the effect of preexisting volume flaws on the fracture behavior of composites. Results show that x ray film radiography can monitor damage accumulation during tensile loading. Matrix cracking, fiber matrix debonding, fiber bridging, and fiber pullout are imaged throughout the tensile loading of the specimens. Further in-situ radiography is found to be a practical technique for estimating interfacial shear strength between the silicon carbide fibers and the reaction bonded silicon nitride matrix. It is concluded that pretest, in-situ, and post test x ray imaging can provide for greater understanding of ceramic matrix composite mechanical behavior.

  2. 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

    2016-05-01

    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.

  3. 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.

    NASA Astrophysics Data System (ADS)

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

    2007-12-01

    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 high pressure minerals. 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 a new experimental design that was tested at HPCAT sector 16 BMD of the Advanced Photon Source. This method allows in situ measurement of stresses and textures in the DAC at simultaneously high- pressures and -temperatures. Details of this new technique that uses radial diffraction geometry are discussed, including the uses of amorphous boron gaskets, external heating using graphite heater, and membrane pressure control. Current coverage in pressure and temperature (~30 GPa and 1100 oC). The use of the method will be demonstrated with in situ texture measurements on the high-pressure phases of iron. In the experiment, we were able to observe strong textures in bcc-Fe, track the evolution of the texture with increasing temperature and during the bcc to fcc phase transition. Finally, we observed plastic deformation in the fcc phase between 5 and 15 GPa at 850 oC till the nucleation of hcp-Fe.

  4. Sound velocities measurement on MgSiO3 akimotoite at high pressures and high temperatures with simultaneous in situ X-ray diffraction and ultrasonic study

    NASA Astrophysics Data System (ADS)

    Zhou, Chunyin; Gréaux, Steeve; Nishiyama, Norimasa; Irifune, Tetsuo; Higo, Yuji

    2014-03-01

    Elastic wave velocities of MgSiO3 akimotoite polycrystalline samples have been measured at pressures up to 25.7 GPa and temperatures to 1500 K by a combination of in situ X-ray diffraction and ultrasonic interferometry techniques in a large volume Kawai-type multianvil apparatus (KMA). The elastic moduli of akimotoite and their pressure and temperature dependences are determined by a 2D linear fitting analysis of the present data, yielding: KS = 219.4(7) GPa, ∂KS/∂P = 4.62(3), ∂KS/∂T = -0.0228(4) GPa/K, G0 = 132.1(7) GPa, ∂G/∂P = 1.63(4), ∂G/∂T = -0.0225(4) GPa/K. The bulk and shear moduli at ambient conditions are generally consistent with the result of a previous Brillouin study. However, significant nonlinear behaviors of the elastic moduli were observed at higher temperatures, indicating that the velocities derived from the linear fitting analysis are overestimated for the actual mantle conditions. Using the present new experimental data, we compared the elastic velocities of various high-pressure forms of MgSiO3 under the mantle conditions. The results demonstrate a large velocity difference between akimotoite and perovskite, which may be relevant to the complex seismic structures near the bottom of the mantle transition zone.

  5. An In Situ High Temperature Investigation of Cation Environments in Aluminate and Silicate Glasses and Liquids at the LUCIA Beamline

    SciTech Connect

    Neuville, Daniel R.; Roux, Jacques; Cormier, Laurent; Ligny, Dominique de; Flank, Anne-Marie; Lagarde, Pierre; Henderson, Grant S.

    2007-02-02

    The structure of crystals and melts were obtained at high temperature using X-ray absorption at the Ca K-edge on CaMgSi2O6 (diopside), CaAl2Si2O8 (anorthite), Ca3Al2O6 (C3A) and CaAl2O4 (CA) compositions. Important changes are observed above the liquidus temperature particularly for the C3A composition where all oscillations in the XANES spectra disappear. Important changes in the Ca K-edge XANES are also visible in the pre-edge region, with increasing temperature, for crystalline CaMgSi2O6.

  6. In situ high temperature magnetic force microscope analysis of thermal stability in the granular-type FePt-MgO double-layered perpendicular recording media

    NASA Astrophysics Data System (ADS)

    Singh, Amarendra K.; Zhang, Zhengang; Yin, Jinhua; Suzuki, Takao

    2005-05-01

    Thermal stability of written bits with different linear densities on granular-type FePt-MgO double-layered perpendicular magnetic recording media has been investigated by magnetic force microscope (MFM) technique, equipped with an in situ heating system up to 200°C. Within the measurement time scale (˜6h), there is no observable degradation in 50- and 100-kfci bits even at 200°C indicating good thermal stability of FePt media, while in 10-kfci bits some reversed domains are found at high temperatures in the center region of the bits due to the presence of strong demagnetizing field. The average MFM signal extracted from MFM images at high temperature is interpreted based on the temperature-dependent magnetic anisotropy (Ku) behavior of the FePt media.

  7. 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

  8. 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

  9. 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.

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

    DOE PAGESBeta

    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 anmore » alternative way to produce germanium epitaxy at reduced temperatures, a key enabler for increased flexibility of integration with CMOS back-end-of-line fabrication.« less

  11. 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.

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

    NASA Astrophysics Data System (ADS)

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

    2015-12-01

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

  13. 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. PMID:22797422

  14. In situ measurement of magnesium carbonate formation from CO2 using static high-pressure and -temperature 13C NMR.

    PubMed

    Surface, J Andrew; Skemer, Philip; Hayes, Sophia E; Conradi, Mark S

    2013-01-01

    We explore a new in situ NMR spectroscopy method that possesses the ability to monitor the chemical evolution of supercritical CO(2) in relevant conditions for geological CO(2) sequestration. As a model, we use the fast reaction of the mineral brucite, Mg(OH)(2), with supercritical CO(2) (88 bar) in aqueous conditions at 80 °C. The in situ conversion of CO(2) into metastable and stable carbonates is observed throughout the reaction. After more than 58 h of reaction, the sample was depressurized and analyzed using in situ Raman spectroscopy, where the laser was focused on the undisturbed products through the glass reaction tube. Postreaction, ex situ analysis was performed on the extracted and dried products using Raman spectroscopy, powder X-ray diffraction, and magic-angle spinning (1)H-decoupled (13)C NMR. These separate methods of analysis confirmed a spatial dependence of products, possibly caused by a gradient of reactant availability, pH, and/or a reaction mechanism that involves first forming hydroxy-hydrated (basic, hydrated) carbonates that convert to the end-product, anhydrous magnesite. This carbonation reaction illustrates the importance of static (unmixed) reaction systems at sequestration-like conditions. PMID:22676479

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

    PubMed

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

    2016-06-01

    A major challenge in lubrication technology is to enhance lubricant performance at extreme temperatures that exceed conventional engine oil thermal degradation limits. Soft noble metals such as silver have low reactivity and shear strength, which make them ideal solid lubricants for wear protection and friction reduction between contacting surfaces at high temperatures. However, achieving adequate dispersion in engine lubricants and metallic silver deposition over predetermined temperatures ranges presents a significant chemical challenge. Here we report the synthesis, characterization, and tribological implementation of the trimeric silver pyrazolate complex, [Ag(3,5-dimethyl-4-n-hexyl-pyrazolate)]3 (1). This complex is oil-soluble and undergoes clean thermolysis at ∼310 °C to deposit lubricious, protective metallic silver particles on metal/metal oxide surfaces. Temperature-controlled tribometer tests show that greater than 1 wt % loading of 1 reduces wear by 60% in PAO4, a poly-α-olefin lubricant base fluid, and by 70% in a commercial fully formulated 15W40 motor oil (FF oil). This silver-organic complex also imparts sufficient friction reduction so that the tribological transition from oil as the primary lubricant through its thermal degradation, to 1 as the primary lubricant, is experimentally undetectable. PMID:27163783

  16. An in situ neutron diffraction study of cation disordering in synthetic quandilite Mg{sub 2}tiO{sub 4} at high temperatures.

    SciTech Connect

    O'Neill, H. St. C.; Redfern, S. A. T.; Kesson, S.; Short, S.; Australian National Univ.; Univ. Cambridge

    2003-05-01

    Temperature-dependent cation order-disorder has been studied in many 2+ - 3+ oxide spinels but 4+ - 2+ spinels have been found to be either completely normal or completely inverse when examined at room temperature. Here we report the temperature dependence of the cation distribution in the 4-2 spinel synthetic qandilite (Mg{sub 2}TiO{sub 4}) from in situ time-of-flight neutron powder diffraction experiments to 1416 {sup o}C. At room temperature, Mg{sub 2}TiO{sub 4} is confirmed to have completely inverse cation distribution, with Ti atoms occupying half the octahedrally coordinated cation sites. Cation disordering becomes observable above about 900 {sup o}C, with 4% of the Ti occupying the tetrahedral site by 1416 {sup o}C. The rate of reordering on cooling is fast, such that high-temperature disorder is not preserved on cooling to room temperature. The thermodynamics of the change in cation distribution with temperature can be described by an enthalpy of Mg-Ti disorder of -46.1 {+-} 0.4 kJ/mol.

