Facility for low-temperature spin-polarized-scanning tunneling microscopy studies of magnetic/spintronic materials prepared in situ by nitride molecular beam epitaxy

International Nuclear Information System (INIS)

Lin, Wenzhi; Foley, Andrew; Alam, Khan; Wang, Kangkang; Liu, Yinghao; Chen, Tianjiao; Pak, Jeongihm; Smith, Arthur R.

2014-01-01

Based on the interest in, as well as exciting outlook for, nitride semiconductor based structures with regard to electronic, optoelectronic, and spintronic applications, it is compelling to investigate these systems using the powerful technique of spin-polarized scanning tunneling microscopy (STM), a technique capable of achieving magnetic resolution down to the atomic scale. However, the delicate surfaces of these materials are easily corrupted by in-air transfers, making it unfeasible to study them in stand-alone ultra-high vacuum STM facilities. Therefore, we have carried out the development of a hybrid system including a nitrogen plasma assisted molecular beam epitaxy/pulsed laser epitaxy facility for sample growth combined with a low-temperature, spin-polarized scanning tunneling microscope system. The custom-designed molecular beam epitaxy growth system supports up to eight sources, including up to seven effusion cells plus a radio frequency nitrogen plasma source, for epitaxially growing a variety of materials, such as nitride semiconductors, magnetic materials, and their hetero-structures, and also incorporating in situ reflection high energy electron diffraction. The growth system also enables integration of pulsed laser epitaxy. The STM unit has a modular design, consisting of an upper body and a lower body. The upper body contains the coarse approach mechanism and the scanner unit, while the lower body accepts molecular beam epitaxy grown samples using compression springs and sample skis. The design of the system employs two stages of vibration isolation as well as a layer of acoustic noise isolation in order to reduce noise during STM measurements. This isolation allows the system to effectively acquire STM data in a typical lab space, which during its construction had no special and highly costly elements included, (such as isolated slabs) which would lower the environmental noise. The design further enables tip exchange and tip coating without

A MEMS-based heating holder for the direct imaging of simultaneous in-situ heating and biasing experiments in scanning/transmission electron microscopes.

Science.gov (United States)

Mele, Luigi; Konings, Stan; Dona, Pleun; Evertz, Francis; Mitterbauer, Christoph; Faber, Pybe; Schampers, Ruud; Jinschek, Joerg R

2016-04-01

The introduction of scanning/transmission electron microscopes (S/TEM) with sub-Angstrom resolution as well as fast and sensitive detection solutions support direct observation of dynamic phenomena in-situ at the atomic scale. Thereby, in-situ specimen holders play a crucial role: accurate control of the applied in-situ stimulus on the nanostructure combined with the overall system stability to assure atomic resolution are paramount for a successful in-situ S/TEM experiment. For those reasons, MEMS-based TEM sample holders are becoming one of the preferred choices, also enabling a high precision in measurements of the in-situ parameter for more reproducible data. A newly developed MEMS-based microheater is presented in combination with the new NanoEx™-i/v TEM sample holder. The concept is built on a four-point probe temperature measurement approach allowing active, accurate local temperature control as well as calorimetry. In this paper, it is shown that it provides high temperature stability up to 1,300°C with a peak temperature of 1,500°C (also working accurately in gaseous environments), high temperature measurement accuracy (in-situ S/TEM imaging experiments, but also elemental mapping at elevated temperatures using energy-dispersive X-ray spectroscopy (EDS). Moreover, it has the unique capability to enable simultaneous heating and biasing experiments. © 2016 Wiley Periodicals, Inc.

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

Science.gov (United States)

2015-05-20

TEMPERATURES IN HIGH-TEMPERATURE THERMOSETTING POLYMERS 5a. CONTRACT NUMBER In-House 5b. GRANT NUMBER 5c. PROGRAM ELEMENT NUMBER 6. AUTHOR(S) 5d...temperature thermosetting polymer via dynamic mechanical analysis alone. These difficulties result from the residual cure of samples heated beyond their...98) Prescribed by ANSI Std. 239.18 Effect of In-Situ Cure on Measurement of Glass Transition Temperatures in High-Temperature Thermosetting

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

International Nuclear Information System (INIS)

Liu Chuan-Jiang; Zheng Hai-Fei

2012-01-01

An in-situ Raman spectroscopic study of gypsum-anhydrite transition under a saturated water condition at high pressure and high temperature is performed using a hydrothermal diamond anvil cell (HDAC). The experimental results show that gypsum dissolvs in water at ambient temperature and above 496 MPa. With increasing temperature, the anhydrite (CaSO 4 ) phase precipitates at 250–320°C in the pressure range of 1.0–1.5GPa, indicating that under a saturated water condition, both stable conditions of pressure and temperature and high levels of Ca and SO 4 ion concentrations in aqueous solution are essential for the formation of anhydrite. A linear relationship between the pressure and temperature for the precipitation of anhydrite is established as P(GPa) = 0.0068T−0.7126 (250°C≤T≤320°C). Anhydrite remained stable during rapid cooling of the sample chamber, showing that the gypsum-anhydrite transition involving both dissolution and precipitation processes is irreversible at high pressure and high temperature. (geophysics, astronomy, and astrophysics)

High Pressure Scanning Tunneling Microscopy Studies of Adsorbate Structure and Mobility during Catalytic Reactions. Novel Design of an Ultra High Pressure, High Temperature Scanning Tunneling Microscope System for Probing Catalytic Conversions

International Nuclear Information System (INIS)

Tang, David Chi-Wai

2005-01-01

The aim of the work presented therein is to take advantage of scanning tunneling microscope's (STM) capability for operation under a variety of environments under real time and at atomic resolution to monitor adsorbate structures and mobility under high pressures, as well as to design a new generation of STM systems that allow imaging in situ at both higher pressures (35 atm) and temperatures (350 C). The design of a high pressure, high temperature scanning tunneling microscope system, that is capable of monitoring reactions in situ at conditions from UHV and ambient temperature up to 1 atm and 250 C, is briefly presented along with vibrational and thermal analysis, as this system serves as a template to improve upon during the design of the new ultra high pressure, high temperature STM. Using this existing high pressure scanning tunneling microscope we monitored the co-adsorption of hydrogen, ethylene and carbon dioxide on platinum (111) and rhodium (111) crystal faces in the mTorr pressure range at 300 K in equilibrium with the gas phase. During the catalytic hydrogenation of ethylene to ethane in the absence of CO the metal surfaces are covered by an adsorbate layer that is very mobile on the time scale of STM imaging. We found that the addition of CO poisons the hydrogenation reaction and induces ordered structures on the single crystal surfaces. Several ordered structures were observed upon CO addition to the surfaces pre-covered with hydrogen and ethylene: a rotated (√19 x √19)R23.4 o on Pt(111), and domains of c(4 x 2)-CO+C 2 H 3 , previously unobserved (4 x 2)-CO+3C 2 H 3 , and (2 x 2)-3CO on Rh(111). A mechanism for CO poisoning of ethylene hydrogenation on the metal single crystals was proposed, in which CO blocks surface metal sites and reduces adsorbate mobility to limit adsorption and reaction rate of ethylene and hydrogen. In order to observe heterogeneous catalytic reactions that occur well above ambient pressure and temperature that more closely

In situ fatigue loading stage inside scanning electron microscope

Science.gov (United States)

Telesman, Jack; Kantzos, Peter; Brewer, David

1988-01-01

A fatigue loading stage inside a scanning electron microscopy (SEM) was developed. The stage allows dynamic and static high-magnification and high-resolution viewing of the fatigue crack initiation and crack propagation processes. The loading stage is controlled by a closed-loop servohydraulic system. Maximum load is 1000 lb (4450 N) with test frequencies ranging up to 30 Hz. The stage accommodates specimens up to 2 inches (50 mm) in length and tolerates substantial specimen translation to view the propagating crack. At room temperature, acceptable working resolution is obtainable for magnifications ranging up to 10,000X. The system is equipped with a high-temperature setup designed for temperatures up to 2000 F (1100 C). The signal can be videotaped for further analysis of the pertinent fatigue damage mechanisms. The design allows for quick and easy interchange and conversion of the SEM from a loading stage configuration to its normal operational configuration and vice versa. Tests are performed entirely in the in-situ mode. In contrast to other designs, the NASA design has greatly extended the life of the loading stage by not exposing the bellows to cyclic loading. The loading stage was used to investigate the fatigue crack growth mechanisms in the (100)-oriented PWA 1480 single-crystal, nickel-based supperalloy. The high-magnification observations revealed the details of the crack growth processes.

Study of CT Scan Flooding System at High Temperature and Pressure

Science.gov (United States)

Chen, X. Y.

2017-12-01

CT scan flooding experiment can scan micro-pore in different flooding stages by the use of CT scan technology, without changing the external morphology and internal structure of the core, and observe the distribution characterization in pore medium of different flooding fluid under different pressure.thus,it can rebuilt the distribution images of oil-water distribution in different flooding stages. However,under extreme high pressure and temperature conditions,the CT scan system can not meet the requirements. Container of low density materials or thin shell can not resist high pressure,while high density materials or thick shell will cause attenuation and scattering of X-ray. The experiment uses a simple Ct scanning systems.X ray from a point light source passing trough a micro beryllium shell on High pressure stainless steal container,continuously irradiates the core holder that can continuously 360° rotate along the core axis. A rare earth intensifying screen behind the core holder emitting light when irradiated with X ray can show the core X ray section image. An optical camera record the core X ray images through a transparency high pressure glazing that placed on the High pressure stainless steal container.Thus,multiple core X ray section images can reconstruct the 3D core reconstruction after a series of data processing.The experiment shows that both the micro beryllium shell and rare earth intensifying screen can work in high temperature and high pressure environment in the stainless steal container. This way that X-ray passes through a thin layer of micro beryllium shell , not high pressure stainless steal shell,avoid the attenuation and scattering of X-ray from the container shell,while improving the high-pressure experiment requirements.

Improved design for a low temperature scanning tunneling microscope with an in situ tip treatment stage.

Science.gov (United States)

Kim, J-J; Joo, S H; Lee, K S; Yoo, J H; Park, M S; Kwak, J S; Lee, Jinho

2017-04-01

The Low Temperature Scanning Tunneling Microscope (LT-STM) is an extremely valuable tool not only in surface science but also in condensed matter physics. For years, numerous new ideas have been adopted to perfect LT-STM performances-Ultra-Low Vibration (ULV) laboratory and the rigid STM head design are among them. Here, we present three improvements for the design of the ULV laboratory and the LT-STM: tip treatment stage, sample cleaving stage, and vibration isolation system. The improved tip treatment stage enables us to perform field emission for the purpose of tip treatment in situ without exchanging samples, while our enhanced sample cleaving stage allows us to cleave samples at low temperature in a vacuum without optical access by a simple pressing motion. Our newly designed vibration isolation system provides efficient space usage while maintaining vibration isolation capability. These improvements enhance the quality of spectroscopic imaging experiments that can last for many days and provide increased data yield, which we expect can be indispensable elements in future LT-STM designs.

Impedance measurements on Au microelectrodes using controlled atmosphere high temperature scanning probe microscope

DEFF Research Database (Denmark)

Wu, Yuehua; Hansen, Karin Vels; Jacobsen, Torben

2011-01-01

High temperature impedance measurements on Au microelectrodes deposited on polished yttria stabilized zirconia (YSZ) pellets were demonstrated using a newly designed controlled atmosphere high temperature scanning probe microscope (CAHT-SPM). Probes based on Pt0.8Ir0.2 were fabricated and employed...

In-Situ Microprobe Observations of Dispersed Oil with Low-Temperature Low-Vacuum Scanning Electron Microscope

International Nuclear Information System (INIS)

Mohsen, H.T.

2010-01-01

A low cost cryostat stage from high heat capacity material is designed and constructed, in attempt to apply size distribution techniques for examination of oil dispersions. Different materials were tested according to their heat capacity to keep the liquid under investigation in frozen state as long as possible during the introduction of the cryostat stage to the low-vacuum scanning electron microscope. Different concentrations of non ionic surfactant were added to artificially contaminated with 10000 ppm Balayeam base oil in 3.5 % saline water, where oil and dispersing liquid have been added and shacked well to be investigated under the microscope as fine frozen droplets. The efficiency of dispersion was examined using low temperature low-vacuum scanning electron microscope. The shape and size distributions of freeze oil droplets were studied by digital imaging processing technique in conjunction with scanning electron microscope counting method. Also elemental concentration of oil droplets was analyzed.

Evolution of Near-Surface Internal and External Oxide Morphology During High-Temperature Selective Oxidation of Steels

Science.gov (United States)

Story, Mary E.; Webler, Bryan A.

2018-05-01

In this work we examine some observations made using high-temperature confocal scanning laser microscopy (HT-CSLM) during selective oxidation experiments. A plain carbon steel and advanced high-strength steel (AHSS) were selectively oxidized at high temperature (850-900°C) in either low oxygen or water vapor atmospheres. Surface evolution, including thermal grooving along grain boundaries and oxide growth, was viewed in situ during heating. Experiments investigated the influence of the microstructure and oxidizing atmosphere on selective oxidation behavior. Sequences of CSLM still frames collected during the experiment were processed with ImageJ to obtain histograms that showed a general darkening trend indicative of oxidation over time with all samples. Additional ex situ scanning electron microscopy and energy dispersive spectroscopy analysis supported in situ observations. Distinct oxidation behavior was observed for each case. Segregation, grain orientation, and extent of internal oxidation were all found to strongly influence surface evolution.

The Silicon Environment in Silica Polymorphs, Aluminosilicate Crystals and Melts: An In Situ High Temperature XAS Study

International Nuclear Information System (INIS)

Cormier, L.; Neuville, D. R.; Roux, J.; Ligny, D. de; Henderson, G. S.; Flank, A.-M.; Lagarde, P.

2007-01-01

High temperature X-ray absorption spectroscopy at the Si K-edge has been used to obtain in situ information on SiO2 phase transitions upon heating. Important modifications are observed for the XANES spectra of the high temperature polymorphs, in relation to disordering of the SiO4 tetrahedra beyond the short-range correlations. This paper also presents the XANES spectra of anorthite (CaAl2Si2O8) from room temperature up to the melt (1900 K). This study shows the possibilities for determining the Si environment in crystals and glasses up to the liquid state using in situ XANES measurements

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

Science.gov (United States)

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

2013-10-01

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

Oxygen-free in situ scanning tunnelling microscopy

DEFF Research Database (Denmark)

Zhang, Jingdong; Ulstrup, Jens

2007-01-01

Scanning tunneling microscopy under full electrochemical potential control (in situ STM) has been used extensively as an efficient method to characterize microstructures at solid/liquid interfaces at the atomic and molecular levels. However, under ambient conditions oxygen may interfere in open i...

In-situ heater test in sedimentary soft rocks under high temperature (Phase I)

International Nuclear Information System (INIS)

Ikenoya, Takafumi; Takakura, Nozomu; Okada, Tetsuji; Sawada, Masataka; Hirano, Kouhei; Tani, Kazuo

2008-01-01

Various researches have been conducted on high level radioactive waste geological disposal in sedimentary soft rocks. It's noted that the long-term mechanical behaviors of sedimentary soft rocks can be affected by various environmental factors such as temperatures or hydraulic conditions. Therefore, in-situ heater test was conducted in an underground cavern at a depth of 50 meters for the purpose of improving thermo-hydro-mechanical coupled analysis code. This report presents the test result demonstrating the changes of temperature and strain distributions with time at the elevated temperature of the heater up to 40 degrees Celsius. (author)

High-Temperature Confocal Laser Scanning Microscopy Studies of Ferrite Formation in Inclusion-Engineered Steels: A Review

Science.gov (United States)

Mu, Wangzhong; Hedström, Peter; Shibata, Hiroyuki; Jönsson, Pär G.; Nakajima, Keiji

2018-05-01

The concepts of oxide metallurgy and inclusion engineering can be utilized to improve the properties of low-alloy steels. These concepts aim at controlling the formation of intragranular ferrite (IGF), often a desirable microstructure providing good mechanical properties without the need for expensive alloying elements. IGF formation is stimulated to occur at non-metallic inclusions and form an arrangement of fine, interlocking ferrite grains. A method that has contributed significantly to investigations in this field lately is high-temperature confocal laser scanning microscopy (HT-CLSM). HT-CLSM is suited for in situ studies of inclusion behavior in liquid steel and phase transformations in solid-state steel, where in particular, displacive phase transformations can be studied, since they provide sufficient topographic contrast. The purpose of the present report is to provide a brief review of the state of the art of HT-CLSM and its application for in situ observations of ferrite formation in inclusion-engineered steels. The scientific literature in this field is surveyed and supplemented by new work to reveal the capability of HT-CLSM as well as to discuss the effect of factors such as cooling rate and parent grain size on IGF formation and growth kinetics. The report concludes with an outlook on the opportunities and challenges of HT-CLSM for applications in oxide metallurgy.

In-situ high-temperature Raman spectroscopic studies of aluminosilicate liquids

Science.gov (United States)

Daniel, Isabelle; Gillet, Philippe; Poe, Brent T.; McMillan, Paul F.

1995-03-01

We have measured in-situ Raman spectra of aluminosilicate glasses and liquids with albite (NaAlSi3 O8) and anorthite (CaAl2Si2O8) compositions at high temperatures, through their glass transition range up to 1700 and 2000 K, respectively. For these experiments, we have used a wire-loop heating device coupled with micro-Raman spectroscopy, in order to achieve effective spatial filtering of the extraneous thermal radiation. A major concern in this work is the development of methodology for reliably extracting the first and second order contributions to the Raman scattering spectra of aluminosilicate glasses and liquids from the high temperature experimental data, and analyzing these in terms of vibrational (anharmonic) and configurational changes. The changes in the first order Raman spectra with temperature are subtle. The principal low frequency band remains nearly constant with increasing temperature, indicating little change in the T-O-T angle, and that the angle bending vibration is quite harmonic. This is in contrast to vitreous SiO2, studied previously. Above Tg, intensity changes in the 560 590 cm-1 regions of both sets of spectra indicate configurational changes in the supercooled liquids, associated with formation of additional Al-O-Al linkages, or 3-membered (Al, Si)-containing rings. Additional intensity at 800 cm-1 reflects also some rearrangement of the Si-O-Al network.

Micro-four-point probes in a UHV scanning electron microscope for in-situ surface-conductivity measurements

DEFF Research Database (Denmark)

Shiraki, I.; Nagao, T.; Hasegawa, S.

2000-01-01

For in-situ measurements of surface conductivity in ultrahigh vacuum (UHV), we have installed micro-four-point probes (probe spacings down to 4 mum) in a UHV scanning electron microscope (SEM) combined with scanning reflection-high-energy electron diffraction (RHEED). With the aid of piezoactuators...

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

Science.gov (United States)

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.

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

Science.gov (United States)

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. Copyright © 2014 ISA. All rights reserved.

In-situ high temperature XRD of calcium phosphate biomaterial using DEHPA as the starting material

International Nuclear Information System (INIS)

Meor Yusoff Meor Sulaiman; Masliana Muslim

2009-01-01

A process to produce calcium phosphate biomaterial was done using an organic based phosphoric acid (DEHPA) as its starting material. The gel obtained from this reaction was used to study calcium phosphate transformation using in-situ XRD with temperature ranges from room temperature to 1300 degree C. The results obtained from this analysis show the following phase transformation: Gel β-Ca 2 P 2 O 7 β-TCP + HA α-TCP + HA, β-Ca 2 P 2 O 7 forms at 400 degree C and as we heat the sample at 1000 degree C peaks belonging to β- TCP and HA appears showing the transformation of the β-Ca 2 P 2 O 7 phase. When the sample is heated up further to 1200 degree C, β-TCP is transform into α-TCP. In the cold in-situ study, XRD analysis was performed on the sample from room temperature to -140 degree C. At room the XRD diffractogram shows the sample as an amorphous material and as the temperature was further lowered sharp peaks begins to form indicating that the material had becomes crystalline. The peaks were identified to be that calcium hydrogen phosphate (Ca(H 2 PO 4 ) 2 ) and this indicates that there is no hydroxyl group removal during the cooling process. The relative crystallinity values obtained for the different cooling temperatures show a slow exponential increase on the initial cooling of 0 to -100 degree C and at further cooling temperatures resulted fast and linear process. Also unlike the in-situ XRD analysis performs at high temperature no phase transformation occurred at this low temperature. (Author)

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

International Nuclear Information System (INIS)

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

2011-01-01

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.

Scanning SQUID microscope with an in-situ magnetization/demagnetization field for geological samples

Science.gov (United States)

Du, Junwei; Liu, Xiaohong; Qin, Huafeng; Wei, Zhao; Kong, Xiangyang; Liu, Qingsong; Song, Tao

2018-04-01

Magnetic properties of rocks are crucial for paleo-, rock-, environmental-magnetism, and magnetic material sciences. Conventional rock magnetometers deal with bulk properties of samples, whereas scanning microscope can map the distribution of remanent magnetization. In this study, a new scanning microscope based on a low-temperature DC superconducting quantum interference device (SQUID) equipped with an in-situ magnetization/demagnetization device was developed. To realize the combination of sensitive instrument as SQUID with high magnetizing/demagnetizing fields, the pick-up coil, the magnetization/demagnetization coils and the measurement mode of the system were optimized. The new microscope has a field sensitivity of 250 pT/√Hz at a coil-to-sample spacing of ∼350 μm, and high magnetization (0-1 T)/ demagnetization (0-300 mT, 400 Hz) functions. With this microscope, isothermal remanent magnetization (IRM) acquisition and the according alternating field (AF) demagnetization curves can be obtained for each point without transferring samples between different procedures, which could result in position deviation, waste of time, and other interferences. The newly-designed SQUID microscope, thus, can be used to investigate the rock magnetic properties of samples at a micro-area scale, and has a great potential to be an efficient tool in paleomagnetism, rock magnetism, and magnetic material studies.