  17. Crystalline phase transition information induced by high temperature susceptibility transformations in bulk PMP-YBCO superconductor growth in-situ

    NASA Astrophysics Data System (ADS)

    Zhang, C. P.; Chaud, X.; Beaugnon, E.; Zhou, L.

    2015-01-01

    The dynamic susceptibility transformations of bulk HTSC PMP-YBCO growth have been investigated from 200 °C up to 1060 °C by the Faraday Balance in-situ. It revealed that the crystalline phase transitions of bulk PMP-YBCO growth in process. A new discovery of Y123 phase pre-formed then melted in heating stage has been found. It also discovered that Y123 crystal solidification started at 1004 °C in cooling stage. Before Y123 solidification the liquid phase CuO change to Cu2O reciprocally as well as the copper ion valence changed between divalent Cu2+ and trivalent Cu1+ each other. It was essential to keep quantities of CuO phase instead of the Cu2O for Y123 crystal solidification.

  18. Seasonal warming of Narragansett Bay and Rhode Island Sound in 1997: Advanced very high resolution radiometer sea surface temperature and in situ measurements

    NASA Astrophysics Data System (ADS)

    Fox, Mary Frances; Kester, Dana R.; Andrews, James E.; Magnuson, Andrea; Zoski, Cynthia G.

    2000-09-01

    The warming of Narragansett Bay and the offshore waters of Rhode Island Sound (RIS) and Buzzards Bay in the spring and early summer of 1997 was studied using in situ time series data and remotely sensed advanced very high resolution radiometer sea surface temperature (SST) satellite images. High-resolution SST images of the New England area were expanded to highlight Narragansett Bay and RIS. To validate this procedure, the remotely sensed data were compared to in situ data at the NOAA buoy in Buzzards Bay and at a spar buoy in mid-Narragansett Bay. The standard error (1.3°C) observed at the buoy in Narragansett Bay was slightly higher than that observed at the buoy in Buzzards Bay (1.0°C). A transect line down Narragansett Bay and into RIS and another across the entrance of Narragansett Bay and Buzzards Bay were extracted from the 47 images. A thermal front was observed at the mouth of the bay with the bay being warmer in the summer and cooler in the winter than the sound. Two areas of cold water were identified in the RIS transect: a cold water plume at the tip of Long Island and a second area near the Elizabeth Islands. We believe that both were caused by vertical mixing. There were three sources of in situ time series data to compare with the SST: (1) a spar buoy with sensors in the surface and bottom waters located near the middle of the Bay, (2) observations from a shore site near the mouth of the Bay, and (3) a National Oceanic and Atmospheric Administration buoy at the mouth of Buzzards Bay. Using the spar buoy data, we were able to calculate the vertical density gradient, and we found that salinity was more important than temperature in controlling the density structure at this site. Time series temperature data from the surface water in Buzzards Bay were almost identical to those observed in the bottom waters of Narragansett Bay, indicating that bottom water in the bay originates as surface water in RIS. Using a cooling event in the surface waters at

  19. 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.

  20. 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. PMID:25769690

  1. Dislocation generation related to micro-cracks in Si wafers: High temperature in situ study with white beam X-ray topography

    NASA Astrophysics Data System (ADS)

    Danilewsky, A.; Wittge, J.; Hess, A.; Cröll, A.; Allen, D.; McNally, P.; Vagovič, P.; Cecilia, A.; Li, Z.; Baumbach, T.; Gorostegui-Colinas, E.; Elizalde, M. R.

    2010-02-01

    The generation and propagation of dislocations in Si at high temperature is observed in situ with white beam X-ray topography. For the heating experiments a double ellipsoidal mirror furnace was installed at the Topo-Tomo beamline of the ANKA synchrotron light source, Research Centre Karlsruhe, Germany. Details of the experimental set-up and the first results on the occurrence of dislocations are presented. Artificial damage was generated in commercial (1 0 0) Si wafers using a nanoindenter with various loads. The applied forces for each set of indents were varied from 100 to 500 mN, respectively. After heating to approx. 790 °C large area transmission topographs were taken every 30 min which were then compared to room temperature topographs before and after heating. At the outset straight 60°-dislocations with b = a/2<1 1 0> originate from the 500 mN indents into the direction of the strongest temperature gradient. After 60 min at constant temperature an increase in the length and number of the dislocations in other directions is also observed. As a result of the continual thermal stressing dislocations develop from the 100 mN indents too.

  2. 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.

  3. In Situ Temperature Jump Dynamic Nuclear Polarization

    PubMed Central

    Joo, Chan-Gyu; Casey, Andrew; Turner, Christopher J.; Griffin, Robert G.

    2009-01-01

    Dynamic nuclear polarization is combined with temperature jump methods to develop a new 2D 13C- 13C NMR experiment that yields a factor or 100-170 increase insensitivity. The polaization step is performed at ∼100 K and the sample is subsequently melted with a 10.6 mm laser pulse to yield a sample with highly polarized 13C spins. 13C detected 2D 13C- 13C spectroscopy is performed in the usual manner. PMID:18942782

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

    SciTech Connect

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

    2014-08-15

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

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

    PubMed

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

    2014-08-01

    A compact ultrahigh temperature tensile testing instrument has been designed and fabricated for in situ x-ray micro-tomography using synchrotron radiation at the Advanced Light Source, Lawrence Berkeley National Laboratory. It allows for real time x-ray micro-tomographic imaging of test materials under mechanical load at temperatures up to 2300 °C in controlled environments (vacuum or controlled gas flow). Sample heating is by six infrared halogen lamps with ellipsoidal reflectors arranged in a confocal configuration, which generates an approximately spherical zone of high heat flux approximately 5 mm in diameter. Samples are held between grips connected to a motorized stage that loads the samples in tension or compression with forces up to 2.2 kN. The heating chamber and loading system are water-cooled for thermal stability. The entire instrument is mounted on a rotation stage that allows stepwise recording of radiographs over an angular range of 180°. A thin circumferential (360°) aluminum window in the wall of the heating chamber allows the x-rays to pass through the chamber and the sample over the full angular range. The performance of the instrument has been demonstrated by characterizing the evolution of 3D damage mechanisms in ceramic composite materials under tensile loading at 1750 °C. PMID:25173271

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

    NASA Astrophysics Data System (ADS)

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

    2014-08-01

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

  7. 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. PMID:26267394

  8. Temperature dependence of Jc for in situ superconductors

    SciTech Connect

    Ostenson, J.E.; Finnemore, D.K.; Gibson, E.D.; Sue, J.J.; Verhoeven, J.D.

    1982-01-01

    The experiments reported in this study seek to define the temperature dependence of the critical current densities for in situ superconducting wire in order to be able to predict the response of magnets when they are treated to temperature excursions well above 4.2 K. Studies of flux pinning in Nb/sub 3/Sn in situ filaments have determined that core pinning at grain boundary surface locations is the dominant factor controlling the critical current density. On the premise that proximity coupling may become a more important factor in the loss of critical current densities at high temperatures than a grain boundary breakdown, and to test whether the breakdown of the proximity effect degrades those densities, samples were chosen in which the proximity effect would show most readily, that is, those samples which have, owing to coarsening, rather short filaments. The samples were prepared from a dendritic Cu-Nb alloy that contained 20 wt% Nb, wound on a 1.27 cm diameter mandrel, and tested. It was found that the critical current density drops by 10% per degree K increase.

  9. 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.

  10. 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

    2014-01-01

    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. PMID:24889679

  11. 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

  12. 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.

  13. A large-volume high-pressure and high-temperature apparatus for in situ X-ray observation, ' SPEED-Mk.II'

    NASA Astrophysics Data System (ADS)

    Katsura, Tomoo; Funakoshi, Ken-ichi; Kubo, Atsushi; Nishiyama, Norimasa; Tange, Yoshinori; Sueda, Yu-ichiro; Kubo, Tomoaki; Utsumi, Wataru

    2004-06-01

    SPEED-Mk.II, the second KAWAI-type high P- T apparatus for in situ X-ray observation that was installed at the bending magnet beam line at SPring-8, is described. The guide block system was designed so that the change of the relative dimension of the cubic compression space with press load can be minimized by repeated adjustments. The hydraulic system was designed so as to enable smooth compression and decompression. These precise controls should be advantageous for high-pressure generation, especially when sintered diamond (SD) anvils are used. An oscillation system was equipped for the first time in a large volume press, making it possible to obtain high-quality diffraction patterns even when the number of sample grains is limited. The use of the oscillation system also reduces errors in pressure determination that may be caused by insufficient averaging of diffraction angles over grains in a limited diffraction volume, because the oscillating grains should sweep through the 2 θ range that is allowed by the finite widths of the optical slits.