High-temperature mechanical properties and fracture mechanisms of Al–Si piston alloy reinforced with in situ TiB{sub 2} particles

Energy Technology Data Exchange (ETDEWEB)

Han, Gang [School of Mechanical Engineering, Beijing Institute of Technology, 5 South Zhongguancun Street, Haidian District, Beijing 100081 (China); Zhang, Weizheng, E-mail: zhangwz@bit.edu.cn [School of Mechanical Engineering, Beijing Institute of Technology, 5 South Zhongguancun Street, Haidian District, Beijing 100081 (China); Zhang, Guohua; Feng, Zengjian; Wang, Yanjun [Shandong Binzhou Bohai Piston Co., Ltd., Binzhou 256602 (China)

2015-05-01

In order to assess the high-temperature performance of aluminum–silicon alloy reinforced with titanium diboride particles as potential piston material, the tensile behaviors and fracture mechanisms of in situ 4 wt% TiB{sub 2}/Al–Si composite were investigated in the temperature range 25–350 °C. The tensile results revealed that the composite exhibited higher modulus than the matrix alloy at all testing temperatures, but both the matrix alloy and the composite presented similar strength levels above 200 °C. The ductility of the composite was found to be lower than that of the unreinforced matrix alloy at 25 and 200 °C, but no obvious distinction was observed at 350 °C. The effects of temperature and the presence of TiB{sub 2} particles on tensile properties of the composite had been evaluated. Fractographic morphology studies were done using scanning electron microscope, which indicated that the fracture of the composite altered from brittle to ductile mode with temperature increasing. At 25 and 200 °C, fracture was dominated by cracked silicon particles and separated TiB{sub 2} particles, while decohesion at particle–matrix interface was prevalent at 350 °C. Analysis of the fracture surfaces also showed that regions of clustered TiB{sub 2} particles were found to be the locations prone to damage in the composite at both room and high temperatures.

Probing the thermal decomposition behaviors of ultrathin HfO2 films by an in situ high temperature scanning tunneling microscope.

Science.gov (United States)

Xue, Kun; Wang, Lei; An, Jin; Xu, Jianbin

2011-05-13

The thermal decomposition of ultrathin HfO(2) films (∼0.6-1.2 nm) on Si by ultrahigh vacuum annealing (25-800 °C) is investigated in situ in real time by scanning tunneling microscopy. Two distinct thickness-dependent decomposition behaviors are observed. When the HfO(2) thickness is ∼ 0.6 nm, no discernible morphological changes are found below ∼ 700 °C. Then an abrupt reaction occurs at 750 °C with crystalline hafnium silicide nanostructures formed instantaneously. However, when the thickness is about 1.2 nm, the decomposition proceeds gradually with the creation and growth of two-dimensional voids at 800 °C. The observed thickness-dependent behavior is closely related to the SiO desorption, which is believed to be the rate-limiting step of the decomposition process.

Global Land Surface Temperature From the Along-Track Scanning Radiometers

Science.gov (United States)

Ghent, D. J.; Corlett, G. K.; Göttsche, F.-M.; Remedios, J. J.

2017-11-01

The Leicester Along-Track Scanning Radiometer (ATSR) and Sea and Land Surface Temperature Radiometer (SLSTR) Processor for LAnd Surface Temperature (LASPLAST) provides global land surface temperature (LST) products from thermal infrared radiance data. In this paper, the state-of-the-art version of LASPLAST, as deployed in the GlobTemperature project, is described and applied to data from the Advanced Along-Track Scanning Radiometer (AATSR). The LASPLAST retrieval formulation for LST is a nadir-only, two-channel, split-window algorithm, based on biome classification, fractional vegetation, and across-track water vapor dependences. It incorporates globally robust retrieval coefficients derived using highly sampled atmosphere profiles. LASPLAST benefits from appropriate spatial resolution auxiliary information and a new probabilistic-based cloud flagging algorithm. For the first time for a satellite-derived LST product, pixel-level uncertainties characterized in terms of random, locally correlated, and systematic components are provided. The new GlobTemperature GT_ATS_2P Version 1.0 product has been validated for 1 year of AATSR data (2009) against in situ measurements acquired from "gold standard reference" stations: Gobabeb, Namibia, and Evora, Portugal; seven Surface Radiation Budget stations, and the Atmospheric Radiation Measurement station at Southern Great Plains. These data show average absolute biases for the GT_ATS_2P Version 1.0 product of 1.00 K in the daytime and 1.08 K in the nighttime. The improvements in data provenance including better accuracy, fully traceable retrieval coefficients, quantified uncertainty, and more detailed information in the new harmonized format of the GT_ATS_2P product will allow for more significant exploitation of the historical LST data record from the ATSRs and a valuable near-real-time service from the Sea and Land Surface Temperature Radiometers (SLSTRs).

Monitoring of high temperature zone by resistivity tomography during in-situ heater test in sedimentary soft rocks

International Nuclear Information System (INIS)

Kubota, Kenji; Suzuki, Koichi; Ikenoya, Takafumi; Takakura, Nozomu; Tani, Kazuo

2008-01-01

In-situ heater test has been conducted to evaluate the influence of high temperature in an underground facility at a depth of 50 m. Resistivity monitoring is thought to be effective to map the extent of the high temperature zone. So we have conducted resistivity tomography during the heater test. As a result, low resistivity zone was appeared near the heated area as starting the heating, and the zone was expanded. Resistivity of rock is proportional to resistivity of pore water. It is known that pore water resistivity decreases as the temperature rise. This suggests that high temperature zone is detected and spatial distribution of temperature can be mapped by resistivity tomography. (author)

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

DEFF Research Database (Denmark)

Ali, Syed Talat; Lebæk, Jesper; Nielsen, Lars Pleth

2010-01-01

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

Application of in-situ nano-scanning calorimetry and X-ray diffraction to characterize Ni–Ti–Hf high-temperature shape memory alloys

Energy Technology Data Exchange (ETDEWEB)

McCluskey, Patrick J., E-mail: mccluske@ge.com [GE Global Research, One Research Circle, Niskayuna, NY 12309 (United States); Xiao, Kechao [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States); Gregoire, John M. [Joint Center for Artificial Photosynthesis, California Institute of Technology, 1200 E. California Blvd., Pasadena, CA 91125 (United States); Dale, Darren [Cornell High Energy Synchrotron Source, Ithaca, NY 14853 (United States); Vlassak, Joost J. [School of Engineering and Applied Sciences, Harvard University, 29 Oxford Street, Cambridge, MA 02138 (United States)

2015-03-10

Combinatorial nanocalorimetry and synchrotron X-ray diffraction were combined to study the martensite–austenite (M–A) phase transformation behavior of Ni–Ti–Hf shape memory alloys. A thin-film library of Ni–Ti–Hf samples with a range of compositions was deposited on a parallel nano-scanning calorimeter device using sputter deposition. Crystallization of each amorphous as-deposited sample by local heating at approximately 10{sup 4} K/s produced a nanoscale grain structure of austenite and martensite. Individual samples were then cycled through the M–A transformation, while the transformation enthalpy was measured by nanocalorimetry and the low- and high-temperature phase compositions were determined by X-ray diffraction. The techniques enable correlation of the observed behavior during thermal cycling with the thermodynamic and structural properties of the samples.

A 10 mK scanning tunneling microscope operating in ultra high vacuum and high magnetic fields.

Science.gov (United States)

Assig, Maximilian; Etzkorn, Markus; Enders, Axel; Stiepany, Wolfgang; Ast, Christian R; Kern, Klaus

2013-03-01

We present design and performance of a scanning tunneling microscope (STM) that operates at temperatures down to 10 mK providing ultimate energy resolution on the atomic scale. The STM is attached to a dilution refrigerator with direct access to an ultra high vacuum chamber allowing in situ sample preparation. High magnetic fields of up to 14 T perpendicular and up to 0.5 T parallel to the sample surface can be applied. Temperature sensors mounted directly at the tip and sample position verified the base temperature within a small error margin. Using a superconducting Al tip and a metallic Cu(111) sample, we determined an effective temperature of 38 ± 1 mK from the thermal broadening observed in the tunneling spectra. This results in an upper limit for the energy resolution of ΔE = 3.5 kBT = 11.4 ± 0.3 μeV. The stability between tip and sample is 4 pm at a temperature of 15 mK as demonstrated by topography measurements on a Cu(111) surface.

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

Science.gov (United States)

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.

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

International Nuclear Information System (INIS)

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

2016-01-01

Highlights: • Investigation of the initial stages of epitaxial growth of Ge on Si(1 1 1) in situ by RHEED. • Impact of growth temperature on strain evolution for temperatures between 200 °C and 400 °C. • Epitaxy with a high degree of structural perfection already at growth temperature of 200 °C. • Ordered interfacial dislocation networks already at 200 °C. • Tensile strain contribution of Si(1 1 1) 7 × 7-surface reconstruction to strain relaxation process for epitaxial growth of Ge. - Abstract: 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 < d c < 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.

A modular designed ultra-high-vacuum spin-polarized scanning tunneling microscope with controllable magnetic fields for investigating epitaxial thin films.

Science.gov (United States)

Wang, Kangkang; Lin, Wenzhi; Chinchore, Abhijit V; Liu, Yinghao; Smith, Arthur R

2011-05-01

A room-temperature ultra-high-vacuum scanning tunneling microscope for in situ scanning freshly grown epitaxial films has been developed. The core unit of the microscope, which consists of critical components including scanner and approach motors, is modular designed. This enables easy adaptation of the same microscope units to new growth systems with different sample-transfer geometries. Furthermore the core unit is designed to be fully compatible with cryogenic temperatures and high magnetic field operations. A double-stage spring suspension system with eddy current damping has been implemented to achieve ≤5 pm z stability in a noisy environment and in the presence of an interconnected growth chamber. Both tips and samples can be quickly exchanged in situ; also a tunable external magnetic field can be introduced using a transferable permanent magnet shuttle. This allows spin-polarized tunneling with magnetically coated tips. The performance of this microscope is demonstrated by atomic-resolution imaging of surface reconstructions on wide band-gap GaN surfaces and spin-resolved experiments on antiferromagnetic Mn(3)N(2)(010) surfaces.

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

Science.gov (United States)

Hayashi, Yasuhiko; Tokunaga, Tomoharu; Iijima, Toru; Iwata, Takuya; Kalita, Golap; Tanemura, Masaki; Sasaki, Katsuhiro; Kuroda, Kotaro

2012-08-08

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.

Single-Crystal Tungsten Carbide in High-Temperature In-Situ Additive Manufacturing Characterization

Energy Technology Data Exchange (ETDEWEB)

Kolopus, James A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Boatner, Lynn A. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-05-18

Nanoindenters are commonly used for measuring the mechanical properties of a wide variety of materials with both industrial and scientific applications. Typically, these instruments employ an indenter made of a material of suitable hardness bonded to an appropriate shaft or holder to create an indentation on the material being tested. While a variety of materials may be employed for the indenter, diamond and boron carbide are by far the most common materials used due to their hardness and other desirable properties. However, as the increasing complexity of new materials demands a broader range of testing capabilities, conventional indenter materials exhibit significant performance limitations. Among these are the inability of diamond indenters to perform in-situ measurements at temperatures above 600oC in air due to oxidation of the diamond material and subsequent degradation of the indenters mechanical properties. Similarly, boron carbide also fails at high temperature due to fracture. [1] Transition metal carbides possess a combination of hardness and mechanical properties at high temperatures that offer an attractive alternative to conventional indenter materials. Here we describe the technical aspects for the growth of single-crystal tungsten carbide (WC) for use as a high-temperature indenter material, and we examine a possible approach to brazing these crystals to a suitable mount for grinding and attachment to the indenter instrument. The use of a by-product of the recovery process is also suggested as possibly having commercial value.

A 20 year independent record of sea surface temperature for climate from Along-Track Scanning Radiometers

Science.gov (United States)

Merchant, Christopher J.; Embury, Owen; Rayner, Nick A.; Berry, David I.; Corlett, Gary K.; Lean, Katie; Veal, Karen L.; Kent, Elizabeth C.; Llewellyn-Jones, David T.; Remedios, John J.; Saunders, Roger

2012-12-01

A new record of sea surface temperature (SST) for climate applications is described. This record provides independent corroboration of global variations estimated from SST measurements made in situ. Infrared imagery from Along-Track Scanning Radiometers (ATSRs) is used to create a 20 year time series of SST at 0.1° latitude-longitude resolution, in the ATSR Reprocessing for Climate (ARC) project. A very high degree of independence of in situ measurements is achieved via physics-based techniques. Skin SST and SST estimated for 20 cm depth are provided, with grid cell uncertainty estimates. Comparison with in situ data sets establishes that ARC SSTs generally have bias of order 0.1 K or smaller. The precision of the ARC SSTs is 0.14 K during 2003 to 2009, from three-way error analysis. Over the period 1994 to 2010, ARC SSTs are stable, with better than 95% confidence, to within 0.005 K yr-1(demonstrated for tropical regions). The data set appears useful for cleanly quantifying interannual variability in SST and major SST anomalies. The ARC SST global anomaly time series is compared to the in situ-based Hadley Centre SST data set version 3 (HadSST3). Within known uncertainties in bias adjustments applied to in situ measurements, the independent ARC record and HadSST3 present the same variations in global marine temperature since 1996. Since the in situ observing system evolved significantly in its mix of measurement platforms and techniques over this period, ARC SSTs provide an important corroboration that HadSST3 accurately represents recent variability and change in this essential climate variable.

Large-scale high-resolution scanning Hall probe microscope used for MgB2 filament characterization

International Nuclear Information System (INIS)

Cambel, V; Fedor, J; Gregusova, D; Kovac, P; Husek, I

2005-01-01

The scanning Hall probe microscope (SHPM) is an important imaging tool used for detailed studies of superconductors in basic science as well as in the industrial sector. It can be used for the studies of losses, current distribution, and effects at grain boundaries. However, only a few SHPMs for magnetic field imaging at temperatures below 77 K have been proposed up to now, most of them designed for small-area (∼10x10 μm 2 ) scanning. We present a large-scale low-temperature SHPM developed for imaging the entire magnetic field in close proximity to magnetic and superconducting samples at 4.2-300 K. The microscope combines a large scanned area and high spatial and magnetic field resolution. The instrument is designed as an insert of standard helium flowing cryostats. The Hall sensor scans an area up to 7 x 25 mm 2 in the whole temperature interval with a spatial resolution better than 5 μm. The presented system is used for the study of ex situ prepared MgB 2 filament. We show that external magnetic field induces local supercurrents in the MgB 2 , from which the critical current can be estimated. Moreover, it indicates the microstructure and space homogeneity of the superconductor

Low temperature ultrahigh vacuum cross-sectional scanning tunneling microscope for luminescence measurements

International Nuclear Information System (INIS)

Khang, Yoonho; Park, Yeonjoon; Salmeron, Miquel; Weber, Eicke R.

1999-01-01

We have constructed a scanning tunneling microscope with simultaneous light collection capabilities in order to investigate the opto-electronic properties of semiconductors. The microscope has in situ sample cleavage mechanism for cross-sectional sample. In order to reach low temperature (4 K), we used a specially designed cryostat. The efficiency of light collection generated in the tip-surface junction was greatly improved by use of a small parabolic mirror with the tip located at its focal point. (c) 1999 American Institute of Physics

In Situ Apparatus to Study Gas-Metal Reactions and Wettability at High Temperatures for Hot-Dip Galvanizing Applications

Science.gov (United States)

Koltsov, A.; Cornu, M.-J.; Scheid, J.

2018-02-01

The understanding of gas-metal reactions and related surface wettability at high temperatures is often limited due to the lack of in situ surface characterization. Ex situ transfers at low temperature between annealing furnace, wettability device, and analytical tools induce noticeable changes of surface composition distinct from the reality of the phenomena.Therefore, a high temperature wettability device was designed in order to allow in situ sample surface characterization by x-rays photoelectron spectroscopy after gas/metal and liquid metal/solid metal surface reactions. Such airless characterization rules out any contamination and oxidation of surfaces and reveals their real composition after heat treatment and chemical reaction. The device consists of two connected reactors, respectively, dedicated to annealing treatments and wettability measurements. Heat treatments are performed in an infrared lamp furnace in a well-controlled atmosphere conditions designed to reproduce gas-metal reactions occurring during the industrial recrystallization annealing of steels. Wetting experiments are carried out in dispensed drop configuration with the precise control of the deposited droplets kinetic energies. The spreading of drops is followed by a high-speed CCD video camera at 500-2000 frames/s in order to reach information at very low contact time. First trials have started to simulate phenomena occurring during recrystallization annealing and hot-dip galvanizing on polished pure Fe and FeAl8 wt.% samples. The results demonstrate real surface chemistry of steel samples after annealing when they are put in contact with liquid zinc alloy bath during hot-dip galvanizing. The wetting results are compared to literature data and coupled with the characterization of interfacial layers by FEG-Auger. It is fair to conclude that the results show the real interest of such in situ experimental setup for interfacial chemistry studies.

Preparation and Loading Process of Single Crystalline Samples into a Gas Environmental Cell Holder for In Situ Atomic Resolution Scanning Transmission Electron Microscopic Observation.

Science.gov (United States)

Straubinger, Rainer; Beyer, Andreas; Volz, Kerstin

2016-06-01

A reproducible way to transfer a single crystalline sample into a gas environmental cell holder for in situ transmission electron microscopic (TEM) analysis is shown in this study. As in situ holders have only single-tilt capability, it is necessary to prepare the sample precisely along a specific zone axis. This can be achieved by a very accurate focused ion beam lift-out preparation. We show a step-by-step procedure to prepare the sample and transfer it into the gas environmental cell. The sample material is a GaP/Ga(NAsP)/GaP multi-quantum well structure on Si. Scanning TEM observations prove that it is possible to achieve atomic resolution at very high temperatures in a nitrogen environment of 100,000 Pa.

Developments in Scanning Hall Probe Microscopy

Science.gov (United States)

Chouinard, Taras; Chu, Ricky; David, Nigel; Broun, David

2009-05-01

Low temperature scanning Hall probe microscopy is a sensitive means of imaging magnetic structures with high spatial resolution and magnetic flux sensitivity approaching that of a Superconducting Quantum Interference Device. We have developed a scanning Hall probe microscope with novel features, including highly reliable coarse positioning, in situ optimization of sensor-sample alignment and capacitive transducers for linear, long range positioning measurement. This has been motivated by the need to reposition accurately above fabricated nanostructures such as small superconducting rings. Details of the design and performance will be presented as well as recent progress towards time-resolved measurements with sub nanosecond resolution.

Fast-scanning heterodyne receiver for measurement of the electron cyclotron emission from high-temperature plasmas

International Nuclear Information System (INIS)

Efthimion, P.C.; Arunasalam, V.; Bitzer, R.; Campbell, L.; Hosea, J.C.

1979-03-01

A fast-scanning heterodyne receiver was developed that measures the fundamental cyclotron emission from the PLT plasma and thus ascertains the time evolution of the electron temperature profile. The receiver scans 60 to 90 GHz every 10 milliseconds and is interfaced to a computer for completely automated calibrated temperature measurements

In-situ continuous scanning high efficiency particulate air (HEPA) filter monitoring system

International Nuclear Information System (INIS)

Kirchner, K.N.; Johnson, C.M.; Lucerna, J.J.; Barnett, R.L.

1985-01-01

The testing and replacement of HEPA filters, which are widely used in the nuclear industry to purify process air before it is ventilated to the atmosphere, is a costly and labor-intensive undertaking. Current methods of testing filter performance, such as differential pressure measurement and scanning air monitoring, allow for determination of overall filter performance but preclude detection of symptoms of incipient filter failure, such as small holes in the filters themselves. Using current technology, a continual in-situ monitoring system has been designed which provides three major improvements over current methods of filter testing and replacement. This system (1) realizes a cost savings by reducing the number of intact filters which are currently being replaced unnecessarily, (2) provides a more accurate and quantitative measurement of filter performance than is currently achieved with existing testing methods, and (3) reduces personnel exposure to a radioactive environment by automatically performing most testing operations. The operation and performance of the HEPA filter monitoring system are discussed

High temperature conductance mapping for correlation of electrical properties with micron-sized chemical and microstructural features

Energy Technology Data Exchange (ETDEWEB)

Hansen, Karin Vels, E-mail: karv@dtu.dk [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, DK-4000 Roskilde (Denmark); Norrman, Kion [Department of Energy Conversion and Storage, Technical University of Denmark, Frederiksborgvej 399, DK-4000 Roskilde (Denmark); Jacobsen, Torben [Department of Chemistry, Technical University of Denmark, Kemitorvet Building 207, DK-2800 Lyngby (Denmark)

2016-11-15

High temperature AC conductance mapping is a scanning probe technique for resolving local electrical properties in microscopic areas. It is especially suited for detecting poorly conducting phases and for ionically conducting materials such as those used in solid oxide electrochemical cells. Secondary silicate phases formed at the edge of lanthanum strontium manganite microelectrodes are used as an example for correlation of chemical, microstructural and electrical properties with a spatial resolution of 1–2 µm to demonstrate the technique. The measurements are performed in situ in a controlled atmosphere high temperature scanning probe microscope at 650 °C in air. - Highlights: • A high temperature SPM technique for conductance measurements was developed. • Two examples from microelectrodes were used for demonstration. • Conductance mapping at 650 °C revealed poorly conducting secondary phases. • The secondary phases could be correlated with microstructure and chemistry.