  14. 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. PMID:26039687

  15. 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

  16. In Situ Measurement of the γ/ γ' Lattice Mismatch Evolution of a Nickel-Based Single-Crystal Superalloy During Non-isothermal Very High-Temperature Creep Experiments

    NASA Astrophysics Data System (ADS)

    Le Graverend, Jean-Briac; Dirand, Laura; Jacques, Alain; Cormier, Jonathan; Ferry, Olivier; Schenk, Thomas; Gallerneau, Franck; Kruch, Serge; Mendez, José

    2012-11-01

    The evolution of the γ/ γ' lattice mismatch of the AM1 single-crystal superalloy was measured during in situ non-isothermal very high-temperature creep tests under X-ray synchrotron radiation. The magnitude of the effective lattice mismatch in the 1273 K to 1323 K (1000 °C to 1050 °C) temperature range always increased after overheatings performed at temperatures lower than 1403 K (1130 °C). In contrast, a decrease of its magnitude was observed after overheatings at temperatures greater than 1453 K (1180 °C) due to massive dislocation recovery processes occurring at very high temperature.

  17. 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

  18. 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. PMID:22404902

  19. 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.

  20. 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).

  1. An in situ synchrotron energy-dispersive diffraction study of the hydration of oilwell cement systems under high temperature/autoclave conditions up to 130 deg. C

    SciTech Connect

    Colston, Sally L.; Barnes, Paul . E-mail: p.barnes@bbk.ac.uk; Jupe, Andrew C.; Jacques, Simon D.M.; Hall, Christopher; Livesey, Paul; Dransfield, John; Meller, Nicola; Maitland, Geoffrey C.

    2005-12-15

    The technique of synchrotron energy dispersive diffraction has been developed for in situ studies of cement hydration under autoclave conditions. This has been applied to oilwell cements hydrating at typical oilwell temperatures up to 130 deg. C. The results show clearly the detailed interplay between 11 detectable phases, from which a phase transformation scheme has been derived; this illustrates the progression of hydration up to 130 deg. C for two extreme cases, with and without conservation of water content and autoclave pressure. The monosulphate hydrate phases are found to exhibit different stability bounds, with a surprising sequence of the 14-water, 10-water then 12-water monosulphate as temperature/time increases; the latter form is particularly associated with conditions of water/pressure loss. The effect of retarders on C{sub 3}S dissolution and CH formation is negligible above 70 deg. C, whereas the effect on the calcium sulphoaluminate hydrates is more complex, and possible reasons for this are discussed.

  2. 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.

  3. 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.

  4. 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.

  5. High Throughput In Situ XAFS Screening of Catalysts

    SciTech Connect

    Tsapatsaris, Nikolaos; Beesley, Angela M.; Weiher, Norbert; Tatton, Helen; Schroeder, Sven L. M.; Dent, Andy J.; Mosselmans, Frederick J. W.; Tromp, Moniek; Russu, Sergio; Evans, John; Harvey, Ian; Hayama, Shu

    2007-02-02

    We outline and demonstrate the feasibility of high-throughput (HT) in situ XAFS for synchrotron radiation studies. An XAS data acquisition and control system for the analysis of dynamic materials libraries under control of temperature and gaseous environments has been developed. The system is compatible with the 96-well industry standard and coupled to multi-stream quadrupole mass spectrometry (QMS) analysis of reactor effluents. An automated analytical workflow generates data quickly compared to traditional individual spectrum acquisition and analyses them in quasi-real time using an HT data analysis tool based on IFFEFIT. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on {gamma}-Al2O3, and for the in situ characterization of Au catalysts supported on Al2O3 and TiO2.

  6. High Throughput In Situ XAFS Screening of Catalysts

    NASA Astrophysics Data System (ADS)

    Tsapatsaris, Nikolaos; Beesley, Angela M.; Weiher, Norbert; Tatton, Helen; Dent, Andy J.; Mosselmans, Frederick J. W.; Tromp, Moniek; Russu, Sergio; Evans, John; Harvey, Ian; Hayama, Shu; Schroeder, Sven L. M.

    2007-02-01

    We outline and demonstrate the feasibility of high-throughput (HT) in situ XAFS for synchrotron radiation studies. An XAS data acquisition and control system for the analysis of dynamic materials libraries under control of temperature and gaseous environments has been developed. The system is compatible with the 96-well industry standard and coupled to multi-stream quadrupole mass spectrometry (QMS) analysis of reactor effluents. An automated analytical workflow generates data quickly compared to traditional individual spectrum acquisition and analyses them in quasi-real time using an HT data analysis tool based on IFFEFIT. The system was used for the automated characterization of a library of 91 catalyst precursors containing ternary combinations of Cu, Pt, and Au on γ-Al2O3, and for the in situ characterization of Au catalysts supported on Al2O3 and TiO2.

  7. 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

  8. High-resolution in-situ thermal imaging of microbial mats at El Tatio Geyser, Chile shows coupling between community color and temperature

    NASA Astrophysics Data System (ADS)

    Dunckel, Anne E.; Cardenas, M. Bayani; Sawyer, Audrey H.; Bennett, Philip C.

    2009-12-01

    Microbial mats have spatially heterogeneous structured communities that manifest visually through vibrant color zonation often associated with environmental gradients. We report the first use of high-resolution thermal infrared imaging to map temperature at four hot springs within the El Tatio Geyser Field, Chile. Thermal images with millimeter resolution show drastic variability and pronounced patterning in temperature, with changes on the order of 30°C within a square decimeter. Paired temperature and visual images show that zones with specific coloration occur within distinct temperature ranges. Unlike previous studies where maximum, minimum, and optimal temperatures for microorganisms are based on isothermally-controlled laboratory cultures, thermal imaging allows for mapping thousands of temperature values in a natural setting. This allows for efficiently constraining natural temperature bounds for visually distinct mat zones. This approach expands current understanding of thermophilic microbial communities and opens doors for detailed analysis of biophysical controls on microbial ecology.

  9. 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.

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

    SciTech Connect

    Yang Jie; Li Ming; Zhang Honglin; Gao Chunxiao

    2011-04-15

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

  11. 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.

  12. 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.

  13. 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

    2016-01-01

    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

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. In situ high-frequency observations of mycorrhizas.

    PubMed

    Allen, Michael F; Kitajima, Kuni

    2013-10-01

    Understanding the temporal variation of soil and root dynamics is a major step towards determining net carbon in ecosystems. We describe the installation and structure of an in situ soil observatory and sensing network consisting of an automated minirhizotron with associated soil and atmospheric sensors. Ectomycorrhizal hyphae were digitized daily during 2011 in a Mediterranean climate, high-elevation coniferous forest. Hyphal length was high, but stable during winter in moist and cold soil. As soil began to warm and dry, simultaneous mortality and production indicating turnover followed precipitation events. Mortality continued through the dry season, although some hyphae persisted through the extremes. With autumn monsoons, rapid hyphal re-growth occurred following each event. Relative hyphal length is dependent upon soil temperature and moisture. Soil respiration is related to the daily change in hyphal production, but not hyphal mortality. Continuous sensor and observation systems can provide more accurate assessments of soil carbon dynamics. PMID:23772913

  19. Low-temperature in situ formation of Y-Ba-Cu-O high T sub c superconducting thin films by plasma-enhanced metalorganic chemical vapor deposition

    SciTech Connect

    Zhao, J.; Noh, D.W.; Chern, C.; Li, Y.Q.; Norris, P.; Gallois, B.; Kear, B. )

    1990-06-04

    Highly textured, highly dense, superconducting YBa{sub 2}Cu{sub 3}O{sub 7{minus}{ital x}} thin films with mirror-like surfaces have been prepared, {ital in} {ital situ}, at a reduced substrate temperature as low as 570 {degree}C by a remote microwave plasma-enhanced metalorganic chemical vapor deposition process (PE-MOCVD). Nitrous oxide was used as the oxidizer gas. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K. PE-MOCVD was carried out in a commercial scale MOCVD reactor.

  20. In-situ Raman spectroscopic study of aluminate speciation in H2O-KOH solutions at high pressures and temperatures

    NASA Astrophysics Data System (ADS)

    Mookherjee, M.; Keppler, H.; Manning, C. E.