In situ X-ray ptychography imaging of high-temperature CO2 acceptor particle agglomerates

DEFF Research Database (Denmark)

Høydalsvik, Kristin; Fløystad, Jostein Bø; Zhao, Tiejun

2014-01-01

be used for in situ phase contrast imaging in structure studies at atmospheric pressure and elevated temperatures. Lithium zirconate, a candidate CO2 capture material, was studied at a pressure of one atmosphere in air and in CO2, at temperatures exceeding 600 °C. Images with a spatial resolution better...

Low-temperature growth of polycrystalline Ge thin film on glass by in situ deposition and ex situ solid-phase crystallization for photovoltaic applications

International Nuclear Information System (INIS)

Tsao, Chao-Yang; Weber, Juergen W.; Campbell, Patrick; Widenborg, Per I.; Song, Dengyuan; Green, Martin A.

2009-01-01

Poly-crystalline germanium (poly-Ge) thin films have potential for lowering the manufacturing cost of photovoltaic devices especially in tandem solar cells, but high crystalline quality would be required. This work investigates the crystallinity of sputtered Ge thin films on glass prepared by in situ growth and ex situ solid-phase crystallization (SPC). Structural properties of the films were characterized by Raman, X-ray diffraction and ultraviolet-visible reflectance measurements. The results show the transition temperature from amorphous to polycrystalline is between 255 deg. C and 280 deg. C for in situ grown poly-Ge films, whereas the transition temperature is between 400 deg. C and 500 deg. C for films produced by SPC for a 20 h annealing time. The in situ growth in situ crystallized poly-Ge films at 450 deg. C exhibit significantly better crystalline quality than those formed by solid-phase crystallization at 600 deg. C. High crystalline quality at low substrate temperature obtained in this work suggests the poly-Ge films could be promising for use in thin film solar cells on glass.

In-situ electrochemical study of Zr1nb alloy corrosion in high temperature Li{sup +} containing water

Energy Technology Data Exchange (ETDEWEB)

Krausová, Aneta [University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Macák, Jan, E-mail: macakj@vscht.cz [University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Sajdl, Petr [University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Novotný, Radek [JRC-IET, Westerduinveg 3, 1755 LE Petten (Netherlands); Renčiuková, Veronika [University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Vrtílková, Věra [ÚJP a.s., Nad Kamínkou 1345, 156 10 Prague 5 (Czech Republic)

2015-12-15

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{sup +}) 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. - Highlights: • Zr1Nb alloy was tested in WWER coolant and in LiOH solutions at 280 °C. • Corrosion rates were estimated in-situ from electrochemical data. • Electrochemical data agreed well with weight gains and metallography data. • Increase of corrosion rate in LiOH appeared after short exposure (300–500 h). • Very high donor densities (1.1–1.2 × 10{sup 20} cm{sup −3}) of Zr oxide grown in LiOH were found.

Studies of superconductors using a low-temperature, high-field scanning tunneling microscope

International Nuclear Information System (INIS)

Kirtley, J.R.; Feenstra, R.M.; Fein, A.P.

1988-01-01

We have developed a scanning tunneling microscope (STM) capable of operating at temperatures as low as 0.4 K and fields as high as 8 T. We have used this STM to study the energy gap of the high-T/sub c/ superconductors La--Sr--Cu--O and Y--Ba--Cu--O. We find that the reduced gap for these oxide superconductors falls in the range 3<2Δ/k/sub B/T/sub c/<7, for polycrystalline, single-crystal, and thin-film samples. We have also simultaneously imaged the surface topography and superconducting energy gap for thin films of the granular superconductor NbN. We occasionally see regions with smaller best-fit gaps that correlate with surface topographical features, but have been unable so far to image flux vortices

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

Science.gov (United States)

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

2016-08-31

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

In Situ Scanning Probe Microscopy and New Perspectives in Analytical Chemistry

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Zhang, Jingdong; Chi, Qijin

1999-01-01

The resolution of scanning probe microscopies is unpresedented but the techniques are fraught with limitations as analytical tools. These limitations and their relationship to the physical mechanisms of image contrast are first discussed. Some new options based on in situ STM, which hold prospect...

Surface polymerization of (3,4-ethylenedioxythiophene) probed by in situ scanning tunneling microscopy on Au(111) in ionic liquids.

Science.gov (United States)

Ahmad, Shahzada; Carstens, Timo; Berger, Rüdiger; Butt, Hans-Jürgen; Endres, Frank

2011-01-01

The electropolymerization of 3,4-ethylenedioxythiophene (EDOT) to poly(3,4-ethylenedioxythiophene) (PEDOT) was investigated in the air and water-stable ionic liquids 1-hexyl-3-methylimidazolium tris(pentafluoroethyl) trifluorophosphate [HMIm]FAP and 1-ethyl-3-methylimidazolium bis(trifluoromethylsulfonyl) amide [EMIm]TFSA. In situ scanning tunnelling microscopy (STM) results show that the electropolymerization of EDOT in the ionic liquid can be probed on the nanoscale. In contrast to present understanding, it was observed that the EDOT can be oxidised in ionic liquids well below its oxidation potential and the under potential growth of polymer was visualized by in situ STM. These results serve as the first study to confirm the under potential growth of conducting polymers in ionic liquids. Furthermore, ex situ microscopy measurements were performed. Quite a high current of 670 nA was observed on the nanoscale by conductive scanning force microscopy (CSFM).

Covalently Immobilised Cytochrome C Imaged by In Situ Scanning Tunnelling Microscopy

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Olesen, Klaus G.; Danilov, Alexey I.

1997-01-01

In situ scanning tunnelling microscopy (STM) imaging of cytochrome c (cyt c) on polycrystalline Pt surfaces and on Au(lll) was achieved first by covalent immobilisation of 3-aminopropyltriethoxysilane (3-APTS) brought to react with oxide present on the Pt surfaces. Covalently bound 3-APTS forms...

Cluster tool for in situ processing and comprehensive characteriza tion of thin films at high temperatures.

Science.gov (United States)

Wenisch, Robert; Lungwitz, Frank; Hanf, Daniel; Heller, Rene; Zscharschuch, Jens; Hübner, René; von Borany, Johannes; Abrasonis, Gintautas; Gemming, Sibylle; Escobar-Galindo, Ramon; Krause, Matthias

2018-05-31

A new cluster tool for in situ real-time processing and depth-resolved compositional, structural and optical characterization of thin films at temperatures from -100 to 800 °C is described. The implemented techniques comprise magnetron sputtering, ion irradiation, Rutherford backscattering spectrometry, Raman spectroscopy and spectroscopic ellipsometry. The capability of the cluster tool is demonstrated for a layer stack MgO/ amorphous Si (~60 nm)/ Ag (~30 nm), deposited at room temperature and crystallized with partial layer exchange by heating up to 650°C. Its initial and final composition, stacking order and structure were monitored in situ in real time and a reaction progress was defined as a function of time and temperature.

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope.

Science.gov (United States)

Fang, Yurui; Zhang, Zhenglong; Sun, Mengtao

2016-03-01

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10(-7) Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 × 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.

High vacuum tip-enhanced Raman spectroscope based on a scanning tunneling microscope

Energy Technology Data Exchange (ETDEWEB)

Fang, Yurui [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, P. O. Box 603-146, Beijing 100190 (China); Bionanophotonics, Department of Applied Physics, Chalmers University of Technology, Göteborg, SE 41296 (Sweden); Zhang, Zhenglong [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, P. O. Box 603-146, Beijing 100190 (China); School of Physics and Information Technology, Shaanxi Normal University, 710062 Xi’an (China); Leibniz Institute of Photonic Technology, Albert-Einstein-Str. 9, 07745 Jena (Germany); Sun, Mengtao, E-mail: mtsun@iphy.ac.cn [Beijing National Laboratory for Condensed Matter Physics, Institute of Physics, Chinese Academy of Sciences, P. O. Box 603-146, Beijing 100190 (China)

2016-03-15

In this paper, we present the construction of a high-vacuum tip-enhanced Raman spectroscopy (HV-TERS) system that allows in situ sample preparation and measurement. A detailed description of the prototype instrument is presented with experimental validation of its use and novel ex situ experimental results using the HV-TERS system. The HV-TERS system includes three chambers held under a 10{sup −7} Pa vacuum. The three chambers are an analysis chamber, a sample preparation chamber, and a fast loading chamber. The analysis chamber is the core chamber and contains a scanning tunneling microscope (STM) and a Raman detector coupled with a 50 × 0.5 numerical aperture objective. The sample preparation chamber is used to produce single-crystalline metal and sub-monolayer molecular films by molecular beam epitaxy. The fast loading chamber allows ex situ preparation of samples for HV-TERS analysis. Atomic resolution can be achieved by the STM on highly ordered pyrolytic graphite. We demonstrate the measurement of localized temperature using the Stokes and anti-Stokes TERS signals from a monolayer of 1,2-benzenedithiol on a gold film using a gold tip. Additionally, plasmonic catalysis can be monitored label-free at the nanoscale using our device. Moreover, the HV-TERS experiments show simultaneously activated infrared and Raman vibrational modes, Fermi resonance, and some other non-linear effects that are not observed in atmospheric TERS experiments. The high spatial and spectral resolution and pure environment of high vacuum are beneficial for basic surface studies.

A variable-temperature scanning tunneling microscope capable of single-molecule vibrational spectroscopy

International Nuclear Information System (INIS)

Stipe, B.C.; Rezaei, M.A.; Ho, W.

1999-01-01

The design and performance of a variable-temperature scanning tunneling microscope (STM) is presented. The microscope operates from 8 to 350 K in ultrahigh vacuum. The thermally compensated STM is suspended by springs from the cold tip of a continuous flow cryostat and is completely surrounded by two radiation shields. The design allows for in situ dosing and irradiation of the sample as well as for the exchange of samples and STM tips. With the STM feedback loop off, the drift of the tip-sample spacing is approximately 0.001 Angstrom/min at 8 K. It is demonstrated that the STM is well-suited for the study of atomic-scale chemistry over a wide temperature range, for atomic-scale manipulation, and for single-molecule inelastic electron tunneling spectroscopy (IETS). copyright 1999 American Institute of Physics

Miniature Variable Pressure Scanning Electron Microscope for In-Situ Imaging and Chemical Analysis

Science.gov (United States)

Gaskin, Jessica A.; Jerman, Gregory; Gregory, Don; Sampson, Allen R.

2012-01-01

NASA Marshall Space Flight Center (MSFC) is leading an effort to develop a Miniaturized Variable Pressure Scanning Electron Microscope (MVP-SEM) for in-situ imaging and chemical analysis of uncoated samples. This instrument development will be geared towards operation on Mars and builds on a previous MSFC design of a mini-SEM for the moon (funded through the NASA Planetary Instrument Definition and Development Program). Because Mars has a dramatically different environment than the moon, modifications to the MSFC lunar mini-SEM are necessary. Mainly, the higher atmospheric pressure calls for the use of an electron gun that can operate at High Vacuum, rather than Ultra-High Vacuum. The presence of a CO2-rich atmosphere also allows for the incorporation of a variable pressure system that enables the in-situ analysis of nonconductive geological specimens. Preliminary testing of Mars meteorites in a commercial Environmental SEM(Tradmark) (FEI) confirms the usefulness of lowcurrent/low-accelerating voltage imaging and highlights the advantages of using the Mars atmosphere for environmental imaging. The unique capabilities of the MVP-SEM make it an ideal tool for pursuing key scientific goals of NASA's Flagship Mission Max-C; to perform in-situ science and collect and cache samples in preparation for sample return from Mars.

In situ repair of bone and cartilage defects using 3D scanning and 3D printing.

Science.gov (United States)

Li, Lan; Yu, Fei; Shi, Jianping; Shen, Sheng; Teng, Huajian; Yang, Jiquan; Wang, Xingsong; Jiang, Qing

2017-08-25

Three-dimensional (3D) printing is a rapidly emerging technology that promises to transform tissue engineering into a commercially successful biomedical industry. However, the use of robotic bioprinters alone is not sufficient for disease treatment. This study aimed to report the combined application of 3D scanning and 3D printing for treating bone and cartilage defects. Three different kinds of defect models were created to mimic three orthopedic diseases: large segmental defects of long bones, free-form fracture of femoral condyle, and International Cartilage Repair Society grade IV chondral lesion. Feasibility of in situ 3D bioprinting for these diseases was explored. The 3D digital models of samples with defects and corresponding healthy parts were obtained using high-resolution 3D scanning. The Boolean operation was used to achieve the shape of the defects, and then the target geometries were imported in a 3D bioprinter. Two kinds of photopolymerized hydrogels were synthesized as bioinks. Finally, the defects of bone and cartilage were restored perfectly in situ using 3D bioprinting. The results of this study suggested that 3D scanning and 3D bioprinting could provide another strategy for tissue engineering and regenerative medicine.

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

Science.gov (United States)

Kawamura, Kunio; Nagayoshi, Hiroki; Yao, Toshio

2010-05-14

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

Nanoparticle Metamorphosis: An in Situ High-Temperature Transmission Electron Microscopy Study of the Structural Evolution of Heterogeneous Au:Fe 2 O 3 Nanoparticles

KAUST Repository

Baumgardner, William J.

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. © 2014 American Chemical Society.

Nanoparticle Metamorphosis: An in Situ High-Temperature Transmission Electron Microscopy Study of the Structural Evolution of Heterogeneous Au:Fe 2 O 3 Nanoparticles

KAUST Repository

Baumgardner, William J.; Yu, Yingchao; Hovden, Robert; Honrao, Shreyas; Hennig, Richard G.; Abruñ a, Hé ctor D.; Muller, David; Hanrath, Tobias

2014-01-01

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. © 2014 American Chemical Society.

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

Energy Technology Data Exchange (ETDEWEB)

Xiao, Hai [Missouri Univ. of Science and Technology, Rolla, MO (United States); Dong, Junhang [Univ. of Cincinnati, OH (United States); Lin, Jerry [Arizona State Univ., Tempe, AZ (United States); Romero, Van [New Mexico Institute of Mining and Technology, Socorro, NM (United States)

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.

Fluorescence in situ hybridization on human metaphase chromosomes detected by near-field scanning optical microscopy

NARCIS (Netherlands)

Moers, M.H.P.; Moers, M.H.P.; Kalle, W.H.J.; Kalle, W.H.J.; Ruiter, A.G.T.; Wiegant, J.C.A.G.; Raap, A.K.; Greve, Jan; de Grooth, B.G.; van Hulst, N.F.

1996-01-01

Fluorescence in situ hybridization o­n human metaphase chromosomes is detected by near-field scanning optical microscopy. This combination of cytochemical and scanning probe techniques enables the localization and identification of several fluorescently labelled genomic DNA fragments o­n a single

In-situ Crystallization of Highly Volatile Commercial Mold Flux Using an Isolated Observation System in the Confocal Laser Scanning Microscope

Science.gov (United States)

Park, Jun-Yong; Ryu, Jae Wook; Sohn, Il

2014-08-01

The in situ crystallization behavior of highly volatile commercial mold fluxes for medium carbon steels was investigated using the confocal laser scanning microscope (CLSM) equipped with an optimized isolated observation system. The highly volatile compounds of the mold flux were suppressed during heating allowing direct observation in the CLSM. Cooling rates of 25, 50, 100, 400, and 800 K/min were incorporated and continuous cooling transformation (CCT) diagrams of 4 different commercial mold fluxes for medium carbon steels were developed. Identification of the crystalline phase was conducted with XRD and SEM-EDS analysis. A cuspidine crystalline was observed in all samples at various cooling rates. With higher basicity, CaF2, and NaF, the crystallization of the fluxes was enhanced according to the CCT diagram. As the slag structure becomes depolymerized, the diffusion rate of the cathodic ions seems to increase.

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

Directory of Open Access Journals (Sweden)

Margaret McCaul

2016-08-01

Full Text Available 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.

Report on the Installation and Preparedness of a Protochips Fusion in-situ Heating Holder for TEM

Energy Technology Data Exchange (ETDEWEB)

Edmondson, Philip D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2017-03-01

This brief report documents the procurement and installation of a Protochips Fusion (formerly Aduro) high-temperature, high stability transmission electron microscopy (TEM) specimen holder that allows for the high spatial resolution characterization of material specimens at high temperature in situ of an electron microscope. This specimen holder was specifically procured for use with The FEI Talos F200X Scanning/Transmission Electron Microscope (STEM) in Oak Ridge National Laboratory’s (ORNL’s) Low Activation Materials Development and Analysis (LAMDA) Laboratory. The Protochips Fusion holder will enable high-resolution structural and chemical analysis of irradiated materials at high temperature, becoming a unique capability worldwide, and would encourage high-quality in situ experiments to be conducted on irradiated materials.

Spectral and raw quasi in-situ energy dispersive X-ray data captured via a TEM analysis of an ODS austenitic stainless steel sample under 1 MeV Kr2+ high temperature irradiation.

Science.gov (United States)

Brooks, Adam J; Yao, Zhongwen

2017-10-01

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

A study on the phase transformation of the nanosized hydroxyapatite synthesized by hydrolysis using in situ high temperature X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Shih, W.-J. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan, 70101, Taiwan (China); Wang, J.-W. [Department of Enviromental and Safety Engineering, Chung Hwa College of Medical Technology, 89 Wen-Hua 1st St., Rende Shiang, Tainan, 71703, Taiwan (China); Wang, M.-C. [Department of Materials Science and Engineering, National United University, 1 Lien-Da, Kung-Ching Li, Miao Li 360, Taiwan (China)]. E-mail: mcwang@nuu.edu.tw; Hon, M.-H. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan, 70101, Taiwan (China); Dayeh University, 112 Shan-Jiau Road, Da-Tsuen, Changhua 515, Taiwan (China)

2006-09-15

The biodegradable hydroxyapatite (HA) was synthesized by hydrolysis and characterized using high temperature X-ray diffraction (HT-XRD), differential thermal analysis and thermogravimetry (DTA/TG), and scanning electron microscopy (SEM). The in situ phase transformation of the HA synthesized from CaHPO{sub 4}.2H{sub 2}O (DCPD) and CaCO{sub 3} with a Ca / P = 1.5 in 2.5 M NaOH{sub (aq)} at 75 deg. C for 1 h was investigated by HT-XRD between 25 and 1500 deg. C. The HA was crystallized at 600 deg. C and maintained as the major phase until 1400 deg. C. The HA steadily transformed to the {alpha}-tricalcium phosphate ({alpha}-TCP) which became the major phosphate phase at 1500 deg. C. At 700 deg. C, the minor CaO phase appeared and vanished at 1300 deg. C. The Na{sup +} impurity from the hydrolysis process was responsible for the formation of the NaCaPO{sub 4} phase, which appeared above 800 deg. C and disappeared at 1200 deg. C.

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

Science.gov (United States)

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

2017-04-01

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

An ultra-high vacuum scanning tunneling microscope operating at sub-Kelvin temperatures and high magnetic fields for spin-resolved measurements

Science.gov (United States)

Salazar, C.; Baumann, D.; Hänke, T.; Scheffler, M.; Kühne, T.; Kaiser, M.; Voigtländer, R.; Lindackers, D.; Büchner, B.; Hess, C.

2018-06-01

We present the construction and performance of an ultra-low-temperature scanning tunneling microscope (STM), working in ultra-high vacuum (UHV) conditions and in high magnetic fields up to 9 T. The cryogenic environment of the STM is generated by a single-shot 3He magnet cryostat in combination with a 4He dewar system. At a base temperature (300 mK), the cryostat has an operation time of approximately 80 h. The special design of the microscope allows the transfer of the STM head from the cryostat to a UHV chamber system, where samples and STM tips can be easily exchanged. The UHV chambers are equipped with specific surface science treatment tools for the functionalization of samples and tips, including high-temperature treatments and thin film deposition. This, in particular, enables spin-resolved tunneling measurements. We present test measurements using well-known samples and tips based on superconductors and metallic materials such as LiFeAs, Nb, Fe, and W. The measurements demonstrate the outstanding performance of the STM with high spatial and energy resolution as well as the spin-resolved capability.

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

Science.gov (United States)

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 (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.

High-pressure differential scanning microcalorimeter.

Science.gov (United States)

Senin, A A; Dzhavadov, L N; Potekhin, S A

2016-03-01

A differential scanning microcalorimeter for studying thermotropic conformational transitions of biopolymers at high pressure has been designed. The calorimeter allows taking measurements of partial heat capacity of biopolymer solutions vs. temperature at pressures up to 3000 atm. The principles of operation of the device, methods of its calibration, as well as possible applications are discussed.

Structure of spinel at high temperature using in-situ XANES study at the Al and Mg K-edge

Energy Technology Data Exchange (ETDEWEB)

Ligny, D de [Universite Claude Bernard Lyon 1, LPCML, 69622 Villeurbanne (France); Neuville, D R [Physique des Mineraux et Magmas, Geochimie-Cosmochimie, CNRS-IPGP, 4 place Jussieu, 75005 Paris (France); Flank, A-M; Lagarde, P, E-mail: deligny@pcml.univ-lyon1.f [Synchrotron SOLEIL, L' Orme des Merisiers, Saint Aubin, 91192 France (France)

2009-11-15

We present structural information obtained on spinel at high temperature (298-2400 K) using in situ XANES at the Mg and Al K-edge. Spinel, {sup [4]}(Al{sub x},Mg{sub 1-x}){sup [6]}(Al{sub 2-x},Mg{sub x})O{sub 4}, with increasing temperature, show a substitution of Mg by Al and Al by Mg in their respective sites. This substitution corresponds to an inversion of the Mg and Al sites. Furthermore, both experiments at the Al and Mg K-edges are in good agreement with XANES calculation made using FDMNES code.

In situ scanning probe spectroscopy at nanoscale solid/liquid interfaces

International Nuclear Information System (INIS)

Schindler, W.; Hugelmann, M.; Hugelmann, Ph.

2005-01-01

Electrochemistry provides unique features for the preparation of low-dimensional structures, but in situ spectroscopy with atomic/molecular resolution at such structures is at present not well established yet. This paper shows that in situ scanning probe spectroscopy at solid/liquid interfaces can be utilized to study electronic properties at nanoscale, if appropriate conditions are applied. Tunneling spectroscopy provides information about tunneling barrier heights and electronic states in the tunneling gap, as shown on Au(1 1 1) substrates, contact spectroscopy allows for transport measurements at single nanostructures, as shown at Au/n-Si(1 1 1) nanodiodes. The influence of the electrolytic environment on spectroscopic investigations is not a principal limitation, but offers additional degrees of freedom, which allow, for example, spectroscopic studies of potential dependent surface phenomena at solid/liquid interfaces

In Situ formation of pentafluorophosphate benzimidazole anion stabilizes high-temperature performance of lithium-ion batteries

International Nuclear Information System (INIS)

Pradanawati, Sylvia Ayu; Wang, Fu-Ming; Rick, John

2014-01-01

Highlights: • A new pentafluorophosphate benzimidazole anion was formed by Lewis acid-base reaction. • This pentafluorophosphate benzimidazole anion is fabricated with the benzimidazole anion and PF 5 . • This pentafluorophosphate benzimidazole anion avoids the ominous side reactions that PF 5 reacts SEI to form LiF and HF at high temperature. • The additional pentafluorophosphate benzimidazole anion formation well maintains the battery performance at 60 °C measurement compares to the electrolyte only with contains the salt, LiPF 6 . - Abstract: Lithium salts play a critical role in initiating electrochemical reactions in Li-ion batteries. Single Li ions dissociate from bulk-salt and associate with carbonates to form a solid electrolyte interface (SEI) during the first charge-discharge of the battery. SEI formation and the chemical stability of salt must both be controlled and optimized to minimize irreversible reactions in SEI formation and to suppress the decomposition of the salt at high temperatures. This study synthesizes a new benzimidazole-based anion in the electrolyte. This anion, pentafluorophosphate benzimidazole, results from a Lewis acid-base reaction between the benzimidazole anion and PF 5 . The new pentafluorophosphate benzimidazole anion inhibits the decomposition of LiPF 6 by inhibiting PF 5 side reactions, which degrade the SEI, and lead to the formation of LiF and HF at high temperatures. In addition, the use of the pentafluorophosphate benzimidazole anion results in the formation of a modified SEI that is able to modify the battery's performance. Cyclic voltammetry, scanning electron microscopy, differential scanning calorimetry, electrochemical impedance spectroscopy, as well as charge-discharge and X-ray photoelectron spectroscopy measurements have been used to characterize the materials in this study. The formation of the pentafluorophosphate benzimidazole anion in the electrolyte caused a 14% decrease in the activation energy

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

Energy Technology Data Exchange (ETDEWEB)

Rahman, Md Taibur; McCloy, John; Panat, Rahul, E-mail: rahul.panat@wsu.edu, E-mail: rvchintalapalle@utep.edu [School of Mechanical and Materials Engineering, Washington State University, Pullman, Washington 99163 (United States); Ramana, C. V., E-mail: rahul.panat@wsu.edu, E-mail: rvchintalapalle@utep.edu [Department of Mechanical Engineering, University of Texas at El Paso, El Paso, Texas 79968 (United States)

2016-08-21

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

International Nuclear Information System (INIS)

Rahman, Md Taibur; McCloy, John; Panat, Rahul; Ramana, C. V.

2016-01-01

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24–500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

Structure, electrical characteristics, and high-temperature stability of aerosol jet printed silver nanoparticle films

Science.gov (United States)

Rahman, Md Taibur; McCloy, John; Ramana, C. V.; Panat, Rahul

2016-08-01

Printed electronics has emerged as a versatile eco-friendly fabrication technique to create sintered nanoparticle (NP) films on arbitrary surfaces with an excellent control over the film microstructure. While applicability of such films for high-temperature applications is not explored previously, herein we report the high-temperature electrical stability of silver (Ag) metal NP films fabricated using an Aerosol Jet based printing technique and demonstrate that this behavior is dictated by changes in the film microstructure. In-situ high temperature (24-500 °C) impedance spectroscopy measurements show that the real part of the impedance increases with increasing temperature up to 150 °C, at which point a decreasing trend prevails until 300 °C, followed again by an increase in impedance. The electrical behavior is correlated with the in-situ grain growth of the Ag NP films, as observed afterwards by scanning electron microscopy and X-ray diffraction (XRD), and could be tailored by controlling the initial microstructure through sintering conditions. Using combined diffraction and spectroscopic analytical methods, it is demonstrated the Aerosol Jet printed Ag NP films exhibit enhanced thermal stability and oxidation resistance. In addition to establishing the conditions for stability of Ag NP films, the results provide a fundamental understanding of the effect of grain growth and reduction in grain boundary area on the electrical stability of sintered NP films.

Development of in situ Brillouin spectroscopy at high pressure and high temperature with synchrotron radiation and infrared laser heating system: Application to the Earth's deep interior

Science.gov (United States)

Murakami, Motohiko; Asahara, Yuki; Ohishi, Yasuo; Hirao, Naohisa; Hirose, Kei

2009-05-01

Seismic wave velocity profiles in the Earth provide one of the strongest constraints on structure, mineralogy and elastic properties of the Earth's deep interior. Accurate sound velocity data of deep Earth materials under relevant high-pressure and high-temperature conditions, therefore, are essential for interpretation of seismic data. Such information can be directly obtained from Brillouin scattering measurement. Here we describe an in situ Brillouin scattering system for measurements at high pressure and high temperature using a laser heated diamond anvil cell and synchrotron radiation for sample characterization. The system has been used with single-crystal and polycrystalline materials, and with glass and fluid phase. It provided high quality sound velocity and elastic data with X-ray diffraction data at high pressure and/or high temperature. Those combined techniques can potentially offer the essential information for resolving many remaining issues in mineral physics.

Miniaturized Environmental Scanning Electron Microscope for In Situ Planetary Studies

Science.gov (United States)

Gaskin, Jessica; Abbott, Terry; Medley, Stephanie; Gregory, Don; Thaisen, Kevin; Taylor , Lawrence; Ramsey, Brian; Jerman, Gregory; Sampson, Allen; Harvey, Ralph

2010-01-01

The exploration of remote planetary surfaces calls for the advancement of low power, highly-miniaturized instrumentation. Instruments of this nature that are capable of multiple types of analyses will prove to be particularly useful as we prepare for human return to the moon, and as we continue to explore increasingly remote locations in our Solar System. To this end, our group has been developing a miniaturized Environmental-Scanning Electron Microscope (mESEM) capable of remote investigations of mineralogical samples through in-situ topographical and chemical analysis on a fine scale. The functioning of an SEM is well known: an electron beam is focused to nanometer-scale onto a given sample where resulting emissions such as backscattered and secondary electrons, X-rays, and visible light are registered. Raster scanning the primary electron beam across the sample then gives a fine-scale image of the surface topography (texture), crystalline structure and orientation, with accompanying elemental composition. The flexibility in the types of measurements the mESEM is capable of, makes it ideally suited for a variety of applications. The mESEM is appropriate for use on multiple planetary surfaces, and for a variety of mission goals (from science to non-destructive analysis to ISRU). We will identify potential applications and range of potential uses related to planetary exploration. Over the past few of years we have initiated fabrication and testing of a proof-of-concept assembly, consisting of a cold-field-emission electron gun and custom high-voltage power supply, electrostatic electron-beam focusing column, and scanning-imaging electronics plus backscatter detector. Current project status will be discussed. This effort is funded through the NASA Research Opportunities in Space and Earth Sciences - Planetary Instrument Definition and Development Program.

A compact sub-Kelvin ultrahigh vacuum scanning tunneling microscope with high energy resolution and high stability.

Science.gov (United States)

Zhang, L; Miyamachi, T; Tomanić, T; Dehm, R; Wulfhekel, W

2011-10-01

We designed a scanning tunneling microscope working at sub-Kelvin temperatures in ultrahigh vacuum (UHV) in order to study the magnetic properties on the nanoscale. An entirely homebuilt three-stage cryostat is used to cool down the microscope head. The first stage is cooled with liquid nitrogen, the second stage with liquid (4)He. The third stage uses a closed-cycle Joule-Thomson refrigerator of a cooling power of 1 mW. A base temperature of 930 mK at the microscope head was achieved using expansion of (4)He, which can be reduced to ≈400 mK when using (3)He. The cryostat has a low liquid helium consumption of only 38 ml/h and standing times of up to 280 h. The fast cooling down of the samples (3 h) guarantees high sample throughput. Test experiments with a superconducting tip show a high energy resolution of 0.3 meV when performing scanning tunneling spectroscopy. The vertical stability of the tunnel junction is well below 1 pm (peak to peak) and the electric noise floor of tunneling current is about 6fA/√Hz. Atomic resolution with a tunneling current of 1 pA and 1 mV was achieved on Au(111). The lateral drift of the microscope at stable temperature is below 20 pm/h. A superconducting spilt-coil magnet allows to apply an out-of-plane magnetic field of up to 3 T at the sample surface. The flux vortices of a Nb(110) sample were clearly resolved in a map of differential conductance at 1.1 K and a magnetic field of 0.21 T. The setup is designed for in situ preparation of tip and samples under UHV condition.

High-bandwidth scanned-wavelength-modulation spectroscopy sensors for temperature and H2O in a rotating detonation engine

International Nuclear Information System (INIS)

Goldenstein, Christopher S; Almodóvar, Christopher A; Jeffries, Jay B; Hanson, Ronald K; Brophy, Christopher M

2014-01-01

The design and use of two-color tunable diode laser (TDL) absorption sensors for measurements of temperature and H 2 O in a rotating detonation engine (RDE) are presented. Both sensors used first-harmonic-normalized scanned-wavelength-modulation spectroscopy with second-harmonic detection (scanned-WMS-2f/1f) to account for non-absorbing transmission losses and emission encountered in the harsh combustion environment. One sensor used two near-infrared (NIR) TDLs near 1391.7 nm and 1469.3 nm that were modulated at 225 kHz and 285 kHz, respectively, and sinusoidally scanned across the peak of their respective H 2 O absorption transitions to provide a measurement rate of 50 kHz and a detection limit in the RDE of 0.2% H 2 O by mole. The other sensor used two mid-infrared (MIR) TDLs near 2551 nm and 2482 nm that were modulated at 90 kHz and 112 kHz, respectively, and sinusoidally scanned across the peak of their respective H 2 O transitions to provide a measurement rate of 10 kHz and a detection limit in the RDE of 0.02% H 2 O by mole. Four H 2 O absorption transitions with different lower-state energies were used to assess the homogeneity of temperature in the measurement plane. Experimentally derived spectroscopic parameters that enable temperature and H 2 O sensing to within 1.5–3.5% of known values are reported. The sensor design enabling the high-bandwidth scanned-WMS-2f/1f measurements is presented. The two sensors were deployed across two orthogonal and coplanar lines-of-sight (LOS) located in the throat of a converging-diverging nozzle at the RDE combustor exit. Measurements in the non-premixed H 2 -fueled RDE indicate that the temperature and H 2 O oscillate at the detonation frequency (≈3.25 kHz) and that production of H 2 O is a weak function of global equivalence ratio. (paper)

High-bandwidth scanned-wavelength-modulation spectroscopy sensors for temperature and H2O in a rotating detonation engine

Science.gov (United States)

Goldenstein, Christopher S.; Almodóvar, Christopher A.; Jeffries, Jay B.; Hanson, Ronald K.; Brophy, Christopher M.

2014-10-01

The design and use of two-color tunable diode laser (TDL) absorption sensors for measurements of temperature and H2O in a rotating detonation engine (RDE) are presented. Both sensors used first-harmonic-normalized scanned-wavelength-modulation spectroscopy with second-harmonic detection (scanned-WMS-2f/1f) to account for non-absorbing transmission losses and emission encountered in the harsh combustion environment. One sensor used two near-infrared (NIR) TDLs near 1391.7 nm and 1469.3 nm that were modulated at 225 kHz and 285 kHz, respectively, and sinusoidally scanned across the peak of their respective H2O absorption transitions to provide a measurement rate of 50 kHz and a detection limit in the RDE of 0.2% H2O by mole. The other sensor used two mid-infrared (MIR) TDLs near 2551 nm and 2482 nm that were modulated at 90 kHz and 112 kHz, respectively, and sinusoidally scanned across the peak of their respective H2O transitions to provide a measurement rate of 10 kHz and a detection limit in the RDE of 0.02% H2O by mole. Four H2O absorption transitions with different lower-state energies were used to assess the homogeneity of temperature in the measurement plane. Experimentally derived spectroscopic parameters that enable temperature and H2O sensing to within 1.5-3.5% of known values are reported. The sensor design enabling the high-bandwidth scanned-WMS-2f/1f measurements is presented. The two sensors were deployed across two orthogonal and coplanar lines-of-sight (LOS) located in the throat of a converging-diverging nozzle at the RDE combustor exit. Measurements in the non-premixed H2-fueled RDE indicate that the temperature and H2O oscillate at the detonation frequency (≈3.25 kHz) and that production of H2O is a weak function of global equivalence ratio.

Development of high temperature scanning electron microscopy and applications to sintering studies

International Nuclear Information System (INIS)

Wang, D.N.K.; Miller, D.J.; Fulrath, R.M.

1978-01-01

The densification and microstructural changes of a metallic and/or ceramic powder compact during sintering is a critically important but incompletely understood process. Whether solely in the solid state or in the presence of a liquid phase, mass transport occurs at elevated temperatures to eliminate porosity and reduce the surface energy of the system. Changes in specimen dimensions, particle shape and pore morphology, formation of liquid phases and other direct evidence of the sintering process have been observed and recorded at temperature using video tape and 16mm time lapse movies of the TV scanning image. Materials that have been examined at elevated temperature are Ni, glass, Al 2 O 3 , UO 2 , W, Cu, WC-Co, and CaF 2

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

Science.gov (United States)

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.

Coupling scanning tunneling microscope and supersonic molecular beams: a unique tool for in situ investigation of the morphology of activated systems.

Science.gov (United States)

Smerieri, M; Reichelt, R; Savio, L; Vattuone, L; Rocca, M

2012-09-01

We report here on a new experimental apparatus combining a commercial low temperature scanning tunneling microscope with a supersonic molecular beam. This setup provides a unique tool for the in situ investigation of the topography of activated adsorption systems and opens thus new interesting perspectives. It has been tested towards the formation of the O/Ag(110) added rows reconstruction and of their hydroxylation, comparing data recorded upon O(2) exposure at thermal and hyperthermal energies.

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

Directory of Open Access Journals (Sweden)

Pei-Chi Chen

2011-10-01

Full Text Available 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.

Isothermal Time-Temperature-Precipitation Diagram for an Aluminum Alloy 6005A by In Situ DSC Experiments

Directory of Open Access Journals (Sweden)

Benjamin Milkereit

2014-03-01

Full Text Available Time-temperature-precipitation (TTP diagrams deliver important material data, such as temperature and time ranges critical for precipitation during the quenching step of the age hardening procedure. Although the quenching step is continuous, isothermal TTP diagrams are often applied. Together with a so-called Quench Factor Analysis, they can be used to describe very different cooling paths. Typically, these diagrams are constructed based on mechanical properties or microstructures after an interrupted quenching, i.e., ex situ analyses. In recent years, an in situ calorimetric method to record continuous cooling precipitation diagrams of aluminum alloys has been developed to the application level by our group. This method has now been transferred to isothermal experiments, in which the whole heat treatment cycle was performed in a differential scanning calorimeter. The Al-Mg-Si-wrought alloy 6005A was investigated. Solution annealing at 540 °C and overcritical quenching to several temperatures between 450 °C and 250 °C were followed by isothermal soaking. Based on the heat flow curves during isothermal soaking, TTP diagrams were determined. An appropriate evaluation method has been developed. It was found that three different precipitation reactions in characteristic temperature intervals exist. Some of the low temperature reactions are not accessible in continuous cooling experiments and require isothermal studies.

Submolecular Electronic Mapping of Single Cysteine Molecules by in Situ Scanning Tunneling Imaging

DEFF Research Database (Denmark)

Zhang, Jingdong; Chi, Qijin; Nazmutdinov, R. R.

2009-01-01

We have used L-Cysteine (Cys) as a model system to study the surface electronic structures of single molecules at the submolecular level in aqueous buffer solution by a combination of electrochemical scanning tunneling microscopy (in situ STM), electrochemistry including voltammetry and chronocou...

A variable-temperature nanostencil compatible with a low-temperature scanning tunneling microscope/atomic force microscope

International Nuclear Information System (INIS)

Steurer, Wolfram; Gross, Leo; Schlittler, Reto R.; Meyer, Gerhard

2014-01-01

We describe a nanostencil lithography tool capable of operating at variable temperatures down to 30 K. The setup is compatible with a combined low-temperature scanning tunneling microscope/atomic force microscope located within the same ultra-high-vacuum apparatus. The lateral movement capability of the mask allows the patterning of complex structures. To demonstrate operational functionality of the tool and estimate temperature drift and blurring, we fabricated LiF and NaCl nanostructures on Cu(111) at 77 K

A variable-temperature nanostencil compatible with a low-temperature scanning tunneling microscope/atomic force microscope

Energy Technology Data Exchange (ETDEWEB)

Steurer, Wolfram, E-mail: wst@zurich.ibm.com; Gross, Leo; Schlittler, Reto R.; Meyer, Gerhard [IBM Research-Zurich, 8803 Rüschlikon (Switzerland)

2014-02-15

We describe a nanostencil lithography tool capable of operating at variable temperatures down to 30 K. The setup is compatible with a combined low-temperature scanning tunneling microscope/atomic force microscope located within the same ultra-high-vacuum apparatus. The lateral movement capability of the mask allows the patterning of complex structures. To demonstrate operational functionality of the tool and estimate temperature drift and blurring, we fabricated LiF and NaCl nanostructures on Cu(111) at 77 K.

A variable-temperature nanostencil compatible with a low-temperature scanning tunneling microscope/atomic force microscope.

Science.gov (United States)

Steurer, Wolfram; Gross, Leo; Schlittler, Reto R; Meyer, Gerhard

2014-02-01

We describe a nanostencil lithography tool capable of operating at variable temperatures down to 30 K. The setup is compatible with a combined low-temperature scanning tunneling microscope/atomic force microscope located within the same ultra-high-vacuum apparatus. The lateral movement capability of the mask allows the patterning of complex structures. To demonstrate operational functionality of the tool and estimate temperature drift and blurring, we fabricated LiF and NaCl nanostructures on Cu(111) at 77 K.

Development of in situ two-coil mutual inductance technique in a multifunctional scanning tunneling microscope.

Science.gov (United States)

Duan, Ming-Chao; Liu, Zhi-Long; Ge, Jian-Feng; Tang, Zhi-Jun; Wang, Guan-Yong; Wang, Zi-Xin; Guan, Dandan; Li, Yao-Yi; Qian, Dong; Liu, Canhua; Jia, Jin-Feng

2017-07-01

Superconducting thin films have been a focal point for intensive research efforts since their reduced dimension allows for a wide variety of quantum phenomena. Many of these films, fabricated in UHV chambers, are highly vulnerable to air exposure, making it difficult to measure intrinsic superconducting properties such as zero resistance and perfect diamagnetism with ex situ experimental techniques. Previously, we developed a multifunctional scanning tunneling microscope (MSTM) containing in situ four-point probe (4PP) electrical transport measurement capability in addition to the usual STM capabilities [Ge et al., Rev. Sci. Instrum. 86, 053903 (2015)]. Here we improve this MSTM via development of both transmission and reflection two-coil mutual inductance techniques for in situ measurement of the diamagnetic response of a superconductor. This addition does not alter the original STM and 4PP functions of the MSTM. We demonstrate the performance of the two-coil mutual inductance setup on a 10-nm-thick NbN thin film grown on a Nb-doped SrTiO 3 (111) substrate.

Phase transformation in sol-gel prepared zirconia using in-situ high temperature X-ray diffraction

International Nuclear Information System (INIS)

Srinivasan, R.; Davis, B.H.; Hubbard, C.R.; Cavin, O.B.; Porter, W.D.

1991-01-01

Zirconia was precipitated at a pH of 10.5 by admixing a solution of ZrCl 4 and NH 4 OH both rapidly (∼ 1 min) and slowly (∼ 8 hr). The precipitate was calcined at 500C for 5 hours and then furnace cooled. The former exhibited monoclinic phase while the latter yielded tetragonal phase. The pathway from amorphous to crystalline form was followed by in-situ high temperature X-ray diffraction in flowing air and in He. The data showed the evolution of the tetragonal crystalline phase on heating. On rapid cooling the tetragonal phase is retained at R.T., and on slow cooling the transformation to monoclinic phase occurs in air

Electrical Characterization of Nanopolyaniline/Porous Silicon Heterojunction at High Temperatures

Directory of Open Access Journals (Sweden)

Salah E. El-Zohary

2013-01-01

Full Text Available Nanopolyaniline/p-type porous silicon (NPANI/PSi heterojunction films were chemically fabricated via in situ polymerization. The composition and morphology of the nanopolymer were confirmed using Fourier transform infrared, scanning electron microscopy, UV-visible, and transmission electron microscopy techniques. The results indicated that the polymerization took place throughout the porous layer. The I-V measurements, performed at different temperatures, enabled the calculation of ideality factor, barrier height, and series resistance of those films. The obtained ideality factor showed a nonideal diode behavior. The series resistance was found to decrease with increasing temperature.

Compact very low temperature scanning tunneling microscope with mechanically driven horizontal linear positioning stage.