    2009-12-01

    The solubility of corundum in H2O is low even at high pressure and temperatures. Therefore, it is commonly assumed that alumina remains essentially immobile during fluid-rock interaction. However, field and experimental evidence suggests that alumina solubility is strongly enhanced in the presence of silica as well as in alkaline solutions. In order to understand what controls the alumina solubility and how it is enhanced as a function of fluid composition, we conducted Raman-spectroscopic study of Al speciation in aqueous fluids at high pressure and temperature. Experiments were carried out in an externally heated hydrothermal diamond-anvil cell equipped with low-fluorescence diamonds and iridium gaskets. Raman spectra were collected with a Horiba Jobin-Yvon Labram HR spectrometer using the 514 nm line of an argon laser for excitation. In a first series of experiments, the speciation of alumina was studied in a 1 M KOH solution in equilibrium with corundum up to 700 oC and ~1 GPa. The Raman spectra show a prominent band at 618 cm-1 interpreted to arise from Al-O stretching vibrations associated with the tetrahedral [Al(OH)4]1- species. At higher pressure and temperature, an additional vibrational mode appears in the spectra at 374 cm-1 (full width at half maximum ~ 20 cm-1). This feature is tentatively attributed to [(OH)3Al-O-Al(OH)3]2- (Moolenaar et al. 1970, Jour. Phys. Chem., 74, 3629-3636). No evidence for KAl(OH)4 was observed, consistent with piston cylinder experiments at 700 oC and 1 GPa (Wohlers & Manning, 2009, Chem. Geol., 262, 310). Upon cooling from high-pressure and high temperature, slow kinetics of corundum regrowth lead to oversaturation in the solutions, as evidenced by sharp peaks at 930 and 1066 cm-1 observed upon cooling. These features are probably due to colloidal aluminum hydroxide. The results provide the first evidence for aluminate polymerization at high pressure and temperature, and offer insights into the causes for enhancement of

  1. 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

  2. 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.

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

    SciTech Connect

    Yoo, C.S.

    1997-12-01

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

  4. In-Situ Measurement of Metal Drop Temperature in GMA Short-Circuiting Welding

    NASA Astrophysics Data System (ADS)

    Hirata, Yoshinori; Onda, Masahiko; Nagaki, Hayato; Ohji, Takayoshi

    Temperatures of metal drop in GMA short-circuiting welding process were in-situ measured using newly developed instrument designed on the basis of two-color pyrometry, which consisted of optical lenses, interference filters for two colors and two sets of high sensitive CCD cameras with fast shutter. In order to avoid radiation from arc plasma, temperature measurement was carried out immediately after molten drop at electrode wire tip was contacted with weld pool and arc was extinguished. Welding current in arcing period was adjusted from 50 A to 250 A using experimental power source in Ar + 20%CO2 mixture gas shielded GMA welding with mild steel wire of 1.2 mm in diameter. It is shown through in-situ measurement that average temperature of metal drop ranges from 2200 K to 2700 K, depending on level and period of arc current governing electrode wire melting.

  5. 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

  6. 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

    2015-01-01

    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

  7. 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.

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

    NASA Astrophysics Data System (ADS)

    Yamamoto, Kazuhiro; Qiu, Nan; Ohara, Satoshi

    2015-11-01

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

  9. 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.

  10. 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.

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

    PubMed Central

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

    2011-01-01

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

  12. 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. PMID:22163735

  13. 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.

  14. Structural behavior of Al 3+ in silicate melts: In situ, high-temperature measurements as a function of bulk chemical composition

    NASA Astrophysics Data System (ADS)

    Mysen, Bjorn

    1995-02-01

    The anionic structure of aluminosilicate melts has been determined along the join Li 2Si 2O 5Li 2(LiAl) 2O 5 (LS2-LA2) with microRaman spectroscopy in the temperature range 25°-1460°C. Those data are compared with the structural behavior of melts along the join Na 2Si 2O 5Na 2(NaAl) 2O 5 (NS2-NA2) in the same temperature interval. In these systems, Li' and Na + serve both to charge-balance Al 3+ in tetrahedral coordination and as network-modifiers. The NBO/ T ( T = Si + Al) equals unity in the Al/(Al + Si) range examined (0-0.3). In the Al-free endmember glass and melt systems, the three species, Q4, Q3, and Q2 coexist and the expression, (1) 2 Q3 ⇔ Q2 + Q4, describes the equilibrium. Substitution of Na- or Li-charge-balanced Al 3+ for Si 4+ results in stabilization of an additional, more depolymerized structural unit, Q1. An additional equilibrium, (2) 2 Q2 ⇔ Q1 + Q3, is needed, therefore, for a complete description of the equilibria. In the LS2-LA2 system, the ΔH for this latter reaction ( ΔH2) ranges between ˜0 and -87 kJ/mol and is negatively correlated with Al/(Al + Si). In the NS2-NA2 system, the ΔH2 is positive with values between 16 and 37 kJ/mol and is positively correlated with Al/(Al + Si). Equilibrium (1) is affected by equilibrium (2) in the Al-bearing melts, so that in the NS2-NA2 melt system, equilibrium (1) shifts to the left with temperature ( ΔH1 = -10--15 kJ/mol), whereas in the LS2-LA2 system, equilibrium (1) shifts more strongly to the right with temperature than in the absence of Al ( ΔH1 is positively correlated with Al/(Al + Si) with values in the range 6-48 kJ/mol). Activity coefficients for Q2 units in the melts calculated from liquidus phase relations in combination with the determined mol fractions of structural units in the melts show simple relations between activity coefficient of the unit and its molar abundance in the melts.

  15. 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. PMID:26202895

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

    DOE PAGESBeta

    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 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

  17. 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.

  18. 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...

  19. Calcium pyroxenes at Mercurian surface temperatures: investigation of in-situ emissivity spectra and thermal expansion

    NASA Astrophysics Data System (ADS)

    Ferrari, S.; Nestola, F.; Helbert, J.; Maturilli, A.; D'Amore, M.; Alvaro, M.; Domeneghetti, M.; Massironi, M.; Hiesinger, H.

    2013-12-01

    The European Space Agency and Japan Aerospace Agency mission to Mercury, named BepiColombo, will carry on board the Mercury Radiometer and Thermal Infrared Spectrometer (MERTIS) that will be able to provide surface Thermal Infra-Red (TIR) emissivity spectra from 7 to 14 μm. This range of wavelengths is very useful to identify the fine-scale structural properties of several silicates. For mineral families as pyroxenes, the emissivity peak positions are good indicators of the composition. A complication in the interpretation of MERTIS data could arise from the extreme daily surface temperature range of Mercury (70 to 725 K) that significantly affects the crystal structure and density of minerals and consequently should affect the TIR spectral signature of each single mineral present on the surface of the planet. In preparation for the MERTIS data analysis, we are extensively investigating at high temperatures conditions several mineral phases potentially detectable on the surface of Mercury. Two C2/c augitic pyroxenes, with constant calcium content and very different magnesium to iron ratio, were studied by in situ high-temperature thermal infrared spectroscopy (up to 750 K) and in situ high-temperature single-crystal X-ray diffraction (up to 770 K). The emissivity spectra of the two samples show similar band center shifts of the main three bands toward lower wavenumbers with increasing temperature. Our results indicate that the center position of bands 1 and 2 is strictly dependent on temperature, whereas the center position of band 3 is a strong function of the composition regardless the temperature. These data suggest that MERTIS spectra will be able to provide indications of C2/c augitic pyroxene with different magnesium contents and will allow a correct interpretation independently on the spectra acquisition temperature.

  20. In situ study of the fractionation of hydrogen isotopes between aluminosilicate melts and coexisting aqueous fluids at high pressure and high temperature - Implications for the δD in magmatic processes

    NASA Astrophysics Data System (ADS)

    Dalou, Célia; Le Losq, Charles; Mysen, Bjorn O.

    2015-09-01

    The hydrogen isotopic composition of melt inclusions trapped in phenocrysts during their crystallization and growth in a magma may contribute to a better understanding of the water cycle between the atmosphere, the hydrosphere and the lithosphere. Such understanding relies on the knowledge of the hydrogen isotopic fractionation factors between aqueous fluids, silicate melts, and minerals at temperature and pressure conditions relevant to the Earth's interior. Significant D/H fractionation between silicate melts and aqueous fluids was reported at hundreds of MPa and °C by using in situ measurements in hydrothermal diamond anvil cell (HDAC) experiments (Mysen, 2013a, 2013b, Am. Mineral. 98, 376-386 and 1754-1764). However, the available dataset is focused on fluids and melts with D/H ratios close to unity. The relevance of such data for natural processes that involve per mil variations of δD-values may not always be clear. To address such concerns, the effect of the bulk D/H ratio on hydrogen isotope partitioning between water-saturated silicate melts and coexisting silicate-saturated aqueous fluids has been determined in the Na2O-Al2O3-SiO2-H2O-D2O system. To this end, in situ Raman spectroscopic measurements were performed on fluids and melts with bulk D/H ratios from 0.05 to 2.67 by using an externally-heated diamond anvil cell in the 300-800 °C and 200-1500 MPa temperature and pressure range, respectively. In these pressure/temperature ranges, the D/H ratios of fluids in equilibrium with melt barely change with temperature (in average ΔHfluid = 0.47 ± 1.15 kJ /mol). In contrast, the D/H ratios of coexisting melts display strong dependence on temperature (average ΔHmelt = 7.18 ± 1.27 kJ /mol). The temperature-dependence of the D/H fractionation factor between melt and fluid (αfluid-melt = D /Hfluid / D /Hmelt) is comparable in all the experiments and can be written: 1000 ṡ ln ⁡ (αfluid-melt) = 263 (± 26) ṡT-2- 126 (± 48). Therefore, the

  1. 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.