Science.gov (United States)

Suderow, H; Guillamon, I; Vieira, S

2011-03-01

We describe a scanning tunneling microscope for operation in a dilution refrigerator with a sample stage which can be moved macroscopically in a range up to a cm and with an accuracy down to the tens of nm. The position of the tip over the sample as set at room temperature does not change more than a few micrometers when cooling down. This feature is particularly interesting for work on micrometer sized samples. Nanostructures can be also localized and studied, provided they are repeated over micrometer sized areas. The same stage can be used to approach a hard single crystalline sample to a knife and cleave it, or break it, in situ. In situ positioning is demonstrated with measurements at 0.1 K in nanofabricated samples. Atomic resolution down to 0.1 K and in magnetic fields of 8 T is demonstrated in NbSe(2). No heat dissipation nor an increase in mechanical noise has been observed at 0.1 K when operating the slider.

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

Science.gov (United States)

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

2016-12-01

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

Low-temperature, ultrahigh-vacuum tip-enhanced Raman spectroscopy combined with molecular beam epitaxy for in situ two-dimensional materials' studies

Science.gov (United States)

Sheng, Shaoxiang; Li, Wenbin; Gou, Jian; Cheng, Peng; Chen, Lan; Wu, Kehui

2018-05-01

Tip-enhanced Raman spectroscopy (TERS), which combines scanning probe microscopy with the Raman spectroscopy, is capable to access the local structure and chemical information simultaneously. However, the application of ambient TERS is limited by the unstable and poorly controllable experimental conditions. Here, we designed a high performance TERS system based on a low-temperature ultrahigh-vacuum scanning tunneling microscope (LT-UHV-STM) and combined with a molecular beam epitaxy (MBE) system. It can be used for growing two-dimensional (2D) materials and for in situ STM and TERS characterization. Using a 2D silicene sheet on the Ag(111) surface as a model system, we achieved an unprecedented 109 Raman single enhancement factor in combination with a TERS spatial resolution down to 0.5 nm. The results show that TERS combined with a MBE system can be a powerful tool to study low dimensional materials and surface science.

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

Energy Technology Data Exchange (ETDEWEB)

Wang, Xuebing; Chen, Ting; Qi, Xintong [Department of Geosciences, Stony Brook University, Stony Brook, New York 11794 (United States); Zou, Yongtao; Liebermann, Robert C.; Li, Baosheng [Mineral Physics Institute, Stony Brook University, Stony Brook, New York 11794 (United States); Kung, Jennifer [Department of Earth Sciences, National Cheng Kung University, Tainan 70101, Taiwan (China); Yu, Tony; Wang, Yanbin [GeoSoilEnviroCARS, Center for Advanced Radiation Sources, The University of Chicago, 5640 S. Ellis Avenue, Chicago, Illinois 60637 (United States)

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.

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

International Nuclear Information System (INIS)

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

2015-01-01

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 Al 2 O 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 2 O 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

Impact of Membrane-Induced Particle Immobilization on Seeded Growth Monitored by In Situ Liquid Scanning Transmission Electron Microscopy.

Science.gov (United States)

Weiner, Rebecca G; Chen, Dennis P; Unocic, Raymond R; Skrabalak, Sara E

2016-05-01

In situ liquid cell scanning transmission electron microscopy probes seeded growth in real time. The growth of Pd on Au nanocubes is monitored as a model system to compare growth within a liquid cell and traditional colloidal synthesis. Different growth patterns are observed due to seed immobilization and the highly reducing environment within the liquid cell. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Crystallization kinetics of Fe-B based amorphous alloys studied in-situ using X-rays diffraction and differential scanning calorimetry

Directory of Open Access Journals (Sweden)

Santos D.R. dos

2001-01-01

Full Text Available The crystallization processes for the amorphous metallic alloys Fe74B17Si2Ni4Mo3 and Fe86B6Zr7Cu1 (at. % were investigated using X-rays diffraction measurements performed in-situ during Joule-heating, with simultaneous monitoring of the electrical resistance. We determined the main structural transitions and crystalline phases formed during heating, and correlated these results to the observed resistance variations. As the annealing current is increased, the resistance shows an initial decrease due to stress relaxation, followed by a drop to a minimum value due to massive nucleation and growth of alpha-Fe nanocrystals. Further annealing causes the formation of small fractions of Fe-B, B2Zr or ZrO2, while the resistance increases due to temperature enhancement. In situ XRD measurements allowed the identification of metastable phases, as the gamma-Fe phase which occurs at high temperatures. The exothermal peaks observed in the differential scanning calorimetry (DSC for each alloy corroborate the results. We also have performed DSC measurements with several heating rates, which allowed the determination of the Avrami exponent and crystallization activation energy for each alloy. The obtained activation energies (362 and 301 kJ/mol for Fe-B-Zr-Cu; 323 kJ/mol for Fe-B-Si-Ni-Mo are comparable to reported values for amorphous iron alloys, while the Avrami exponent values (n = 1.0 or n = 1.2 are consistent with diffusion controlled crystallization processes with nucleation rates close to zero.

A novel fabrication technology of in situ TiB2/6063Al composites: High energy ball milling and melt in situ reaction

International Nuclear Information System (INIS)

Zhang, S.-L.; Yang, J.; Zhang, B.-R.; Zhao, Y.-T.; Chen, G.; Shi, X.-X.; Liang, Z.-P.

2015-01-01

Highlights: • This paper presents a novel technology to fabricate the TiB 2 /6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB 2 /6063Al matrix composites are fabricated from Al–TiO 2 –B 2 O 3 system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO 2 –B 2 O 3 system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB 2 particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB 2 particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB 2 /6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character

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

International Nuclear Information System (INIS)

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

2015-01-01

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

Analysis and Calibration of in situ scanning tunnelling microscopy Images with atomic Resolution Influenced by Surface Drift Phenomena

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Møller, Per

1994-01-01

The influence of surface drift velocities on in situ scanning tunnelling microscopy (STM) experiments with atomic resolution is analysed experimentally and mathematically. Constant drift velocities much smaller than the speed of scanning can in many in situ STM experiments with atomic resolution ...... as well as the vectors of the non-distorted surface lattice can be determined. The calibration of distances can thus be carried out also when the image is influenced by drift. Results with gold surfaces and graphite surfaces are analysed and discussed....

An ultrahigh vacuum fast-scanning and variable temperature scanning tunneling microscope for large scale imaging.

Science.gov (United States)

Diaconescu, Bogdan; Nenchev, Georgi; de la Figuera, Juan; Pohl, Karsten

2007-10-01

We describe the design and performance of a fast-scanning, variable temperature scanning tunneling microscope (STM) operating from 80 to 700 K in ultrahigh vacuum (UHV), which routinely achieves large scale atomically resolved imaging of compact metallic surfaces. An efficient in-vacuum vibration isolation and cryogenic system allows for no external vibration isolation of the UHV chamber. The design of the sample holder and STM head permits imaging of the same nanometer-size area of the sample before and after sample preparation outside the STM base. Refractory metal samples are frequently annealed up to 2000 K and their cooldown time from room temperature to 80 K is 15 min. The vertical resolution of the instrument was found to be about 2 pm at room temperature. The coarse motor design allows both translation and rotation of the scanner tube. The total scanning area is about 8 x 8 microm(2). The sample temperature can be adjusted by a few tens of degrees while scanning over the same sample area.

In situ high temperature MAS NMR study of the mechanisms of catalysis. Ethane aromatization on Zn-modified zeolite BEA.

Science.gov (United States)

Arzumanov, Sergei S; Gabrienko, Anton A; Freude, Dieter; Stepanov, Alexander G

2009-04-01

Ethane conversion into aromatic hydrocarbons over Zn-modified zeolite BEA has been analyzed by high-temperature MAS NMR spectroscopy. Information about intermediates (Zn-ethyl species) and reaction products (mainly toluene and methane), which were formed under the conditions of a batch reactor, was obtained by (13)C MAS NMR. Kinetics of the reaction, which was monitored by (1)H MAS NMR in situ at the temperature of 573K, provided information about the reaction mechanism. Simulation of the experimental kinetics within the frames of the possible kinetic schemes of the reaction demonstrates that a large amount of methane evolved under ethane aromatization arises from the stage of direct ethane hydrogenolysis.

Combined Scanning Nanoindentation and Tunneling Microscope Technique by Means of Semiconductive Diamond Berkovich Tip

International Nuclear Information System (INIS)

Lysenko, O; Novikov, N; Gontar, A; Grushko, V; Shcherbakov, A

2007-01-01

A combined Scanning Probe Microscope (SPM) - nanoindentation instrument enables submicron resolution indentation tests and in-situ scanning of structure surfaces. A newly developed technique is based on the scanning tunneling microscopy (STM) with integrated Berkovich diamond semiconductive tip. Diamond tips for a combined SPM were obtained using the developed procedure including the synthesis of the semiconductive borondoped diamond monocrystals by the temperature gradient method at high pressure - high temperature conditions and fabrication of the tips from these crystals considering their zonal structure. Separately grown semiconductive diamond single crystals were studied in order to find the best orientation of diamond crystals. Optimal scanning characteristics and experimental data errors were calculated by an analysis of the general functional dependence of the tunneling current from properties of the tip and specimen. Tests on the indentation and scanning of the gold film deposited on the silicon substrate employing the fabricated tips demonstrated their usability, acceptable resolution and sensitivity

Monitoring of high temperature area by resistivity tomography during in-situ heating test in sedimentary soft rocks

International Nuclear Information System (INIS)

Kubota, Kenji; Suzuki, Koichi; Ikenoya, Takafumi; Takakura, Nozomu; Tani, Kazuo

2009-01-01

One of the major issues in disposal of nuclear waste is that the long term behaviors of sedimentary soft rocks can be affected by various environmental factors such as temperature, mechanical conditions or hydraulic conditions. Therefore, it is necessary to develop a method for evaluating the long term stability of caverns in sedimentary soft rocks as subjected to changes of environment. We have conducted in-situ heating test to evaluate the influence of high temperature to the surrounding rock mass at a depth of 50 m. The well with a diameter of 30 cm and 60 cm of height, was drilled and filled with groundwater. The heater was installed in the well for heating the surrounding rock mass. During the heating, temperature and deformation around the well were measured. To evaluate the influence of heating on sedimentary soft rocks, it is important to monitor the extent of heated area. Resistivity monitoring is thought to be effective to map the extent of the high temperature area. So we have conducted resistivity tomography during the heating test. The results demonstrated that the resistivity of the rock mass around the heating well decreased and this area was gradually expanded from the heated area during the heating. The decreasing rate of resistivity on temperature is correlated to that of laboratory experimental result and existing empirical formula between aqueous solution resistivity and temperature. Resistivity is changed by many other factors, but it is expected that resistivity change by other factors is very few in this test. This suggests that high temperature area is detected and spatial distribution of temperature can be mapped by resistivity tomography. So resistivity tomography is expected to be one of the promising methods to monitor the area heated by nuclear waste. (author)

In situ measurement of the kinetic friction of ZnO nanowires inside a scanning electron microscope

Energy Technology Data Exchange (ETDEWEB)

Polyakov, Boris, E-mail: boriss.polakovs@ut.ee [Institute of Physics, University of Tartu, Riia st. 142, Tartu (Estonia); Institute of Solid State Physics, University of Latvia, Kengaraga st. 8, Riga (Latvia); Dorogin, Leonid M; Lohmus, Ants [Institute of Physics, University of Tartu, Riia st. 142, Tartu (Estonia); Romanov, Alexey E [Institute of Physics, University of Tartu, Riia st. 142, Tartu (Estonia); Ioffe Physical Technical Institute, RAS, Politehnicheskaja st. 26, St. Petersburg (Russian Federation); Lohmus, Rynno [Institute of Physics, University of Tartu, Riia st. 142, Tartu (Estonia)

2012-01-15

A novel method for measuring the kinetic friction force in situ was developed for zinc oxide nanowires on highly oriented pyrolytic graphite and oxidised silicon wafers. The experiments were performed inside a scanning electron microscope and used a nanomanipulation device as an actuator, which also had an atomic force microscope tip attached to it as a probe. A simple model based on the Timoshenko elastic beam theory was applied to interpret the elastic deformation of a sliding nanowire (NW) and to determine the distributed kinetic friction force.

Catalytic monolayer voltammetry and in situ scanning tunneling microscopy of copper nitrite reductase on cysteamine-modified Au(111) electrodes

DEFF Research Database (Denmark)

Zhang, Jingdong; Welinder, A.C.; Hansen, Allan Glargaard

2003-01-01

electrochemical scanning tunneling microscopy (in situ STM) directly in aqueous acetate buffer, pH 6.0 has been used. High-resolution in situ STM shows that cysteamine packs into ordered domains with strip features of a periodic distance of 11.7 +/- 0.3 Angstrom. No voltammetric signals of the nitrite substrate...... on this surface could be detected. A strong cathodic catalytic wave appears in the presence of nitrite. The catalytic current follows a Michaelis-Menten pattern with a Michaelis constant of K-m approximate to 44 muM, which is close to the value for AxCuNiR in homogeneous solution. The apparent catalytic rate...

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

Science.gov (United States)

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

In Situ X-Ray Diffraction Study on Surface Melting of Bi Nanoparticles Embedded in a SiO2 Matrix

International Nuclear Information System (INIS)

Chen Xiao-Ming; Huo Kai-Tuo; Liu Peng

2014-01-01

Bi nanoparticles embedded in a SiO 2 matrix were prepared via the high energy ball milling method. The melting behavior of Bi nanoparticles was studied by means of differential scanning calorimetry (DSC) and high-temperature in situ X-ray diffraction (XRD). DSC cannot distinguish the surface melting from ‘bulk’ melting of the Bi nanoparticles. The XRD intensity of the Bi nanoparticles decreases progressively during the in situ heating process. The variation in the normalized integrated XRD intensity versus temperature is related to the average grain size of Bi nanoparticles. Considering the effects of temperature on Debye—Waller factor and Lorentz-polarization factor, we discuss the XRD results in accordance with surface melting. Our results show that the in situ XRD technique is effective to explore the surface melting of nanoparticles

Comparison between remotely-sensed sea-surface temperature (AVHRR and in situ records in San Matías Gulf (Patagonia, Argentina

Directory of Open Access Journals (Sweden)

Gabriela N Williams

2014-03-01

Full Text Available In situ records of sea surface temperature collected between 2005 and 2009 were used to compare, for the first time, the temperature estimated by the Multichannel algorithms (MCSST of the Advanced Very High Resolution Radiometer (AVHRR sensors in San Matías Gulf, in the north of the Argentinean Patagonian Continental Shelf (between 40°47'-42°13'S. Match-ups between in situ records and satellite sea surface temperature (SST were analyzed. In situ records came from fixed stations and oceanographic cruises, while satellite data came from different NOAA satellites. The fitting of temperature data to a Standard Major Axis (SMA type II regression model indicated that a high proportion of the total variance (0.53< r² <0.99 was explained by this model showing a high correlation between in situ data and satellite estimations. The mean differences between satellite and in situ data for the full data set were 1.64 ± 1.49°C. Looking separately into in situ data from different sources and day and night estimates from different NOAA satellites, the differences were between 0.30 ± 0.60°C and 2.60 ± 1.50°C. In this paper we discuss possible reasons for the above-mentioned performance of the MCSST algorithms in the study area.

A novel fabrication technology of in situ TiB{sub 2}/6063Al composites: High energy ball milling and melt in situ reaction

Energy Technology Data Exchange (ETDEWEB)

Zhang, S.-L.; Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Zhang, B.-R. [School of Mechanical Engineering, Qilu University of Technology, Jinan, Shandong 250022 (China); Zhao, Y.-T., E-mail: 278075525@qq.com [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Chen, G.; Shi, X.-X.; Liang, Z.-P. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China)

2015-08-05

Highlights: • This paper presents a novel technology to fabricate the TiB{sub 2}/6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB{sub 2}/6063Al matrix composites are fabricated from Al–TiO{sub 2}–B{sub 2}O{sub 3} system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO{sub 2}–B{sub 2}O{sub 3} system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB{sub 2} particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB{sub 2} particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB{sub 2}/6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character.

An in situ FTIR step-scan photoacoustic investigation of kerogen and minerals in oil shale.

Science.gov (United States)

Alstadt, Kristin N; Katti, Dinesh R; Katti, Kalpana S

2012-04-01

Step-scan photoacoustic infrared spectroscopy experiments were performed on Green River oil shale samples obtained from the Piceance Basin located in Colorado, USA. We have investigated the molecular nature of light and dark colored areas of the oil shale core using FTIR photoacoustic step-scan spectroscopy. This technique provided us with the means to analyze the oil shale in its original in situ form with the kerogen-mineral interactions intact. All vibrational bands characteristic of kerogen were found in the dark and light colored oil shale samples confirming that kerogen is present throughout the depth of the core. Depth profiling experiments indicated that there are changes between layers in the oil shale molecular structure at a length scale of micron. Comparisons of spectra from the light and dark colored oil shale core samples suggest that the light colored regions have high kerogen content, with spectra similar to that from isolated kerogen, whereas, the dark colored areas contain more mineral components which include clay minerals, dolomite, calcite, and pyrite. The mineral components of the oil shale are important in understanding how the kerogen is "trapped" in the oil shale. Comparing in situ kerogen spectra with spectra from isolated kerogen indicate significant band shifts suggesting important nonbonded molecular interactions between the kerogen and minerals. Copyright © 2011 Elsevier B.V. All rights reserved.

Design of a new reactor-like high temperature near ambient pressure scanning tunneling microscope for catalysis studies.

Science.gov (United States)

Tao, Franklin Feng; Nguyen, Luan; Zhang, Shiran

2013-03-01

Here, we present the design of a new reactor-like high-temperature near ambient pressure scanning tunneling microscope (HT-NAP-STM) for catalysis studies. This HT-NAP-STM was designed for exploration of structures of catalyst surfaces at atomic scale during catalysis or under reaction conditions. In this HT-NAP-STM, the minimized reactor with a volume of reactant gases of ∼10 ml is thermally isolated from the STM room through a shielding dome installed between the reactor and STM room. An aperture on the dome was made to allow tip to approach to or retract from a catalyst surface in the reactor. This dome minimizes thermal diffusion from hot gas of the reactor to the STM room and thus remains STM head at a constant temperature near to room temperature, allowing observation of surface structures at atomic scale under reaction conditions or during catalysis with minimized thermal drift. The integrated quadrupole mass spectrometer can simultaneously measure products during visualization of surface structure of a catalyst. This synergy allows building an intrinsic correlation between surface structure and its catalytic performance. This correlation offers important insights for understanding of catalysis. Tests were done on graphite in ambient environment, Pt(111) in CO, graphene on Ru(0001) in UHV at high temperature and gaseous environment at high temperature. Atom-resolved surface structure of graphene on Ru(0001) at 500 K in a gaseous environment of 25 Torr was identified.

Quantitative and Qualitative Aspects of Gas-Metal-Oxide Mass Transfer in High-Temperature Confocal Scanning Laser Microscopy

Science.gov (United States)

Piva, Stephano P. T.; Pistorius, P. Chris; Webler, Bryan A.

2018-05-01

During high-temperature confocal scanning laser microscopy (HT-CSLM) of liquid steel samples, thermal Marangoni flow and rapid mass transfer between the sample and its surroundings occur due to the relatively small sample size (diameter around 5 mm) and large temperature gradients. The resulting evaporation and steel-slag reactions tend to change the chemical composition in the metal. Such mass transfer effects can change observed nonmetallic inclusions. This work quantifies oxide-metal-gas mass transfer of solutes during HT-CSLM experiments using computational simulations and experimental data for (1) dissolution of MgO inclusions in the presence and absence of slag and (2) Ca, Mg-silicate inclusion changes upon exposure of a Si-Mn-killed steel to an oxidizing gas atmosphere.

  In situ identification of streptococci and other bacteria in initial dental biofilm by confocal laser scanning microscopy and fluorescence in situ hybridization

DEFF Research Database (Denmark)

Dige, Irene; Kilian, Mogens; Nilsson, Holger

2007-01-01

Confocal laser scanning microscopy (CLSM) has been employed as a method for studying intact natural biofilm. When combined with fluorescence in situ hybridization (FISH) it is possible to analyze spatial relationships and changes of specific members of microbial populations over time. The aim...

A new contact electric resistance technique for in-situ measurement of the electric resistance of surface films on metals in electrolytes at high temperatures and pressures

International Nuclear Information System (INIS)

Saario, T.; Marichev, V.A.

1993-01-01

Surface films play a major role in corrosion assisted cracking. A new Contact Electric Resistance (CER) method has been recently developed for in situ measurement of the electric resistance of surface films. The method has been upgraded for high temperature high pressure application. The technique can be used for any electrically conductive material in any environment including liquid, gas or vacuum. The technique has been used to determine in situ the electric resistance of films on metals during adsorption of water and anions, formation and destruction of oxides and hydrides, electroplating of metals and to study the electric resistance of films on semiconductors. The resolution of the CER technique is 10 -9 Ω, which corresponds to about 0.03 monolayers of deposited copper during electrochemical deposition Cu/Cu 2+ . Electric resistance data can be measured with a frequency of the order of one hertz, which enables one to follow in situ the kinetics of surface film related processes. The kinetics of these processes and their dependence on the environment, temperature, pH and electrochemical potential can be investigated

In situ scanning tunnelling microscopy of redox molecules. Coherent electron transfer at large bias voltages

DEFF Research Database (Denmark)

Zhang, Jingdong; Kuznetsov, A.M.; Ulstrup, Jens

2003-01-01

Theories of in situ scanning tunnelling microscopy (STM) of molecules with redox levels near the substrate and tip Fermi levels point to 'spectroscopic' current-overpotential features. Prominent features require a narrow 'probing tip', i.e. a small bias voltage, eV(bias), compared...

In situ electron backscatter diffraction investigation of recrystallization in a copper wire.

Science.gov (United States)

Brisset, François; Helbert, Anne-Laure; Baudin, Thierry

2013-08-01

The microstructural evolution of a cold drawn copper wire (reduction area of 38%) during primary recrystallization and grain growth was observed in situ by electron backscatter diffraction. Two thermal treatments were performed, and successive scans were acquired on samples undergoing heating from ambient temperature to a steady state of 200°C or 215°C. During a third in situ annealing, the temperature was continuously increased up to 600°C. Nuclei were observed to grow at the expense of the deformed microstructure. This growth was enhanced by the high stored energy difference between the nuclei and their neighbors (driving energy in recrystallization) and by the presence of high-angle grain boundaries of high mobility. In the early stages of growth, the nuclei twin and the newly created orientations continue to grow to the detriment of the strained copper. At high temperatures, the disappearance of some twins was evidenced by the migration of the incoherent twin boundaries. Thermal grooving of grain boundaries is observed at these high temperatures and affects the high mobile boundaries but tends to preserve the twin boundaries of lower energy. Thus, grooving may contribute to the twin vanishing.

Preparation of Ti-aluminide reinforced in situ aluminium matrix composites by reactive hot pressing

International Nuclear Information System (INIS)

Roy, D.; Ghosh, S.; Basumallick, A.; Basu, B.

2007-01-01

Aluminium based metal matrix composites reinforced with in situ Ti-aluminide and alumina particles were prepared by reactive hot pressing a powder mix of aluminium and nanosized TiO 2 powders. The reinforcements were formed in situ by exothermal reaction between the TiO 2 nano crystalline powder and aluminium. The thermal characteristics of the in situ reaction were studied with the aid of Differential scanning calorimetry (DSC). X-ray diffraction (XRD), Energy dispersive spectroscopy (EDS) and Scanning electron microscopy (SEM) techniques were employed to study the microstructural architecture of the composites as a function of hot pressing temperature and volume percent reinforcement. Microhardness measurements on the as prepared in situ aluminium matrix composites exhibit significant increase in hardness with increase in hot pressing temperature and volume fraction of reinforcement

In-situ Study of Dynamic Phenomena at Metal Nanosolder Interfaces Using Aberration Corrected Scanning Transmission Electron Microcopy.

Energy Technology Data Exchange (ETDEWEB)

Lu, Ping

2014-10-01

Controlling metallic nanoparticle (NP) interactions plays a vital role in the development of new joining techniques (nanosolder) that bond at lower processing temperatures but remain viable at higher temperatures. The pr imary objective of this project is t o develop a fundamental understanding of the actual reaction processes, associated atomic mechanisms, and the resulting microstructure that occur during thermally - driven bond formation concerning metal - metal nano - scale (%3C50nm) interfaces. In this LDRD pr oject, we have studied metallic NPs interaction at the elevated temperatures by combining in - situ transmission electron microscopy (TEM ) using an aberration - corrected scanning transmission electron microscope (AC - STEM) and atomic - scale modeling such as m olecular dynamic (MD) simulations. Various metallic NPs such as Ag, Cu and Au are synthesized by chemical routines. Numerous in - situ e xperiments were carried out with focus of the research on study of Ag - Cu system. For the first time, using in - situ STEM he ating experiments , we directly observed t he formation of a 3 - dimensional (3 - D) epitaxial Cu - Ag core - shell nanoparticle during the thermal interaction of Cu and Ag NPs at elevated temperatures (150 - 300 o C). The reaction takes place at temperatures as low as 150 o C and was only observed when care was taken to circumvent the effects of electron beam irradiation during STEM imaging. Atomic - scale modeling verified that the Cu - Ag core - shell structure is energetically favored, and indicated that this phenomenon is a nano - scale effect related to the large surface - to - volume ratio of the NPs. The observation potentially can be used for developing new nanosolder technology that uses Ag shell as the "glue" that stic ks the particles of Cu together. The LDRD has led to several journal publications and numerous conference presentations, and a TA. In addition, we have developed new TEM characterization techniques and phase

In-situ heating test in the sedimentary soft rock. Part 3. Monitoring of the extent of high temperature zone by resistivity tomography

International Nuclear Information System (INIS)

Kubota, Kenji; Suzuki, Koichi; Ikenoya, Takafumi; Takakura, Nozomu; Tani, Kazuo

2009-01-01

One of the major issues in disposal of nuclear waste is that the long term behaviors of sedimentary soft rocks can be affected by various environmental factors such as temperature or hydraulic conditions. Therefore, it is necessary to develop a method for evaluating the long term stability of caverns in sedimentary soft rocks as subjected to changes of environment. We have conducted in-situ heating test to evaluate the influence of high temperature to the surrounding rock mass at a depth of 50m. Resistivity monitoring is thought to be effective to map the extent of high temperature zone. So resistivity tomography was conducted during the heating. The results demonstrated that the resistivity of the rock mass around the heater well was decreased and this area was gradually expanded from the heated area during the heating. Resistivity of rock is proportional to that of pore water which is known to decrease with increasing temperature. This suggests that high temperature zone is detected and spatial distribution of temperature can be mapped by resistivity tomography. So resistivity tomography is expected to be one of the promising methods to monitor the heated area by nuclear waste. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Zhang, Shuo; Ma, Ping, E-mail: maping@semi.ac.cn; Liu, Boting; Wu, Dongxue; Li, Jinmin [Research and Development Center for Solid State Lighting, Institute of Semiconductors, Chinese Academy of Sciences, Beijing 100083 (China); Huang, Yuliang [Beijing Engineering Research Center for the 3rd Generation Semiconductor Materials and Application, Beijing 100083 (China); Wang, Junxi [State Key Laboratory of Solid State Lighting, Beijing 100083 (China)

2016-06-15

High-resistive layers were obtained by periodic growth and in situ annealing of InGaN. The effect of the annealing temperature of InGaN on the indium content and the material sheet resistive was investigated. The indium content decreased as the increase of in situ annealing temperature. Additionally, the material sheet resistance increased with the increase of the in situ annealing temperature for the annealed samples and reached 2 × 10{sup 10}Ω/sq in the light and 2 × 10{sup 11}Ω/sq in the dark when the in situ annealing temperature reached 970{sup ∘}C. The acquirement of high-resistive layers is attributed to the generation of indium vacancy-related defects. Introducing indium vacancy-related defects to compensate background carriers can be an effective method to grow high-resistance material.

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

International Nuclear Information System (INIS)

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

2016-01-01

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 × 10"1"0Ω/sq in the light and 2 × 10"1"1Ω/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.

In situ investigation of ion-induced dewetting of a thin iron-oxide film on silicon by high resolution scanning electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Amirthapandian, S. [Institut fuer Halbleiteroptik und Funktionelle Grenzflaechen, Universitaet Stuttgart, 70569 Stuttgart (Germany); Material Physics Division, Materials Science Group, Indira Gandhi Centre for Atomic Research, Kalpakkam 603 102 (India); Schuchart, F.; Garmatter, D.; Bolse, W. [Institut fuer Halbleiteroptik und Funktionelle Grenzflaechen, Universitaet Stuttgart, 70569 Stuttgart (Germany)

2012-11-15

Using our new in situ high resolution scanning electron microscope, which is integrated into the UNILAC ion beamline at the Helmholtzzentrum fuer Schwerionenforschung (GSI) in Darmstadt, Germany, we investigated the swift heavy ion induced dewetting of a thin iron oxide layer on Si. Besides heterogeneous hole nucleation at defects and spontaneous (homogeneous) hole nucleation, we could clearly identify a dewetting mechanism, which is similar to the spinodal dewetting observed for liquid films. Instead of being due to capillary waves, it is based on a stress induced surface instability. The latter results in the formation of a wavy surface with constant dominant wave-length and increasing amplitude during ion irradiation. Dewetting sets in as soon as the wave-troughs reach the film-substrate interface. Inspection of the hole radii and rim shapes indicates that removal of the material from the hole area occurs mainly by plastic deformation at the inner boundary and ion induced viscous flow in the peripheral zone due to surface tension.

In-Situ tensile testing of propellants in SEM: influence of temperature

NARCIS (Netherlands)

Di Benedetto, G.L.; Ramshorst, M.C.J.; Duvalois, W.; Hooijmeijer, P.; Heijden, A. van der

2017-01-01

A tensile module system placed within a Scanning Electron Microscope (SEM) was utilized to conduct insitu tensile testing of propellant samples. The tensile module system allows for real-time in-situ SEM analysis of the samples to determine the failure mechanism of the propellant material under

A scanning Hall probe microscope for high resolution magnetic imaging down to 300 mK

International Nuclear Information System (INIS)

Khotkevych, V. V.; Bending, S. J.; Milosevic, M. V.

2008-01-01

We present the design, construction, and performance of a low-temperature scanning Hall probe microscope with submicron lateral resolution and a large scanning range. The detachable microscope head is mounted on the cold flange of a commercial 3 He-refrigerator (Oxford Instruments, Heliox VT-50) and operates between room temperature and 300 mK. It is fitted with a three-axis slip-stick nanopositioner that enables precise in situ adjustment of the probe location within a 6x6x7 mm 3 space. The local magnetic induction at the sample surface is mapped with an easily changeable microfabricated Hall probe [typically GsAs/AlGaAs or AlGaAs/InGaAs/GaAs Hall sensors with integrated scanning tunnel microscopy (STM) tunneling tips] and can achieve minimum detectable fields ≥10 mG/Hz 1/2 . The Hall probe is brought into very close proximity to the sample surface by sensing and controlling tunnel currents at the integrated STM tip. The instrument is capable of simultaneous tunneling and Hall signal acquisition in surface-tracking mode. We illustrate the potential of the system with images of superconducting vortices at the surface of a Nb thin film down to 372 mK, and also of labyrinth magnetic-domain patterns of an yttrium iron garnet film captured at room temperature.

A new variable temperature solution-solid interface scanning tunneling microscope.

Science.gov (United States)

Jahanbekam, Abdolreza; Mazur, Ursula; Hipps, K W

2014-10-01

We present a new solution-solid (SS) interface scanning tunneling microscope design that enables imaging at high temperatures with low thermal drift and with volatile solvents. In this new design, distinct from the conventional designs, the entire microscope is surrounded in a controlled-temperature and controlled-atmosphere chamber. This allows users to take measurements at high temperatures while minimizing thermal drift. By incorporating an open solution reservoir in the chamber, solvent evaporation from the sample is minimized; allowing users to use volatile solvents for temperature dependent studies at high temperatures. The new design enables the user to image at the SS interface with some volatile solvents for long periods of time (>24 h). An increase in the nonlinearity of the piezoelectric scanner in the lateral direction as a function of temperature is addressed. A temperature dependent study of cobalt(II) octaethylporphyrin (CoOEP) at the toluene/Au(111) interface has been performed with this instrument. It is demonstrated that the lattice parameters remain constant within experimental error from 24 °C to 75 °C. Similar quality images were obtained over the entire temperature range. We report the unit cell of CoOEP at the toluene/Au(111) interface (based on two molecules per unit cell) to be A = (1.36 ± 0.04) nm, B = (2.51 ± 0.04) nm, and α = 97° ± 2°.

Measuring the temperature dependent thermal diffusivity of geomaterials using high-speed differential scanning calorimetry

Science.gov (United States)

von Aulock, Felix W.; Wadsworth, Fabian B.; Vasseur, Jeremie; Lavallée, Yan

2016-04-01

Heat diffusion in the Earth's crust is critical to fundamental geological processes, such as the cooling of magma, heat dissipation during and following transient heating events (e.g. during frictional heating along faults), and to the timescales of contact metamorphosis. The complex composition and multiphase nature of geomaterials prohibits the accurate modeling of thermal diffusivities and measurements over a range of temperatures are sparse due to the specialized nature of the equipment and lack of instrument availability. We present a novel method to measure the thermal diffusivity of geomaterials such as minerals and rocks with high precision and accuracy using a commercially available differential scanning calorimeter (DSC). A DSC 404 F1 Pegasus® equipped with a Netzsch high-speed furnace was used to apply a step-heating program to corundum single crystal standards of varying thicknesses. The standards were cylindrical discs of 0.25-1 mm thickness with 5.2-6 mm diameter. Heating between each 50 °C temperature interval was conducted at a rate of 100 °C/min over the temperature range 150-1050 °C. Such large heating rates induces temperature disequilibrium in the samples used. However, isothermal segments of 2 minutes were used during which the temperature variably equilibrated with the furnace between the heating segments and thus the directly-measured heat-flow relaxed to a constant value before the next heating step was applied. A finite-difference 2D conductive heat transfer model was used in cylindrical geometry for which the measured furnace temperature was directly applied as the boundary condition on the sample-cylinder surfaces. The model temperature was averaged over the sample volume per unit time and converted to heat-flow using the well constrained thermal properties for corundum single crystals. By adjusting the thermal diffusivity in the model solution and comparing the resultant heat-flow with the measured values, we obtain a model

In situ laser processing in a scanning electron microscope

Energy Technology Data Exchange (ETDEWEB)

Roberts, Nicholas A.; Magel, Gregory A.; Hartfield, Cheryl D.; Moore, Thomas M.; Fowlkes, Jason D.; Rack, Philip D. [Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States) and Omniprobe, Inc., an Oxford Instruments Company, 10410 Miller Rd., Dallas, Texas 75238 (United States); Omniprobe, Inc., an Oxford Instruments Company, 10410 Miller Rd., Dallas, Texas 75238 (United States); Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States); Department of Materials Science and Engineering, University of Tennessee, Knoxville, Tennessee 37996 (United States) and Center for Nanophase Materials Sciences, Oak Ridge National Laboratory, Oak Ridge, Tennessee 37831 (United States)

2012-07-15

Laser delivery probes using multimode fiber optic delivery and bulk focusing optics have been constructed and used for performing materials processing experiments within scanning electron microscope/focused ion beam instruments. Controlling the current driving a 915-nm semiconductor diode laser module enables continuous or pulsed operation down to sub-microsecond durations, and with spot sizes on the order of 50 {mu}m diameter, achieving irradiances at a sample surface exceeding 1 MW/cm{sup 2}. Localized laser heating has been used to demonstrate laser chemical vapor deposition of Pt, surface melting of silicon, enhanced purity, and resistivity via laser annealing of Au deposits formed by electron beam induced deposition, and in situ secondary electron imaging of laser induced dewetting of Au metal films on SiO{sub x}.

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

Science.gov (United States)

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

2014-11-01

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

An in situ Raman spectroscopy system for long-term corrosion experiments in high temperature water up to 673 K

International Nuclear Information System (INIS)

Domae, Masafumi; Tani, Jun-ichi; Fujiwara, Kazutoshi; Katsumura, Yosuke

2006-01-01

A Raman spectroscopy system has been developed, in order to identify oxides formed on the surfaces of metals and steels in high temperature water up to 673 K. A supercritical water loop system including a Raman cell was installed. The design of the loop system is up to 673 K and 40 MPa. The Raman cell has a diamond window without window-to-metal packing. Raman spectrum of alumina plate was measured at room temperature, at 523 and at 673 K under pressure of 25 MPa. A long-term measurement was also performed at 523 K and 25 MPa for 117.5 h. In all cases intense Raman peaks attributed to alumina were observed. Raman spectrum of anatase particles in suspension was measured at 673 K and 25 MPa. The results show that the Raman spectroscopy system developed in the present study works well not only for plate sample but also for suspension. Raman spectra observed for titanium plate in high temperature water of 673 K and 25 MPa show growth of several Raman peaks with time up to 257 h. The peaks disappeared after cooled down to room temperature. The experimental results have demonstrated importance of in situ Raman spectroscopy. (author)

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

Energy Technology Data Exchange (ETDEWEB)

Weber, Richard [Materials Development, Inc., Arlington Heights, IL (United States)

2016-04-22

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

In situ scanning tunneling microscopy study of Ca-modified rutile TiO2(110 in bulk water

Directory of Open Access Journals (Sweden)

Giulia Serrano

2015-02-01

Full Text Available Despite the rising technological interest in the use of calcium-modified TiO2 surfaces in biomedical implants, the Ca/TiO2 interface has not been studied in an aqueous environment. This investigation is the first report on the use of in situ scanning tunneling microscopy (STM to study calcium-modified rutile TiO2(110 surfaces immersed in high purity water. The TiO2 surface was prepared under ultrahigh vacuum (UHV with repeated sputtering/annealing cycles. Low energy electron diffraction (LEED analysis shows a pattern typical for the surface segregation of calcium, which is present as an impurity on the TiO2 bulk. In situ STM images of the surface in bulk water exhibit one-dimensional rows of segregated calcium regularly aligned with the [001] crystal direction. The in situ-characterized morphology and structure of this Ca-modified TiO2 surface are discussed and compared with UHV-STM results from the literature. Prolonged immersion (two days in the liquid leads to degradation of the overlayer, resulting in a disordered surface. X-ray photoelectron spectroscopy, performed after immersion in water, confirms the presence of calcium.

In-situ environmental (scanning) transmission electron microscopy of catalysts at the atomic level

International Nuclear Information System (INIS)

Gai, P L; Boyes, E D

2014-01-01

Observing reacting single atoms on the solid catalyst surfaces under controlled reaction conditions is a key goal in understanding and controlling heterogeneous catalytic reactions. In-situ real time aberration corrected environmental (scanning) transmission electron microscopy (E(S)TEM permit the direct imaging of dynamic surface and sub-surface structures of reacting catalysts. In this paper in-situ AC ETEM and AC ESTEM studies under controlled reaction environments of oxide catalysts and supported metal nanocatalysts important in chemical industry are presented. They provide the direct evidence of dynamic processes at the oxide catalyst surface at the atomic scale and single atom dynamics in catalytic reactions. The ESTEM studies of single atom dynamics in controlled reaction environments show that nanoparticles act as reservoirs of ad-atoms. The results have important implications in catalysis and nanoparticle studies

Note: Low-temperature scanning tunneling microscope with detachable scanner and reliable transfer mechanism for tip and sample exchange.

Science.gov (United States)

Ge, Weifeng; Wang, Jihao; Wang, Junting; Zhang, Jing; Hou, Yubin; Lu, Qingyou

2017-12-01

A homebuilt low-temperature scanning tunneling microscope (STM) featuring a detachable scanner based on a double slider design, along with a reliable transfer mechanism for tip and sample exchange, is present. The coarse motor is decoupled from the scanner, which prevents the motor instabilities including vibrations and drifts from entering the tip-sample loop and thus improves the performance of the STM. In addition, in situ exchange of tips and samples can be implemented easily and reliably using a winch-type transfer mechanism. Atomically resolved images on graphite are demonstrated to show the performance of the proposed STM.

Cytochrome C Dynamics at Gold and Glassy Carbon Surfaces Monitored by in Situ Scanning Tunnel Microscopy

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov; Møller, Per; Pedersen, Marianne Vind

1995-01-01

We have investigated the absorption of cytochrome c on gold and glassy carbon substrates by in situ scanning tunnel microscopy under potentiostatic control of both substrate and tip. Low ionic strength and potential ranges where no Faradaic current flows were used. Cyt c aggregates into flat...

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

Energy Technology Data Exchange (ETDEWEB)

Weber, J. K. R.; Alderman, O. L. G. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Tamalonis, A.; Sendelbach, S. [Materials Development, Inc., Arlington Heights, Illinois 60004 (United States); Benmore, C. J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States); Hebden, A.; Williamson, M. A. [Nuclear Engineering Division, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

2016-07-15

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

Analysis of the structural stability of the smectite submitted to high pressures and temperatures

International Nuclear Information System (INIS)

Alabarse, Frederico Gil

2009-10-01

The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

Investigating the use of in situ liquid cell scanning transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Nguy, Amanda [Iowa State Univ., Ames, IA (United States)

2016-02-19

Engineering nanoparticles with desired shape-dependent properties is the key to many applications in nanotechnology. Although many synthetic procedures exist to produce anisotropic gold nanoparticles, the dynamics of growth are typically unknown or hypothetical. In the case of seed-mediated growth in the presence of DNA into anisotropic nanoparticles, it is not known exactly how DNA directs growth into specific morphologies. A series of preliminary experiments were carried out to contribute to the investigation of the possible mechanism of DNA-mediated growth of gold nanoprisms into gold nanostars using liquid cell scanning transmission electron microscopy (STEM). Imaging in the liquid phase was achieved through the use of a liquid cell platform and liquid cell holder that allow the sample to be contained within a “chip sandwich” between two electron transparent windows. Ex situ growth experiments were performed using Au-T30 NPrisms (30-base thymine oligonucleotide-coated gold nanoprisms) that are expected to grow into gold nanostars. Growth to form these nanostars were imaged using TEM (transmission electron microscopy) and liquid cell STEM (scanning transmission electron microscopy). An attempt to perform in situ growth experiments with the same Au-T30 nanoprisms revealed challenges in obtaining desired morphology results due to the environmental differences within the liquid cell compared to the ex situ environment. Different parameters in the experimental method were explored including fluid line set up, simultaneous and alternating reagent addition, and the effect of different liquid cell volumes to ensure adequate flow of reagents into the liquid cell. Lastly, the binding affinities were compared for T30 and A30 DNA incubated with gold nanoparticles using zeta potential measurements, absorption spectroscopy, and isothermal titration calorimetry (ITC). It was previously reported thymine bases have a lower binding affinity to gold surfaces than adenine

Micelle-stabilized room-temperature phosphorescence with synchronous scanning

International Nuclear Information System (INIS)

Femia, R.A.; Love, L.J.C.

1984-01-01

The experimental requirements for synchronous wavelength scanning micelle-stabilized room temperature phosphorescence and the factors affecting peak resolution are presented and compared with those for synchronous wavelength scanning fluorescence. Identification of individual compounds in a four-component mixture is illustrated, and criteria to identify and minimize triplet state energy transfer are given. Considerable improvement in resolution of the synchronous peaks is obtained via second derivative spectra. 20 references, 7 figures, 2 tables

In Situ Synchrotron Radiation X-ray Diffraction Study on Phase and Oxide Growth during a High Temperature Cycle of a NiTi-20 at.% Zr High Temperature Shape Memory Alloy

Science.gov (United States)

Carl, Matthew; Van Doren, Brian; Young, Marcus L.