  2. In situ X-ray diffraction study of structural evaluation in Fe73Cu1.5Nd3Si13.5B9 amorphous alloy at high temperature

    NASA Astrophysics Data System (ADS)

    Li, Gong; Xu, Tao; Gao, Yunpeng; Liu, Riping

    2008-04-01

    The thermodynamics structural relaxation of Fe73Cu1.5Nd3Si13.5B9 amorphous alloy from room temperature to 400°C has been investigated by measuring the structure factor with in situ X-ray diffraction. The structural information of the atomic configuration such as radial distribution function (RDF) and neighbor atomic distance was gained by Fourier transformation. The research result shows that the amorphous structure remains stable in the temperature range of 30 to 400°C but exhibits distinct changes in local atomic configuration with the increase of temperature. The quantitative determination of the neighbor atomic distance suggests that the degree of short-range order changes by the temperature altering the second nearest neighbor local atomic configuration of the amorphous when structural relaxation occurs.

  3. In situ thermal imaging and absolute temperature monitoring by luminescent diphenylalanine nanotubes.

    PubMed

    Gan, Zhixing; Wu, Xinglong; Zhang, Jinlei; Zhu, Xiaobin; Chu, Paul K

    2013-06-10

    The temperature sensing capability of diphenylalanine nanotubes is investigated. The materials can detect local rapid temperature changes and measure the absolute temperature in situ with a precision of 1 °C by monitoring the temperature-dependent photoluminescence (PL) intensity and lifetime, respectively. The PL lifetime is independent of ion concentrations in the medium as well as pH in the physiological range. This biocompatible thermal sensing platform has immense potential in the in situ mapping of microenvironmental temperature fluctuations in biological systems for disease diagnosis and therapeutics. PMID:23679829

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

    NASA Astrophysics Data System (ADS)

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

    2013-12-01

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

  5. 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. PMID:26429448

  6. 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.

  7. 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.

  8. 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

  9. Temperature-dependent properties of silver-poly(methylmethacrylate) nanocomposites synthesized by in-situ technique

    PubMed Central

    2014-01-01

    Ag/PMMA nanocomposites were successfully synthesized by in-situ technique. Transmission electron microscopy (TEM) images show that the particles are spherical in shape and their sizes are dependent on temperature. The smallest particle achieved high stability as indicated from Zeta sizer analysis. The red shift of surface plasmon resonance (SPR) indicated the increases of particle sizes. X-ray diffraction (XRD) patterns exhibit a two-phase (crystalline and amorphous) structure of Ag/PMMA nanocomposites. The complexation of Ag/PMMA nanocomposites was confirmed using Raman spectroscopy. Fourier transform infrared spectroscopy spectra confirmed that the bonding was dominantly influenced by the PMMA and DMF solution. Finally, thermogravimetric analysis (TGA) results indicate that the total weight loss increases as the temperature increases. PMID:24450850

  10. Low-Temperature in Situ Growth of Graphene on Metallic Substrates and Its Application in Anticorrosion.

    PubMed

    Zhu, Minmin; Du, Zehui; Yin, Zongyou; Zhou, Wenwen; Liu, Zhengdong; Tsang, Siu Hon; Teo, Edwin Hang Tong

    2016-01-13

    Metal or alloy corrosion brings about huge economic cost annually, which is becoming one area of growing concern in various industries, being in bulk state or nanoscale range. Here, single layer or few layers of graphene are deposited on various metallic substrates directly at a low temperature down to 400 °C. These substrates can be varied from hundreds-micrometer bulk metallic or alloy foils to tens of nanometer nanofibers (NFs). Corrosion analysis reveals that both graphene-grown steel sheets and NFs have reduced the corrosion rate of up to ten times lower than that of their bare corresponding counterparts. Moreover, such low-temperature in situ growth of graphene demonstrates stable and long-lasting anticorrosion after long-term immersion. This new class of graphene coated nanomaterials shows high potentials in anticorrosion applications for submarines, oil tankers/pipelines, and ruggedized electronics. PMID:26683895

  11. Simple and compact optode for real-time in-situ temperature detection in very small samples

    PubMed Central

    Long, Feng; Shi, Hanchang

    2014-01-01

    Real-time in-situ temperature detection is essential in many applications. In this paper, a simple and robust optode, which uses Ruthenium (II) complex as a temperature indicator, has been developed for rapid and sensitive temperature detection in small volume samples (<5 μL). Transmission of excitation light and collection and transmission of fluorescence are performed by a homemade single-multi mode fiber coupler, which provides the entire system with a simple and robust structure. The photoluminescence intensity of Ruthenium (II) complex diminishes monotonically from 0°C to 80°C, and the response to temperature is rapid and completely reversible. When temperature is less than (or higher than) 50°C, a linear correlation exists between the fluorescence intensity and the temperature. Excellent agreement was also observed between the continuous and in situ measurements obtained by the presented optode and the discrete temperature values measured by a conventional thermometer. The proposed optode has high sensitivity, high photostability and chemical stability, a wide detection range, and thermal reversibility, and can be applied to real-time in-situ temperature detection of a very small volume biological, environmental, and chemical sample. PMID:24875420

  12. Simple and compact optode for real-time in-situ temperature detection in very small samples

    NASA Astrophysics Data System (ADS)

    Long, Feng; Shi, Hanchang

    2014-05-01

    Real-time in-situ temperature detection is essential in many applications. In this paper, a simple and robust optode, which uses Ruthenium (II) complex as a temperature indicator, has been developed for rapid and sensitive temperature detection in small volume samples (<5 μL). Transmission of excitation light and collection and transmission of fluorescence are performed by a homemade single-multi mode fiber coupler, which provides the entire system with a simple and robust structure. The photoluminescence intensity of Ruthenium (II) complex diminishes monotonically from 0°C to 80°C, and the response to temperature is rapid and completely reversible. When temperature is less than (or higher than) 50°C, a linear correlation exists between the fluorescence intensity and the temperature. Excellent agreement was also observed between the continuous and in situ measurements obtained by the presented optode and the discrete temperature values measured by a conventional thermometer. The proposed optode has high sensitivity, high photostability and chemical stability, a wide detection range, and thermal reversibility, and can be applied to real-time in-situ temperature detection of a very small volume biological, environmental, and chemical sample.

  13. 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

  14. 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.

  15. 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.

  16. 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.

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

    PubMed

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

    2012-07-21

    Aqueous solutions that undergo sol-to-gel transition as the temperature increases have been extensively studied during the last decade. The material can be designed by controlling the hydrophilic and hydrophobic balance of the material. Basically, the molecular weight of the hydrophilic block and hydrophobic block of a compound should be fine-tuned from the synthetic point of view. In addition, stereochemistry, microsequence, topology, and nanostructures of the compound also affect the transition temperature, gel window, phase diagram, and modulus of the gel. From a practical point of view, biodegradability, biocompatibility, and interactions between the material and drug or cell should be considered in designing a thermogelling material. The interactions are particularly important in that they control drug release profile and initial burst release of the drug in the drug delivery system, and affect cell proliferation, differentiation, and biomarker expression in three-dimensional cell culture and tissue engineering application. This review provides an in-depth summary of the recent progress of thermogelling systems including polymers, low molecular compounds, and nanoemulsions. Their biomedical applications were also comparatively discussed. In addition, perspectives on future material design of a new thermogelling material and its application are suggested. PMID:22688789

  18. 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

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

    DOE PAGESBeta

    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 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

  20. 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.

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

    PubMed Central

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

    2015-01-01

    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. 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. PMID:26639147

  2. A new method for in situ electron temperature determinations from plasma wave phenomena

    NASA Technical Reports Server (NTRS)

    Oya, H.; Benson, R. F.

    1972-01-01

    A discrepancy has been reported between the values of the electron temperature t sub e deduced from satellite electrostatic probe measurements and ground based radar backscatter measurements. This discrepancy (radar backscatter temperature less than the probe temperature) is not present when the probe experiment is flown on a rocket to lower altitudes but reappears when the rocket probe attains higher altitudes. There is a need for an independent radio wave method for making in-situ t sub e measurements in order to help resolve this problem. A new method of determining t sub e from the satellite resonant phenomena is presented. It is based on the splitting (observed at high latitudes) of the diffuse resonance which occurs at the frequency f sub d1 between f sub h and 2 f sub h. The advantage of this method over the other methods involving ionospheric resonances is the simplicity of the required calculations. There is, however, the limitation of plasma conditions where the f sub d1 resonance can be observed and the limitation to mid-to-high latitudes where the splitting is observed.

  3. High material efficiency MOVPE growth with in situ monitoring

    NASA Astrophysics Data System (ADS)

    Onitsuka, R.; Sugiyama, M.; Nakano, Y.