2018-02-01

Ternary additions to binary NiTi shape memory alloys are known to significantly affect the characteristic martensite-to-austenite phase transformation, i.e., decrease or increase transformation temperatures. High temperature shape memory alloys can be created by adding Au, Pt, Pd, Hf, or Zr to binary NiTi in appropriate amounts; however, the majority of these ternary additions are exceedingly expensive, unfortunately making them impractical for most commercial applications. Zr is the exception of the group, but it is often disregarded because of its poor workability and thermal stability. In an effort to find a temperature range that allows for the potential workability of NiTiZr alloys in normal atmosphere environments and to gain understanding as to the cause of failure during processing, a NiTi-20 at.% Zr was subjected to a thermal cycle ranging from RT to 1000 °C with short 15 min holds at select temperatures during both heating and cooling while simultaneously collecting high-energy synchrotron radiation X-ray diffraction measurements. This study provides valuable insight into the kinetics of precipitation and oxide formation and its relationship to processing. In addition, scanning electron microscopy was performed on five samples, each isothermally held to examine precipitation and oxide structure and growth.

Impact of process temperature on GaSb metal-oxide-semiconductor interface properties fabricated by ex-situ process

Energy Technology Data Exchange (ETDEWEB)

Yokoyama, Masafumi, E-mail: yokoyama@mosfet.t.u-tokyo.ac.jp; Takenaka, Mitsuru; Takagi, Shinichi [Department of Electrical Engineering and Information Systems, The University of Tokyo, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); JST-CREST, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); Asakura, Yuji [Department of Electrical Engineering and Information Systems, The University of Tokyo, Yayoi 2-11-16, Bunkyo, Tokyo 113-0032 (Japan); Yokoyama, Haruki [NTT Photonics Laboratories, NTT Corporation, Atsugi 243-0198 (Japan)

2014-06-30

We have studied the impact of process temperature on interface properties of GaSb metal-oxide-semiconductor (MOS) structures fabricated by an ex-situ atomic-layer-deposition (ALD) process. We have found that the ALD temperature strongly affects the Al{sub 2}O{sub 3}/GaSb MOS interface properties. The Al{sub 2}O{sub 3}/GaSb MOS interfaces fabricated at the low ALD temperature of 150 °C have the minimum interface-trap density (D{sub it}) of ∼4.5 × 10{sup 13 }cm{sup −2} eV{sup −1}. We have also found that the post-metalization annealing at temperature higher than 200 °C degrades the Al{sub 2}O{sub 3}/GaSb MOS interface properties. The low-temperature process is preferable in fabricating GaSb MOS interfaces in the ex-situ ALD process to avoid the high-temperature-induced degradations.

Study of gamma irradiated polyethylenes by temperature modulated differential scanning calorimetry

International Nuclear Information System (INIS)

Secerov, B.; Galovic, S.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

2011-01-01

Complete text of publication follows. The various polyethylenes (PEs) and effects of high energy radiation on theirs structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we applied the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and nonreversing part enabled to observed the low temperature enthalpy relaxation (related to the existence of the 'rigid amorphous phase') and recrystallization processes as well as to follow their and/or radiation-induced evolution of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

Variable-temperature independently driven four-tip scanning tunneling microscope

International Nuclear Information System (INIS)

Hobara, Rei; Nagamura, Naoka; Hasegawa, Shuji; Matsuda, Iwao; Yamamoto, Yuko; Miyatake, Yutaka; Nagamura, Toshihiko

2007-01-01

The authors have developed an ultrahigh vacuum (UHV) variable-temperature four-tip scanning tunneling microscope (STM), operating from room temperature down to 7 K, combined with a scanning electron microscope (SEM). Four STM tips are mechanically and electrically independent and capable of positioning in arbitrary configurations in nanometer precision. An integrated controller system for both of the multitip STM and SEM with a single computer has also been developed, which enables the four tips to operate either for STM imaging independently and for four-point probe (4PP) conductivity measurements cooperatively. Atomic-resolution STM images of graphite were obtained simultaneously by the four tips. Conductivity measurements by 4PP method were also performed at various temperatures with the four tips in square arrangement with direct contact to the sample surface

In-situ deformation studies of an aluminum metal-matrix composite in a scanning electron microscope

Science.gov (United States)

Manoharan, M.; Lewandowski, J. J.

1989-01-01

Tensile specimens made of a metal-matrix composite (cast and extruded aluminum alloy-based matrix reinforced with Al2O3 particulate) were tested in situ in a scanning electron microscope equipped with a deformation stage, to directly monitor the crack propagation phenomenon. The in situ SEM observations revealed the presence of microcracks both ahead of and near the crack-tip region. The microcracks were primarily associated with cracks in the alumina particles. The results suggest that a region of intense deformation exists ahead of the crack and corresponds to the region of microcracking. As the crack progresses, a region of plastically deformed material and associated microcracks remains in the wake of the crack.

Development of conductivity probe and temperature probe for in-situ measurements in hydrological studies

International Nuclear Information System (INIS)

Chandra, U.; Galindo, B.J.; Castagnet, A.C.G.

1981-05-01

A conductivity probe and a temperature probe have been developed for in-situ measurements in various hydrological field studies. The conductivity probe has platinum electrodes and is powered with two 12 volt batteries. The sensing element of the temperature probe consists of a resistor of high coefficient of temperature. Response of the conductivity probe is measured in a milliampere mater while the resistance of the thermistor is read by a digital meter. The values of conductivity and temperature are derived from respective calibration. The probes are prototype and their range of measurement can be improved depending upon the requirement of the field problem. (Author) [pt

In situ observation of the impact of surface oxidation on the crystallization mechanism of GeTe phase-change thin films by scanning transmission electron microscopy

Science.gov (United States)

Berthier, R.; Bernier, N.; Cooper, D.; Sabbione, C.; Hippert, F.; Noé, P.

2017-09-01

The crystallization mechanisms of prototypical GeTe phase-change material thin films have been investigated by in situ scanning transmission electron microscopy annealing experiments. A novel sample preparation method has been developed to improve sample quality and stability during in situ annealing, enabling quantitative analysis and live recording of phase change events. Results show that for an uncapped 100 nm thick GeTe layer, exposure to air after fabrication leads to composition changes which promote heterogeneous nucleation at the oxidized surface. We also demonstrate that protecting the GeTe layer with a 10 nm SiN capping layer prevents nucleation at the surface and allows volume nucleation at a temperature 50 °C higher than the onset of crystallization in the oxidized sample. Our results have important implications regarding the integration of these materials in confined memory cells.

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

Energy Technology Data Exchange (ETDEWEB)

Pickrell, Gary [Virginia Polytechnic Institute & State University, Blacksburg, VA (United States); Scott, Brian [Virginia Polytechnic Institute & State University, Blacksburg, VA (United States)

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

In Situ Ptychography of Heterogeneous Catalysts using Hard X-Rays

DEFF Research Database (Denmark)

Baier, Sina; Damsgaard, Christian Danvad; Scholz, Maria

2016-01-01

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...... 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....

Microstructure and high temperature oxidation resistance of in-situ synthesized TiN/Ti_3Al intermetallic composite coatings on Ti6Al4V alloy by laser cladding process

International Nuclear Information System (INIS)

Liu, Hongxi; Zhang, Xiaowei; Jiang, Yehua; Zhou, Rong

2016-01-01

High temperature anti-oxidation TiN/Ti_3Al intermetallic composite coatings were fabricated with the powder and AlN powder on Ti6Al4V titanium alloy surface by 6 kW transverse-flow CO_2 laser apparatus. The chemical composition, morphology and microstructure of the TiN/Ti_3Al composite coatings were characterized by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometer (EDS). In order to evaluate the high temperature oxidation resistance of TiN/Ti_3Al coating, the isothermal oxidation test was performed in a high temperature resistance furnace at 600 °C and 800 °C, respectively. The result shows that the composite coating has a rapidly solidified fine microstructure consisting of TiN primary phase (granular-like, flake-like or dendrites), with an even distribution in Ti_3Al matrix. It indicates that a physical and chemical reaction between Ti powder and AlN powder has completely occurred under the laser irradiation condition. In addition, the microhardness of the TiN/Ti3Al intermetallic composite coating is 3.4 times higher than that of the Ti6Al4V alloy substrate and reaches 844 HV_0_._2. The high temperature oxidation behavior test reveals that the high temperature oxidation resistance of TiN/Ti_3Al composite coating is much better than that of titanium alloy substrate. The excellent high temperature oxidation resistance of TiN/Ti_3Al intermetallic composite coating is attributed to the formation of reinforced phases TiN, Al_2O_3 and TiO_2. The laser cladding TiN/Ti_3Al intermetallic composite coating is anticipated to be a promising high temperature oxidation resistance coating for Ti6Al4V alloy. - Highlights: • In-situ TiN/Ti_3Al composite coating was synthesized on Ti6Al4V alloy by laser cladding. • The influence of Ti and AlN molar ratio on the microstructure of the coating was studied. • The TiN/Ti_3Al intermetallic coating is mainly composed of α-Ti, TiN and Ti_3Al phases. • The

Crystallization of TiO2 Nanotubes by In Situ Heating TEM

KAUST Repository

Casu, Alberto

2018-01-15

The thermally-induced crystallization of anodically grown TiO2 amorphous nanotubes has been studied so far under ambient pressure conditions by techniques such as differential scanning calorimetry and in situ X-ray diffraction, then looking at the overall response of several thousands of nanotubes in a carpet arrangement. Here we report a study of this phenomenon based on an in situ transmission electron microscopy approach that uses a twofold strategy. First, a group of some tens of TiO2 amorphous nanotubes was heated looking at their electron diffraction pattern change versus temperature, in order to determine both the initial temperature of crystallization and the corresponding crystalline phases. Second, the experiment was repeated on groups of few nanotubes, imaging their structural evolution in the direct space by spherical aberration-corrected high resolution transmission electron microscopy. These studies showed that, differently from what happens under ambient pressure conditions, under the microscope’s high vacuum (p < 10−5 Pa) the crystallization of TiO2 amorphous nanotubes starts from local small seeds of rutile and brookite, which then grow up with the increasing temperature. Besides, the crystallization started at different temperatures, namely 450 and 380 °C, when the in situ heating was performed irradiating the sample with electron beam energy of 120 or 300 keV, respectively. This difference is due to atomic knock-on effects induced by the electron beam with diverse energy.

High Throughput In Situ XAFS Screening of Catalysts

International Nuclear Information System (INIS)

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

2007-01-01

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

In situ electron beam irradiated rapid growth of bismuth nanoparticles in bismuth-based glass dielectrics at room temperature

International Nuclear Information System (INIS)

Singh, Shiv Prakash; Karmakar, Basudeb

2011-01-01

In this study, in situ control growth of bismuth nanoparticles (Bi 0 NPs) was demonstrated in bismuth-based glass dielectrics under an electron beam (EB) irradiation at room temperature. The effects of EB irradiation were investigated in situ using transmission electron microscopy (TEM), selected-area electron diffraction and high-resolution transmission electron microscopy. The EB irradiation for 2–8 min enhanced the construction of bismuth nanoparticles with a rhombohedral structure and diameter of 4–9 nm. The average particle size was found to increase with the irradiation time. Bismuth metal has a melting point of 271 °C and this low melting temperature makes easy the progress of energy induced structural changes during in situ TEM observations. This is a very useful technique in nano-patterning for integrated optics and other applications.

Validation of multi-channel scanning microwave radiometer on-board Oceansat-1

Digital Repository Service at National Institute of Oceanography (India)

Muraleedharan, P.M.; Pankajakshan, T.; Harikrishnan, M.

Sea surface temperature (SST), sea surface wind speed (WS) and columnar water vapour (WV) derived from Multi-frequency Scanning Microwave Radiometer (MSMR) sensor on-board IRS-P4 (Oceansat-1) were validated against the in situ measurements from ship...

High-temperature Raman spectroscopy of solid oxide fuel cell materials and processes.

Science.gov (United States)

Pomfret, Michael B; Owrutsky, Jeffrey C; Walker, Robert A

2006-09-07

Chemical and material processes occurring in high temperature environments are difficult to quantify due to a lack of experimental methods that can probe directly the species present. In this letter, Raman spectroscopy is shown to be capable of identifying in-situ and noninvasively changes in material properties as well as the formation and disappearance of molecular species on surfaces at temperatures of 715 degrees C. The material, yttria-stabilized zirconia or YSZ, and the molecular species, Ni/NiO and nanocrystalline graphite, factor prominently in the chemistry of solid oxide fuel cells (SOFCs). Experiments demonstrate the ability of Raman spectroscopy to follow reversible oxidation/reduction kinetics of Ni/NiO as well as the rate of carbon disappearance when graphite, formed in-situ, is exposed to a weakly oxidizing atmosphere. In addition, the Raman active phonon mode of YSZ shows a temperature dependent shift that correlates closely with the expansion of the lattice parameter, thus providing a convenient internal diagnostic for identifying thermal gradients in high temperature systems. These findings provide direct insight into processes likely to occur in operational SOFCs and motivate the use of in-situ Raman spectroscopy to follow chemical processes in these high-temperature, electrochemically active environments.

An interchangeable scanning Hall probe/scanning SQUID microscope

International Nuclear Information System (INIS)

Tang, Chiu-Chun; Lin, Hui-Ting; Wu, Sing-Lin; Chen, Tse-Jun; Wang, M. J.; Ling, D. C.; Chi, C. C.; Chen, Jeng-Chung

2014-01-01

We have constructed a scanning probe microscope for magnetic imaging, which can function as a scanning Hall probe microscope (SHPM) and as a scanning SQUID microscope (SSM). The scanning scheme, applicable to SHPM and SSM, consists of a mechanical positioning (sub) micron-XY stage and a flexible direct contact to the sample without a feedback control system for the Z-axis. With the interchangeable capability of operating two distinct scanning modes, our microscope can incorporate the advantageous functionalities of the SHPM and SSM with large scan range up to millimeter, high spatial resolution (⩽4 μm), and high field sensitivity in a wide range of temperature (4.2 K-300 K) and magnetic field (10 −7 T-1 T). To demonstrate the capabilities of the system, we present magnetic images scanned with SHPM and SSM, including a RbFeB magnet and a nickel grid pattern at room temperature, surface magnetic domain structures of a La 2/3 Ca 1/3 MnO 3 thin film at 77 K, and superconducting vortices in a striped niobium film at 4.2 K

Low-temperature transitions in cod and tuna determined by differential scanning calorimetry

DEFF Research Database (Denmark)

Jensen, Kristina Nedenskov; Jørgensen, Bo; Nielsen, Jette

2003-01-01

Differential scanning calorimetry measurements have revealed different thermal transitions in cod and tuna samples. Transition temperatures detected Lit -11degreesC, -15degreesC and -21degreesC were highly dependent on the annealing temperature. In tuna muscle an additional transition was observed...... at -72degreesC. This transition appeared differently than the thermal events observed at higher temperatures, as it spanned a broad temperature interval of 25degreesC. The transition was comparable to low-temperature glass transitions reported in protein-rich systems. No transition at this low...... temperature was detected in cod samples. The transitions observed at higher temperatures (-11degreesC to -21degreesC) may possibly stein from a glassy matrix containing muscle proteins. However, the presence of a glass transition at - 11degreesC was in disagreement with the low storage stability at -18degrees...

Versatile variable temperature and magnetic field scanning probe microscope for advanced material research

Science.gov (United States)

Jung, Jin-Oh; Choi, Seokhwan; Lee, Yeonghoon; Kim, Jinwoo; Son, Donghyeon; Lee, Jhinhwan

2017-10-01

We have built a variable temperature scanning probe microscope (SPM) that covers 4.6 K-180 K and up to 7 T whose SPM head fits in a 52 mm bore magnet. It features a temperature-controlled sample stage thermally well isolated from the SPM body in good thermal contact with the liquid helium bath. It has a 7-sample-holder storage carousel at liquid helium temperature for systematic studies using multiple samples and field emission targets intended for spin-polarized spectroscopic-imaging scanning tunneling microscopy (STM) study on samples with various compositions and doping conditions. The system is equipped with a UHV sample preparation chamber and mounted on a two-stage vibration isolation system made of a heavy concrete block and a granite table on pneumatic vibration isolators. A quartz resonator (qPlus)-based non-contact atomic force microscope (AFM) sensor is used for simultaneous STM/AFM operation for research on samples with highly insulating properties such as strongly underdoped cuprates and strongly correlated electron systems.

High spatial resolution and high brightness ion beam probe for in-situ elemental and isotopic analysis

Science.gov (United States)

Long, Tao; Clement, Stephen W. J.; Bao, Zemin; Wang, Peizhi; Tian, Di; Liu, Dunyi

2018-03-01

A high spatial resolution and high brightness ion beam from a cold cathode duoplasmatron source and primary ion optics are presented and applied to in-situ analysis of micro-scale geological material with complex structural and chemical features. The magnetic field in the source as well as the influence of relative permeability of magnetic materials on source performance was simulated using COMSOL to confirm the magnetic field strength of the source. Based on SIMION simulation, a high brightness and high spatial resolution negative ion optical system has been developed to achieve Critical (Gaussian) illumination mode. The ion source and primary column are installed on a new Time-of-Flight secondary ion mass spectrometer for analysis of geological samples. The diameter of the ion beam was measured by the knife-edge method and a scanning electron microscope (SEM). Results show that an O2- beam of ca. 5 μm diameter with a beam intensity of ∼5 nA and an O- beam of ca. 5 μm diameter with a beam intensity of ∼50 nA were obtained, respectively. This design will open new possibilities for in-situ elemental and isotopic analysis in geological studies.

Electrochemical activation of Li2MnO3 at elevated temperature investigated by in situ Raman microscopy

International Nuclear Information System (INIS)

Lanz, Patrick; Villevieille, Claire; Novák, Petr

2013-01-01

Layered-layered oxides of the type xLi 2 MnO 3 ·(1 − x)LiMO 2 (M = Mn, Ni, Co) have been postulated to contain Li 2 MnO 3 domains which, upon electrochemical activation, give rise to a characteristic potential plateau at 4.5 V vs. Li + /Li. To improve our understanding of the complex reaction mechanisms at play, we applied in situ Raman microscopy to investigate the constituent Li 2 MnO 3 . Li 2 MnO 3 synthesised via a two-step solid-state reaction was characterised by scanning electron microscopy and X-ray diffraction. Preliminary electrochemical tests and ex situ Raman microscopy showed the need for elevated temperatures to achieve activation. For the first time, in situ Raman microscopy (at 50 °C) confirmed the activation of Li 2 MnO 3 . The main signal at 615 cm −1 shifted to higher wavenumbers upon charging. After reaching 4.4 V vs. Li + /Li, this shift grew significantly, which is in good agreement with the onset of the potential plateau in both Li 2 MnO 3 and xLi 2 MnO 3 ·(1 − x)LiMO 2 , and is assigned to the partial formation of a spinel-like phase

Application on electrochemistry measurement of high temperature high pressure condition in PWR nuclear power plants

International Nuclear Information System (INIS)

Li Yuchun; Xiao Zhongliang; Jiang Ya; Yu Xiaowei; Pang Feifei; Deng Fenfang; Gao Fan; Zhou Nianguang

2011-01-01

High temperature high pressure electrochemistry testing system was comprehensively analyzed in this paper, according to actual status for supervision in primary and secondary circuits of PWR nuclear power plants. Three research methods were reviewed and discussed for in-situ monitor system. By combination with ECP realtime measurement it was executed for evaluation and water chemistry optimization in nuclear power plants. It is pointed out that in-situ electrochemistry measurement has great potential application for water chemistry evaluation in PWR nuclear power plants. (authors)

Arctic surface temperatures from Metop AVHRR compared to in situ ocean and land data

Directory of Open Access Journals (Sweden)

G. Dybkjær

2012-11-01

Full Text Available The ice surface temperature (IST is an important boundary condition for both atmospheric and ocean and sea ice models and for coupled systems. An operational ice surface temperature product using satellite Metop AVHRR infra-red data was developed for MyOcean. The IST can be mapped in clear sky regions using a split window algorithm specially tuned for sea ice. Clear sky conditions prevail during spring in the Arctic, while persistent cloud cover limits data coverage during summer. The cloud covered regions are detected using the EUMETSAT cloud mask. The Metop IST compares to 2 m temperature at the Greenland ice cap Summit within STD error of 3.14 °C and to Arctic drifting buoy temperature data within STD error of 3.69 °C. A case study reveals that the in situ radiometer data versus satellite IST STD error can be much lower (0.73 °C and that the different in situ measurements complicate the validation. Differences and variability between Metop IST and in situ data are analysed and discussed. An inter-comparison of Metop IST, numerical weather prediction temperatures and in situ observation indicates large biases between the different quantities. Because of the scarcity of conventional surface temperature or surface air temperature data in the Arctic, the satellite IST data with its relatively good coverage can potentially add valuable information to model analysis for the Arctic atmosphere.

Temperature dependence of the in situ widths of a rotating condensate in one dimensional optical potential

International Nuclear Information System (INIS)

Hassan, Ahmed S.; Soliman, Shemi S.M.