    2010-04-01

    The possibility of growing a GaAs single-junction solar cell structure with high growth rate and low partial pressure of tertiary-butylarsine (TBAs) has been explored in order to minimize the cost and material consumption in metal-organic vapor phase epitaxy (MOVPE). In situ surface reflectance anisotropy measurements suggested that we can grow reasonable quality GaAs layers at a growth rate of 3.3 μm/h and a V/III ratio of 2.5. Dark current-voltage characteristics of the pn junction that was grown at this condition yielded an ideality factor of 1.3, which was equivalent to the value obtained with a lower growth rate and higher V/III ratio, suggesting a possibility that we can grow GaAs with reasonable crystal quality at a high material efficiency. However, there seemed to exist spots of accumulated defects with a spacing of hundreds of micrometers at such a growth condition with a high material efficiency. If they are situated in the vicinity of the pn junction, the efficiency of the PV cell was significantly degraded, which suggests the necessity of tuning the growth conditions according to the impact of a layer on the electrical properties of a PV cell.

  4. In Situ Contaminate Stabilization within a Complex and Highly Heterogeneous Fractured Media

    NASA Astrophysics Data System (ADS)

    Scott, C. L.; Heath, G. L.; Baker, K. E.; Schafer, A. L.

    2006-12-01

    Radionuclides that are adsorbed in vadose zone soils are a contamination source of subsurface waters on DOE sites. Source contamination typically was a localized leak in surface or near-surface process equipment. Immobilizing or sequestering such contaminants in situ is a preferred remediation technique for economic and technical reasons. In situ contaminate stabilization can be challenging when the subsurface geology is complex and highly heterogeneous. The contaminate stabilization is accomplished by introducing an amendment, water-soluble polymer, into contact with the contaminated porous medium. This paper will present results from a series of laboratory experiments preformed in layered heterogeneous tanks that were monitored using 4 D electrical resistivity, temperature, conductivity of incoming and outgoing tank fluids. The experiments were designed to show that monitoring as well as sequestering radionuclides (Sr90) in perched groundwater within fractured media was possible.

  5. 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

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

    NASA Astrophysics Data System (ADS)

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

    2015-08-01

    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 Al2O3 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 Al2O3 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.

  7. 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.

  8. 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.

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

    NASA Astrophysics Data System (ADS)

    Labovská, Veronika; Katunský, Dušan

    2016-06-01

    Historical building envelope is characterized by a large accumulation that impact is mainly by changing the inner surface temperature over time. The minimum value of the inner surface temperature is set Code requirements. In the case of thermal technology assessment of building envelope contemplates a steady state external temperature and internal environment, thereby neglecting the heat accumulation capacity of building envelopes. Monitoring surface temperature in real terms in situ shows the real behavior of the building envelope close to reality. The recorded data can be used to create a numerical model for the simulation.

  10. In-situ high-pressure transmission electron microscopy of minerals

    NASA Astrophysics Data System (ADS)

    Wu, J.; Buseck, P. R.

    2010-12-01

    We show that high-resolution studies are possible at high pressure and temperature within a transmission electron microscope (TEM). To achieve this goal, which avoids the crystallographic and chemical changes that can occur upon quenching, we use the unusual structural properties of carbon nanotubes (CNTs) and fullerenes. These carbon materials, which are used as sample containers, contract under radiation by energetic electrons at elevated temperatures in a TEM. The result is compression of materials that have been encapsulated within these containers. We estimated pressures greater than 20 GPa from the Fourier transforms of high-resolution images of oxide particles such as ZnO and Sm2O3 under compression within CNTs. Using an arc-discharge technique, we recently also loaded olivine into fullerenes. Such ability to compress and then examine minerals in situ at high resolution opens up new possibilities for the high-pressure research of minerals.

  11. Polarimetric fiber grating biosensor for in-situ high-sensitive intracellular density measurement

    NASA Astrophysics Data System (ADS)

    Guo, Tuan; Liu, Fu; Liu, Yu; Chen, Nan-Kuang; Guan, Bai-Ou; Albert, Jacques

    2014-05-01

    High sensitivity biological sample measurements have been achieved by using a 12o tilted fiber Bragg grating (TFBG). Human acute leukemia cells with different intracellular densities and refractive index (RI) ranging from 1.3342 to 1.3344 were clearly discriminated in-situ by using the differential transmission spectrum between two orthogonal polarizations for the last guided mode resonance before "cut-off", with an amplitude variation sensitivity of 1.8×104 dB/RIU and a limit of detection of 2×10-5 RIU. The technique is inherently temperature-insensitive.

  12. 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.

  13. 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

  14. In situ high-temperature high-pressure Raman spectroscopy on single-crystal relaxor ferroelectrics PbSc1/2Ta1/2O3 and PbSc1/2Nb1/2O3

    NASA Astrophysics Data System (ADS)

    Waeselmann, N.; Mihailova, B.; Gospodinov, M.; Bismayer, U.

    2013-04-01

    The effect of temperature on the pressure-induced structural changes in perovskite-type (ABO3) relaxor ferroelectrics is studied by in situ high-temperature high-pressure Raman spectroscopy on single crystals of PbSc1/2Ta1/2O3 (PST) and PbSc1/2Nb1/2O3 (PSN), which allowed us to elucidate the interplay between the polar and antiferrodistortive order coexisting on the mesoscopic scale at ambient conditions. High-pressure experiments were carried out at elevated temperatures below and above the characteristic intermediate temperature T*. The results were compared with those obtained at room temperature, which for PST is just above the paraelectric-ferroelectric phase transition TC, whereas for PSN is below TC. It is shown that the first critical pressure pc1, at which a transition from a relaxor to a non-polar rhombohedral state with antiphase octahedral tilt ordering occurs, decreases at elevated temperatures due to the weakening of the polar coupling, which in turn facilitates the evolution of the preexisting medium-range antiferrodistortive order into a long-range order. The critical pressure pc2 of the second phase transition, involving a change in the type of the antiferrodistortive order, is not affected by temperature, i.e. it is independent of the state of polar coupling and is mainly related to the initial correlation length of antiferrodistortive order. The strong influence of temperature on pc1, which occurs only when the mesoscopic polar order is suppressed, emphasizes the importance of coexisting ferroelectric and antiferrodistortive coupling for the occurrence of the relaxor states.

  15. 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.

  16. Comparison of MTI satellite-derived surface water temperatures and in-situ measurements

    NASA Astrophysics Data System (ADS)

    Kurzeja, Robert J.; Pendergast, Malcolm M.; Villa-Aleman, Eliel; Garrett, Alfred J.

    2002-01-01

    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% of the calculated values at the Pacific Ocean site but were 1-2% different over the mid-latitude lake.

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

    NASA Astrophysics Data System (ADS)

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

    2015-09-01

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

  18. Temperature control in thermal microactuators with applications to in-situ nanomechanical testing

    NASA Astrophysics Data System (ADS)

    Qin, Qingquan; Zhu, Yong

    2013-01-01

    Thermal microactuators are used in many micro/nano-technologies. To circumvent undesired heating of the end effector, heat sink beams are co-fabricated with the thermal actuator and connected to the substrate. This paper reports a combined experimental and modeling study on the effect of such heat sink beams. Temperature distribution is measured and simulated using Raman scattering and multiphysics finite element method, respectively. Our results show that heat sink beams are effective in controlling the temperature of the thermal actuator. Insights on how to achieve both low temperature and large actuator displacement for in-situ mechanical testing of nanoscale specimens are provided.

  19. 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.

  20. 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.

  1. In situ LIF temperature measurements in aqueous ammonium chloride solution during uni-directional solidification

    NASA Astrophysics Data System (ADS)

    Shafii, M. Behshad; Lum, Chee L.; Koochesfahani, Manoochehr M.

    2010-04-01

    We present in situ whole-field measurements of the temperature field using laser-induced fluorescence in a study of bottom-chilled uni-directional solidification of aqueous ammonium chloride. We utilize a two-color, two-dye, ratiometric approach to address the significant spatial and temporal variations of laser sheet intensity field due to refractive index variations caused by the evolving concentration and temperature fields. In our work we take advantage of two temperature sensitive fluorescent dyes with opposite temperature sensitivities in order to increase the overall sensitivity and temperature resolution of the measurements. The resulting temperature sensitivity (about 4% K-1) is more than a factor of two higher than the original work of Sakakibara and Adrian (Exp Fluids 26:7-15, 1999) with a sensitivity 1.7% K-1. In situ measurements of the temperature field during solidification are presented, along with temperature characteristics of some of the complex flow features, such as plumes and fingers.

  2. 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

  3. High-resistive layers obtained through periodic growth and in situ annealing of InGaN by metalorganic chemical vapor deposition

    NASA Astrophysics Data System (ADS)

    Zhang, Shuo; Ma, Ping; Liu, Boting; Wu, Dongxue; Huang, Yuliang; Wang, Junxi; Li, Jinmin

    2016-06-01

    High-resistive layers were obtained by periodic growth and in situ annealing of InGaN. The effect of the annealing temperature of InGaN on the indium content and the material sheet resistive was investigated. The indium content decreased as the increase of in situ annealing temperature. Additionally, the material sheet resistance increased with the increase of the in situ annealing temperature for the annealed samples and reached 2 × 1010Ω/sq in the light and 2 × 1011Ω/sq in the dark when the in situ annealing temperature reached 970∘C. The acquirement of high-resistive layers is attributed to the generation of indium vacancy-related defects. Introducing indium vacancy-related defects to compensate background carriers can be an effective method to grow high-resistance material.

  4. 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}.

  5. 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.

  6. 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.

  7. Fractured rock stress-permeability relationships from in situ data and effects of temperature and chemical-mechanical couplings

    SciTech Connect

    Rutqvist, J.

    2014-09-19

    The purpose of this paper is to (i) review field data on stress-induced permeability changes in fractured rock; (ii) describe estimation of fractured rock stress-permeability relationships through model calibration against such field data; and (iii) discuss observations of temperature and chemically mediated fracture closure and its effect on fractured rock permeability. The field data that are reviewed include in situ block experiments, excavation-induced changes in permeability around tunnels, borehole injection experiments, depth (and stress) dependent permeability, and permeability changes associated with a large-scale rock-mass heating experiment. Data show how the stress-permeability relationship of fractured rock very much depends on local in situ conditions, such as fracture shear offset and fracture infilling by mineral precipitation. Field and laboratory experiments involving temperature have shown significant temperature-driven fracture closure even under constant stress. Such temperature-driven fracture closure has been described as thermal overclosure and relates to better fitting of opposing fracture surfaces at high temperatures, or is attributed to chemically mediated fracture closure related to pressure solution (and compaction) of stressed fracture surface asperities. Back-calculated stress-permeability relationships from field data may implicitly account for such effects, but the relative contribution of purely thermal-mechanical and chemically mediated changes is difficult to isolate. Therefore, it is concluded that further laboratory and in situ experiments are needed to increase the knowledge of the true mechanisms behind thermally driven fracture closure, and to further assess the importance of chemical-mechanical coupling for the long-term evolution of fractured rock permeability.

  8. Fractured rock stress-permeability relationships from in situ data and effects of temperature and chemical-mechanical couplings

    DOE PAGESBeta

    Rutqvist, J.

    2014-09-19

    The purpose of this paper is to (i) review field data on stress-induced permeability changes in fractured rock; (ii) describe estimation of fractured rock stress-permeability relationships through model calibration against such field data; and (iii) discuss observations of temperature and chemically mediated fracture closure and its effect on fractured rock permeability. The field data that are reviewed include in situ block experiments, excavation-induced changes in permeability around tunnels, borehole injection experiments, depth (and stress) dependent permeability, and permeability changes associated with a large-scale rock-mass heating experiment. Data show how the stress-permeability relationship of fractured rock very much depends on localmore » in situ conditions, such as fracture shear offset and fracture infilling by mineral precipitation. Field and laboratory experiments involving temperature have shown significant temperature-driven fracture closure even under constant stress. Such temperature-driven fracture closure has been described as thermal overclosure and relates to better fitting of opposing fracture surfaces at high temperatures, or is attributed to chemically mediated fracture closure related to pressure solution (and compaction) of stressed fracture surface asperities. Back-calculated stress-permeability relationships from field data may implicitly account for such effects, but the relative contribution of purely thermal-mechanical and chemically mediated changes is difficult to isolate. Therefore, it is concluded that further laboratory and in situ experiments are needed to increase the knowledge of the true mechanisms behind thermally driven fracture closure, and to further assess the importance of chemical-mechanical coupling for the long-term evolution of fractured rock permeability.« less

  9. 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

  10. 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. PMID:26998522

  11. Temperature response of denitrification and anammox reveals the adaptation of microbial communities to in situ temperatures in permeable marine sediments that span 50° in latitude

    NASA Astrophysics Data System (ADS)

    Canion, A.; Kostka, J. E.; Gihring, T. M.; Huettel, M.; van Beusekom, J. E. E.; Gao, H.; Lavik, G.; Kuypers, M. M. M.

    2013-09-01

    Despite decades of research on the physiology and biochemistry of nitrate/nitrite-respiring microorganisms, little is known regarding their metabolic response to temperature, especially under in situ conditions. The temperature regulation of microbial communities that mediate anammox and denitrification was investigated in near shore permeable sediments at polar, temperate, and subtropical sites with annual mean temperatures ranging from -5 to 23 °C. Total N2 production rates were determined using the isotope pairing technique in intact core incubations under diffusive and simulated advection conditions and ranged from 2 to 359 μmol N m-2 d-1. For the majority of sites studied, N2 removal was 2 to 7 times more rapid under advective flow conditions. Anammox comprised 6 to 14% of total N2 production at temperate and polar sites and was not detected at the subtropical site. Potential rates of denitrification and anammox were determined in anaerobic slurries in a temperature gradient block incubator across a temperature range of -1 to 42 °C. The highest optimum temperature (Topt) for denitrification was 36 °C and was observed in subtropical sediments, while the lowest Topt of 21 °C was observed at the polar site. Seasonal variation in the Topt was observed at the temperate site with values of 26 and 34 °C in winter and summer, respectively. The Topt values for anammox were 9 and 26 °C at the polar and temperate sites, respectively. The results demonstrate adaptation of denitrifying communities to in situ temperatures in permeable marine sediments across a wide range of temperatures, whereas marine anammox bacteria may be predominately psychrophilic to psychrotolerant. To our knowledge, we provide the first rates of denitrification and anammox from permeable sediments of a polar permanently cold ecosystem. The adaptation of microbial communities to in situ temperatures suggests that the relationship between temperature and rates of N removal is highly dependent

  12. Temperature response of denitrification and anammox reveals the adaptation of microbial communities to in situ temperatures in permeable marine sediments that span 50° in latitude

    NASA Astrophysics Data System (ADS)

    Canion, A.; Kostka, J. E.; Gihring, T. M.; Huettel, M.; van Beusekom, J. E. E.; Gao, H.; Lavik, G.; Kuypers, M. M. M.

    2014-01-01

    Despite decades of research on the physiology and biochemistry of nitrate/nitrite-respiring microorganisms, little is known regarding their metabolic response to temperature, especially under in situ conditions. The temperature regulation of microbial communities that mediate anammox and denitrification was investigated in near shore permeable sediments at polar, temperate, and subtropical sites with annual mean temperatures ranging from -5 to 23 °C. Total N2 production rates were determined using the isotope pairing technique in intact core incubations under diffusive and simulated advection conditions and ranged from 2 to 359 μmol N m-2 d-1. For the majority of sites studied, N2 removal was 2-7 times more rapid under simulated advective flow conditions. Anammox comprised 6-14% of total N2 production at temperate and polar sites and was not detected at the subtropical site. Potential rates of denitrification and anammox were determined in anaerobic slurries in a temperature gradient block incubator across a temperature range of -1 °C to 42 °C. The highest optimum temperature (Topt) for denitrification was 36 °C and was observed in subtropical sediments, while the lowest Topt of 21 °C was observed at the polar site. Seasonal variation in the Topt was observed at the temperate site with values of 26 and 34 °C in winter and summer, respectively. The Topt values for anammox were 9 and 26 °C at the polar and temperate sites, respectively. The results demonstrate adaptation of denitrifying communities to in situ temperatures in permeable marine sediments across a wide range of temperatures, whereas marine anammox bacteria may be predominately psychrophilic to psychrotolerant. The adaptation of microbial communities to in situ temperatures suggests that the relationship between temperature and rates of N removal is highly dependent on community structure.

  13. In situ investigation of Geobacillus stearothermophilus spore germination and inactivation mechanisms under moderate high pressure.

    PubMed

    Georget, Erika; Kapoor, Shobhna; Winter, Roland; Reineke, Kai; Song, Youye; Callanan, Michael; Ananta, Edwin; Heinz, Volker; Mathys, Alexander

    2014-08-01

    Bacterial spores are a major concern for food safety due to their high resistance to conventional preservation hurdles. Innovative hurdles can trigger bacterial spore germination or inactivate them. In this work, Geobacillus stearothermophilus spore high pressure (HP) germination and inactivation mechanisms were investigated by in situ infrared spectroscopy (FT-IR) and fluorometry. G. stearothermophilus spores' inner membrane (IM) was stained with Laurdan fluorescent dye. Time-dependent FT-IR and fluorescence spectra were recorded in situ under pressure at different temperatures. The Laurdan spectrum is affected by the lipid packing and level of hydration, and provided information on the IM state through the Laurdan generalized polarization. Changes in the -CH2 and -CH3 asymmetric stretching bands, characteristic of lipids, and in the amide I' band region, characteristic of proteins' secondary structure elements, enabled evaluation of the impact of HP on endospores lipid and protein structures. These studies were complemented by ex situ analyses (plate counts and microscopy). The methods applied showed high potential to identify germination mechanisms, particularly associated to the IM. Germination up to 3 log10 was achieved at 200 MPa and 55 °C. A molecular-level understanding of these mechanisms is important for the development and validation of multi-hurdle approaches to achieve commercial sterility. PMID:24750808

  14. 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

  15. High pressure optical cell for synthesis and in situ Raman spectroscopy of hydrogen clathrate hydrates

    NASA Astrophysics Data System (ADS)

    Celli, Milva; Zoppi, Marco; Zaghloul, Mohamed A. S.; Ulivi, Lorenzo

    2012-11-01

    We report the design, realization, and test of a high-pressure optical cell that we have used to measure the Raman spectra of hydrogen clathrate hydrates, synthesized in situ by the application of 200-300 MPa of gas pressure on solid water. The optical apparatus is mounted on a cryogenic system so to allow measurements and sample treatment at any temperature between 300 and 20 K. A capillary pipe is connected to the inside of the cell to allow the gas flow into and out of the cell, and to regulate the internal pressure at any value from 0 to 300 MPa. In the experimental test described in this paper, the cell has been partly filled, at room temperature, with a small amount of water, then frozen at 263 K before injecting hydrogen gas, at pressure of 150 MPa, into the cell. This procedure has permitted to study hydrogen clathrate formation, by measuring Raman spectra as a function of time.

  16. 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.

  17. 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.

  18. In situ growth of carbon nanotube wrapped Si composites as anodes for high performance lithium ion batteries.

    PubMed

    Zhou, Jianbin; Lan, Yang; Zhang, Kailong; Xia, Guoliang; Du, Jin; Zhu, Yongchun; Qian, Yitai

    2016-03-01

    The composites of carbon nanotube wrapped Si particles (CNTWS) were synthesized in situ by using the catalytic chemical vapor deposition (CCVD) method. In this process, carbon nanotubes were produced in situ to wrap Si by the catalysis action of nascent Cu* under an acetylene atmosphere at a relatively low temperature of 400 °C, in which nascent Cu* was created by the reaction between Si particles and CuCl synchronously. The weight ratio of Si/C in CNTWS is 0.76/0.24. As anode materials for lithium ion batteries, the CNTWS composites exhibit a reversible discharge capacity of 1031.1 mA h g(-1) at 1.8 A g(-1) after 500 cycles, and 868.2 mA h g(-1) at 10.0 A g(-1). The high electrochemical performance of CNTWS composites is associated with the in situ formed carbon nanotubes. PMID:26875542

  19. In situ growth of carbon nanotube wrapped Si composites as anodes for high performance lithium ion batteries

    NASA Astrophysics Data System (ADS)

    Zhou, Jianbin; Lan, Yang; Zhang, Kailong; Xia, Guoliang; Du, Jin; Zhu, Yongchun; Qian, Yitai

    2016-02-01

    The composites of carbon nanotube wrapped Si particles (CNTWS) were synthesized in situ by using the catalytic chemical vapor deposition (CCVD) method. In this process, carbon nanotubes were produced in situ to wrap Si by the catalysis action of nascent Cu* under an acetylene atmosphere at a relatively low temperature of 400 °C, in which nascent Cu* was created by the reaction between Si particles and CuCl synchronously. The weight ratio of Si/C in CNTWS is 0.76/0.24. As anode materials for lithium ion batteries, the CNTWS composites exhibit a reversible discharge capacity of 1031.1 mA h g-1 at 1.8 A g-1 after 500 cycles, and 868.2 mA h g-1 at 10.0 A g-1. The high electrochemical performance of CNTWS composites is associated with the in situ formed carbon nanotubes.The composites of carbon nanotube wrapped Si particles (CNTWS) were synthesized in situ by using the catalytic chemical vapor deposition (CCVD) method. In this process, carbon nanotubes were produced in situ to wrap Si by the catalysis action of nascent Cu* under an acetylene atmosphere at a relatively low temperature of 400 °C, in which nascent Cu* was created by the reaction between Si particles and CuCl synchronously. The weight ratio of Si/C in CNTWS is 0.76/0.24. As anode materials for lithium ion batteries, the CNTWS composites exhibit a reversible discharge capacity of 1031.1 mA h g-1 at 1.8 A g-1 after 500 cycles, and 868.2 mA h g-1 at 10.0 A g-1. The high electrochemical performance of CNTWS composites is associated with the in situ formed carbon nanotubes. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr08961a

  20. 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.

  1. 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.

  2. Enhancing the elevated temperature performance of high voltage LiNi0.5Mn1.5O4 by V doping with in-situ carbon and polyimide encapsulation

    NASA Astrophysics Data System (ADS)

    Lee, G. H.; Kim, H. S.; Baek, S. G.; Choi, H. J.; Chung, K. Y.; Cho, B. W.; Lee, S. Y.; Lee, Yun-Sung

    2015-12-01

    We report the enhanced electrochemical performance of high voltage LiNi0.5Mn1.5O4 cathode by small amount of aliovalent doping in Li-site (Li0.995V0.005Ni0.5Mn1.5O4) and polyimide-carbon (PI-C) coating as well. Such small amount of V-doping in Li-sites leads to the crystallization of ordered spinel. The performances of the cathodes are studied in half-cell assembly at elevated temperature conditions (50, 55 and 60 °C). Although, the notable improvement in elevated temperature conditions are noted for Li0.995V0.005Ni0.5Mn1.5O4 phase at 50 °C, but not sustained while increasing to 55 and 60 °C. Nevertheless, the combined advantages of mixed conducting (ionic and electronic) features of PI-C, an excellent performance are noted for the Li0.995V0.005Ni0.5Mn1.5O4 phase after introducing the PI-C layer, irrespective of the testing temperature. Cyclic voltammetry and impedance studies are also performed to corroborate the Li-ion kinetics.

  3. 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.

  4. In situ synchrotron IR study relating temperature and heating rate to surface functional group changes in biomass.

    PubMed

    Kirtania, Kawnish; Tanner, Joanne; Kabir, Kazi Bayzid; Rajendran, Sharmen; Bhattacharya, Sankar

    2014-01-01

    Three types of woody biomass were investigated under pyrolysis condition to observe the change in the surface functional groups by Fourier transform infrared (FTIR) technique with increasing temperature under two different (5 and 150°C/min) heating rates. The experiments were carried out in situ in the infrared microscopy beamline (IRM) of the Australian Synchrotron. The capability of the beamline made it possible to focus on single particles to obtain low noise measurements without mixing with KBr. At lower heating rate, the surface functional groups were completely removed by 550°C. In case of higher heating rate, a delay was observed in losing the functional groups. Even at a high temperature, significant number of functional groups was retained after the higher heating rate experiments. This implies that at considerably high heating rates typical of industrial reactors, more functional groups will remain on the surface. PMID:24189382

  5. 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.

  6. 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.

  7. 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

  8. Temperature-dependent luminescent properties of Eu-Tb complexes synthesized in situ in gel glass

    NASA Astrophysics Data System (ADS)

    Liu, Yan; Qian, Guodong; Wang, Zhiyu; Wang, Minquan

    2005-02-01

    The chelates of europium and terbium with hexafluoroacetylacetone (HFA) and triphenylphoshine oxide (TPPO), Eu /Tb(HFA)3(TPPO)2, have been synthesized in situ in gel glasses with various concentrations of Eu3+ and Tb3+ ions. The photoluminescence spectra have been measured and the characteristic transitions of Tb3+ and Eu3+ have been observed. Due to the variance of energy transfer efficiencies from Tb3+ to Eu3+, the intensity ratios of europium luminescent band to terbium band vary remarkably with measurement temperatures. In addition, the Förster mechanism has been proved to be responsible for the energy transfer between Eu3+ and Tb3+. The materials doped with Eu /Tb(HFA)3(TPPO)2 are promising for being used as a temperature detector and thermal-sensitive probe of optical fiber sensor.

  9. 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.

  10. A sample chamber for in situ high-energy X-ray studies of crystal growth at deeply buried interfaces in harsh environments

    NASA Astrophysics Data System (ADS)

    de Jong, A. E. F.; Vonk, V.; Honkimäki, V.; Gorges, B.; Vitoux, H.; Vlieg, E.

    2015-06-01

    We introduce a high pressure high temperature chamber for in situ synchrotron X-ray studies. The chamber design allows for in situ studies of thin film growth from solution at deeply buried interfaces in harsh environments. The temperature can be controlled between room temperature and 1073 K while the pressure can be set as high as 50 bar using a variety of gases including N2 and NH3. The formation of GaN on the surface of a Ga13Na7 melt at 1073 K and 50 bar of N2 is presented as a performance test.