2016-01-01

In this paper, a conventional method of quantum statistical mechanics is used to study the temperature dependence of the in situ widths of a rotating condensate bosons in 1D optical potential. We trace the experimentally accessible parameters for which the temperature dependence of the in situ widths becomes perceivable. The calculated results showed that the temperature dependence of the in situ widths is completely different from that of a rotating condensate or trapped bosons in the optical lattice separately. The z-width shows distinct behavior from x- and y-widths due to the rotation effect. The obtained results provide useful qualitative theoretical results for future Bose Einstein condensation experiments in such traps. - Highlights: • The temperature dependence of the in situ widths of a rotating condensate boson in 1D optical potential is investigated. • We trace the experimentally accessible parameters for which the in situ widths become perceivable. • The above mentioned parameters exhibit a characteristic rotation rate and optical potential depth dependence. • Characteristic dependence of the effective widths on temperature is investigated. • Our results provide useful qualitatively and quantitative theoretical results for experiments in various traps.

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

Energy Technology Data Exchange (ETDEWEB)

Chakraborty, R., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu; Serdy, J.; Culpepper, M. L.; Buonassisi, T., E-mail: rupak@alum.mit.edu, E-mail: buonassisi@mit.edu [Department of Mechanical Engineering, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); West, B.; Stuckelberger, M.; Bertoni, M. I. [School of Electrical, Computer and Energy Engineering, Arizona State University, Tempe, Arizona 85287 (United States); Lai, B.; Maser, J. [Advanced Photon Source, Argonne National Laboratory, Argonne, Illinois 60439 (United States)

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.

Distribution Analysis of the Local Critical Temperature and Current Density in YBCO Coated Conductors using Low-temperature Scanning Laser and Hall Probe Microscopy

International Nuclear Information System (INIS)

Park, S. K.; Cho, B. R.; Park, H. Y.; Ri, H. C.

2011-01-01

Distribution of the local critical temperature and current density in YBCO coated conductors were analyzed using Low-temperature Scanning Laser and Hall Probe Microscopy (LTSLHPM). We prepared YBCO coated conductors of various bridge types to study the spatial distribution of the critical temperature and the current density in single and multi bridges. LTSLHPM system was modified for detailed linescan or two-dimensional scan both scanning laser and scanning Hall probe method simultaneously. We analyzed the local critical temperature of single and multi bridges from series of several linescans of scanning laser microscopy. We also investigated local current density and hysteresis curve of single bridge from experimental results of scanning Hall probe microscopy.

Development of micro-four-point probe in a scanning tunneling microscope for in situ electrical transport measurement.

Science.gov (United States)

Ge, Jian-Feng; Liu, Zhi-Long; Gao, Chun-Lei; Qian, Dong; Liu, Canhua; Jia, Jin-Feng

2015-05-01

Electrons at surface may behave differently from those in bulk of a material. Multi-functional tools are essential in comprehensive studies on a crystal surface. Here, we developed an in situ microscopic four-point probe (4PP) transport measurement system on the basis of a scanning tunneling microscope (STM). In particular, convenient replacement between STM tips and micro-4PPs enables systematic investigations of surface morphology, electronic structure, and electrical transport property of a same sample surface. Performances of the instrument are demonstrated with high-quality STM images, tunneling spectra, and low-noise electrical I-V characteristic curves of a single-layer FeSe film grown on a conductive SrTiO3 surface.

Development of micro-four-point probe in a scanning tunneling microscope for in situ electrical transport measurement

Energy Technology Data Exchange (ETDEWEB)

Ge, Jian-Feng; Liu, Zhi-Long; Gao, Chun-Lei; Qian, Dong; Liu, Canhua, E-mail: canhualiu@sjtu.edu.cn, E-mail: jfjia@sjtu.edu.cn; Jia, Jin-Feng, E-mail: canhualiu@sjtu.edu.cn, E-mail: jfjia@sjtu.edu.cn [Key Laboratory of Artificial Structures and Quantum Control (Ministry of Education), Department of Physics and Astronomy, Shanghai Jiao Tong University, 800 Dongchuan Road, Shanghai 200240 (China)

2015-05-15

Electrons at surface may behave differently from those in bulk of a material. Multi-functional tools are essential in comprehensive studies on a crystal surface. Here, we developed an in situ microscopic four-point probe (4PP) transport measurement system on the basis of a scanning tunneling microscope (STM). In particular, convenient replacement between STM tips and micro-4PPs enables systematic investigations of surface morphology, electronic structure, and electrical transport property of a same sample surface. Performances of the instrument are demonstrated with high-quality STM images, tunneling spectra, and low-noise electrical I-V characteristic curves of a single-layer FeSe film grown on a conductive SrTiO{sub 3} surface.

A study of gamma-irradiated polyethylenes by temperature modulated differential scanning calorimetry

Science.gov (United States)

Galovic, S.; Secerov, B.; Trifunovic, S.; Milicevic, D.; Suljovrujic, E.

2012-09-01

Various polyethylenes (PEs) and the effects of high-energy radiation on their structures were widely studied in the past using conventional Differential Scanning Calorimetry (DSC) measurements. In this work, we used the Temperature Modulated Differential Scanning Calorimetry (TMDSC) technique in order to obtain more information about the influence of the initial structural differences and gamma radiation on the evolution in structure and thermal properties of different polyethylenes. For this reason, low density polyethylene (LDPE), linear low density polyethylene (LLDPE) and high density polyethylene (HDPE) samples were exposed to gamma radiation, in air, to a wide range of absorbed doses (up to 2400 kGy). The separation of the total heat flow TMDSC signal into a reversing and non-reversing part enabled us to observe the low-temperature enthalpy relaxation (related to the existence of the "rigid amorphous phase") and recrystallisation processes, as well as to follow their radiation-induced evolution and/or that of melting in a more revealing manner compared to the case of the conventional DSC. Consequently, our results indicate that TMDSC could improve the understanding of radiation-induced effects in polymers.

First results from the in-situ temperature measurements by the newly developed downhole tool during the drilling cruise in the hydrothermal fields of the mid-Okinawa Trough

Science.gov (United States)

Kitada, K.; Wu, H. Y.; Miyazaki, J.; Akiyama, K.; Nozaki, T.; Ishibashi, J. I.; Kumagai, H.; Maeda, L.

2016-12-01

The Okinawa trough is an active backarc basin behind the Ryukyu subduction zone and exhibits active rifting associated with extension of the continental margin. The temperature measurement in this area is essential for understanding hydrothermal system and hydraulic structure. During the CK16-01 cruise this March, we have conducted the in-situ temperature measurements by the newly developed downhole tool, TRDT (Thermo-Resistant Downhole Thermometer) in hydrothermal fields of the mid-Okinawa Trough. The purpose of this measurement is to investigate the in-situ temperature structure in deep-hot zones and its variation after coring and/or drilling. TRDT was designed by JAMSTEC as a memory downhole tool to measure in-situ borehole temperature under the extreme high temperature environment. First trial was conducted in the CK14-04 cruise by the free fall deployment to reduce the operation time. However, there was no temperature data recorded due to the strong vibration during the operation. After CK14-04 cruise, TRDT was modified to improve the function against vibration and shock. The improved TRDT passed the high temperature, vibration and shock tests to ensure the data acquisition of borehole logging. During the CK16-01 cruise, we have first successfully collected the in-situ temperature data from hydrothermal borehole in the Iheya North Knoll with wireline system. The temperature at depth of 187mbsf continued to increase almost linearly from 220 to 245°C during the 20 minute measurements time. This suggests that the inside borehole was cooled down by pumping seawater through drill pipes during the coring and lowering down the TRDT tool to the bottom hole. The in-situ temperature were extrapolated with exponential curve using nonlinear least squares fitting and the estimated equilibrium temperature was 278°C. To recover the in-situ temperature more precisely, the measurement time should kept as long as possible by considering the temperature rating. The operational

An interchangeable scanning Hall probe/scanning SQUID microscope

Energy Technology Data Exchange (ETDEWEB)

Tang, Chiu-Chun; Lin, Hui-Ting; Wu, Sing-Lin [Department of Physics, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Chen, Tse-Jun; Wang, M. J. [Institute of Astronomy and Astrophysics, Academia Sinica, Taipei 10617, Taiwan (China); Ling, D. C. [Department of Physics, Tamkang University, Tamsui Dist., New Taipei City 25137, Taiwan (China); Chi, C. C.; Chen, Jeng-Chung [Department of Physics, National Tsing Hua University, Hsinchu 30013, Taiwan (China); Frontier Research Center on Fundamental and Applied Sciences of Matters, National Tsing Hua University, Hsinchu 30013, Taiwan (China)

2014-08-15

We have constructed a scanning probe microscope for magnetic imaging, which can function as a scanning Hall probe microscope (SHPM) and as a scanning SQUID microscope (SSM). The scanning scheme, applicable to SHPM and SSM, consists of a mechanical positioning (sub) micron-XY stage and a flexible direct contact to the sample without a feedback control system for the Z-axis. With the interchangeable capability of operating two distinct scanning modes, our microscope can incorporate the advantageous functionalities of the SHPM and SSM with large scan range up to millimeter, high spatial resolution (⩽4 μm), and high field sensitivity in a wide range of temperature (4.2 K-300 K) and magnetic field (10{sup −7} T-1 T). To demonstrate the capabilities of the system, we present magnetic images scanned with SHPM and SSM, including a RbFeB magnet and a nickel grid pattern at room temperature, surface magnetic domain structures of a La{sub 2/3}Ca{sub 1/3}MnO{sub 3} thin film at 77 K, and superconducting vortices in a striped niobium film at 4.2 K.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

International Nuclear Information System (INIS)

Taendl, J.; Nambu, S.; Orthacker, A.; Kothleitner, G.; Inoue, J.; Koseki, T.; Poletti, C.

2015-01-01

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al 3 (Sc,Zr) precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.

In-situ observation of recrystallization in an AlMgScZr alloy using confocal laser scanning microscopy

Energy Technology Data Exchange (ETDEWEB)

Taendl, J., E-mail: johannes.taendl@tugraz.atl [Institute of Materials Science and Welding, Graz University of Technology, Graz (Austria); Nambu, S. [Department of Materials Engineering, The University of Tokyo, Tokyo 113-8656 (Japan); Orthacker, A.; Kothleitner, G. [Institute of Electron Microscopy and Nanoanalysis, Graz University of Technology, Graz (Austria); Graz Center for Electron Microscopy, Graz (Austria); Inoue, J.; Koseki, T. [Department of Materials Engineering, The University of Tokyo, Tokyo 113-8656 (Japan); Poletti, C. [Institute of Materials Science and Welding, Graz University of Technology, Graz (Austria)

2015-10-15

In this work we present a novel in-situ approach to study the recrystallization behavior of age hardening alloys. We use confocal laser scanning microscopy (CLSM) at 400 °C to investigate the static recrystallization of an AlMg4Sc0.4Zr0.12 alloy in-situ. The results are combined with electron backscatter diffraction (EBSD) and transmission electron microscopy (TEM) analyses. It was found that CLSM is a powerful tool to visualize both the local initiation and temporal sequence of recrystallization. After fast nucleation and initial growth, the grain growth rate decreases and the grain boundary migration stops after some minutes due to Zener pinning from Al{sub 3}(Sc,Zr) precipitates produced during the heat treatment. EBSD and TEM analyses confirm both the boundary movements and the particle-boundary interactions. - Highlights: • First time that CLSM is used to study recrystallization in-situ. • The start and end of recrystallization can be directly observed. • The procedure is easy to apply and requires only simple data interpretation. • In-situ observations on the surface correlate to modifications inside the bulk. • In-situ observations correlate to EBSD and EFTEM analyses.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Energy Technology Data Exchange (ETDEWEB)

Axford, Danny [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Foadi, James [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Imperial College London, London SW7 2AZ (United Kingdom); Hu, Nien-Jen; Choudhury, Hassanul Ghani [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Imperial College London, London SW7 2AZ (United Kingdom); Rutherford Appleton Laboratory, Oxfordshire OX11 0FA (United Kingdom); Iwata, So [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Imperial College London, London SW7 2AZ (United Kingdom); Rutherford Appleton Laboratory, Oxfordshire OX11 0FA (United Kingdom); Kyoto University, Kyoto 606-8501 (Japan); Beis, Konstantinos [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Imperial College London, London SW7 2AZ (United Kingdom); Rutherford Appleton Laboratory, Oxfordshire OX11 0FA (United Kingdom); Evans, Gwyndaf, E-mail: gwyndaf.evans@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Alguel, Yilmaz, E-mail: gwyndaf.evans@diamond.ac.uk [Diamond Light Source, Harwell Science and Innovation Campus, Oxfordshire OX11 0DE (United Kingdom); Imperial College London, London SW7 2AZ (United Kingdom); Rutherford Appleton Laboratory, Oxfordshire OX11 0FA (United Kingdom)

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.

In-situ deposition of YBCO high-Tc superconducting thin films by MOCVD and PE-MOCVD

International Nuclear Information System (INIS)

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

1991-01-01

Metal-Organic Chemical Vapor Deposition (MOCVD) offers the advantages of a high degree of compositional control, adaptability for large scale production, and the potential for low temperature fabrication. The capability of operating at high oxygen partial pressure is particularly suitable for in situ formation of high temperature superconducting (HTSC) films. Yttrium barium copper oxide (YBCO) thin films having a sharp zero-resistance transition with T(sub c) greater than 90 K and J(sub c) of approximately 10(exp 4) A on YSZ have been prepared, in situ, at a substrate temperature of about 800 C. Moreover, the ability to form oxide films at low temperature is very desirable for device applications of HTSC materials. Such a process would permit the deposition of high quality HTSC films with a smooth surface on a variety of substrates. Highly c-axis oriented, dense, scratch resistant, superconducting YBCO thin films with mirror-like surfaces have been prepared, in situ, at a reduced substrate temperature as low as 570 C by a remote microwave-plasma enhanced metal-organic chemical vapor deposition (PE-MOCVD) process. Nitrous oxide was used as a reactant gas to generate active oxidizing species. This process, for the first time, allows the formation of YBCO thin films with the orthorhombic superconducting phase in the as-deposited state. The as-deposited films grown by PE-MOCVD show attainment of zero resistance at 72 K with a transition width of about 5 K. MOCVD was carried out in a commercial production scale reactor with the capability of uniform deposition over 100 sq cm per growth run. Preliminary results indicate that PE-MOCVD is a very attractive thin film deposition process for superconducting device technology

Long-Term Water Temperature Variations in Daya Bay, China Using Satellite and In Situ Observations

Directory of Open Access Journals (Sweden)

Jing Yu

2010-01-01

Full Text Available Daya Bay is a shallow, semi-en closed bay in the northern section of the South China Sea. The present study analyzed variations of water temperature in Daya Bay over the past 21 years (1985 - 2005 using Advanced Very High Resolution Radiometer (AVHRR satellite remote sensing data and in situ observations. Results showed that AVHRR readings of sea surface temperature (SST increased by 0.07°C y-1. Linear regression anal y sis for monthly SST anomalies (SSTA showed a shift from negative to positive from 1995 - 1996, when the Daya Bay nuclear power station commenced operations in 1994. The slope of linear regression analysis for SSTA nearly doubled from 0.05 (1985 - 1993 to 0.09 (1994 - 2005. Monthly AVHRR images showed a thermal plume from the power station and revealed the in crease of SST over 21 years. In situ observations in water temperature also showed an in creasing trend for the same period (1985 - 2005. Variations in water temperature in Daya Bay were connected with climatic perturbations and in creasing human activity including thermal discharge from nuclear power stations and the rapid economic development around the bay area.

A novel and compact nanoindentation device for in situ nanoindentation tests inside the scanning electron microscope

Directory of Open Access Journals (Sweden)

Hu Huang

2012-03-01

Full Text Available In situ nanomechanical tests provide a unique insight into mechanical behaviors of materials, such as fracture onset and crack propagation, shear band formation and so on. This paper presents a novel in situ nanoindentation device with dimensions of 103mm×74mm×60mm. Integrating the stepper motor, the piezoelectric actuator and the flexure hinge, the device can realize coarse adjustment of the specimen and precision loading and unloading of the indenter automatically. A novel indenter holder was designed to guarantee that the indenter penetrates into and withdraws from the specimen surface vertically. Closed-loop control of the indentation process was established to solve the problem of nonlinearity of the piezoelectric actuator and to enrich the loading modes. The in situ indentation test of Indium Phosphide (InP inside the scanning electron microscope (SEM was carried out and the experimental result indicates the feasibility of the developed device.

High Temperature Fuel Cladding Chemical Interactions Between TRIGA Fuels and 304 Stainless Steel

Energy Technology Data Exchange (ETDEWEB)

Perez, Emmanuel [Idaho National Lab. (INL), Idaho Falls, ID (United States); Keiser, Jr., Dennis D. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Forsmann, Bryan [Boise State Univ., ID (United States); Janney, Dawn E. [Idaho National Lab. (INL), Idaho Falls, ID (United States); Henley, Jody [Idaho National Lab. (INL), Idaho Falls, ID (United States); Woolstenhulme, Eric C. [Idaho National Lab. (INL), Idaho Falls, ID (United States)

2016-02-01

High-temperature fuel-cladding chemical interactions (FCCI) between TRIGA (Training, Research, Isotopes, General Atomics) fuel elements and the 304 stainless steel (304SS) are of interest to develop an understanding of the fuel behavior during transient reactor scenarios. TRIGA fuels are composed of uranium (U) particles dispersed in a zirconium-hydride (Zr-H) matrix. In reactor, the fuel is encased in 304-stainless-steel (304SS) or Incoloy 800 clad tubes. At high temperatures, the fuel can readily interact with the cladding, resulting in FCCI. A number of FCCI can take place in this system. Interactions can be expected between the cladding and the Zr-H matrix, and/or between the cladding and the U-particles. Other interactions may be expected between the Zr-H matrix and the U-particles. Furthermore, the fuel contains erbium-oxide (Er-O) additions. Interactions can also be expected between the Er-O, the cladding, the Zr-H and the U-particles. The overall result is that very complex interactions may take place as a result of fuel and cladding exposures to high temperatures. This report discusses the characterization of the baseline fuel microstructure in the as-received state (prior to exposure to high temperature), characterization of the fuel after annealing at 950C for 24 hours and the results from diffusion couple experiments carries out at 1000C for 5 and 24 hours. Characterization was carried out via scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with sample preparation via focused ion beam in situ-liftout-technique.

High Temperature Fuel Cladding Chemical Interactions Between TRIGA Fuels and 304 Stainless Steel

International Nuclear Information System (INIS)

Perez, Emmanuel; Keiser Jr, Dennis D.; Forsmann, Bryan; Janney, Dawn E.; Henley, Jody; Woolstenhulme, Eric C.

2016-01-01

High-temperature fuel-cladding chemical interactions (FCCI) between TRIGA (Training, Research, Isotopes, General Atomics) fuel elements and the 304 stainless steel (304SS) are of interest to develop an understanding of the fuel behavior during transient reactor scenarios. TRIGA fuels are composed of uranium (U) particles dispersed in a zirconium-hydride (Zr-H) matrix. In reactor, the fuel is encased in 304-stainless-steel (304SS) or Incoloy 800 clad tubes. At high temperatures, the fuel can readily interact with the cladding, resulting in FCCI. A number of FCCI can take place in this system. Interactions can be expected between the cladding and the Zr-H matrix, and/or between the cladding and the U-particles. Other interactions may be expected between the Zr-H matrix and the U-particles. Furthermore, the fuel contains erbium-oxide (Er-O) additions. Interactions can also be expected between the Er-O, the cladding, the Zr-H and the U-particles. The overall result is that very complex interactions may take place as a result of fuel and cladding exposures to high temperatures. This report discusses the characterization of the baseline fuel microstructure in the as-received state (prior to exposure to high temperature), characterization of the fuel after annealing at 950C for 24 hours and the results from diffusion couple experiments carries out at 1000C for 5 and 24 hours. Characterization was carried out via scanning electron microscopy (SEM) and transmission electron microscopy (TEM) with sample preparation via focused ion beam in situ-liftout-technique.

Application of piezoceramic materials in low temperature scanning tunnel microscope

International Nuclear Information System (INIS)

Volodin, A.P.; Panich, A.E.

1989-01-01

Temperature dependences of the voltage-to-movement conversion coefficients for piezoceramic domestic materials PKR and TsTS-19 are measured using a capacitance dilatometer in the 0.4< T<300K temperature range. Anisotropy of thermal expansion of materials determined by the polarization vector is observed. Some recommendations concerning the use of the given materials in low-temperature scanning tunnel microscopes are given

9% Cr steel high temperature oxidation. Solutions investigated for improving corrosion resistance of the steel

Energy Technology Data Exchange (ETDEWEB)

Evin, Harold Nicolas; Heintz, Olivier; Chevalier, Sebastien [UMR 5209 CNRS-Bourgogne Univ. (France). Lab. Interdisciplinaire Carnot de Bourgogne; Foejer, Cecilia; Jakani, Saad; Dhont, Annick; Claessens, Serge [OCAS N.V. ArcelorMittal Global R and D, Gent (Belgium)

2010-07-01

The improvement of high temperature oxidation resistance of low chromium content steels, such as T/P91, is of great interest in regards with their application in thermal power generating plants. Indeed, they possess good creep properties, but are facing their limits of use at temperature higher than 600 C, due to accelerated corrosion phenomena. Good knowledge of the mechanisms involved during their oxidation process is needed to prevent the degradation of the materials and to extend life time of the power plants components. Oxide layers thermally grown, on 9% Cr steels (provided by OCAS N.V), during isothermal tests between 600 C and 750 C in laboratory air under atmospheric pressure were investigated, by Scanning Electron Microscopy (SEM) and X-ray diffraction (XRD). The oxidation behaviour appeared very limited at 750 C, due to the presence of a breakaway, which can be linked to iron porous oxide grown over the surface of the samples. ''In situ'' X-ray Photoelectron spectroscopy (XPS) analyses were performed in air at 600 C after short exposures (between 5 min and 25 h). A complex mixture of iron oxide, Cr{sub 2}O{sub 3} and Cr (VI) species were characterized in the scales. The in-situ analyses were compared and related to XPS analyses performed on thick oxide scales formed on samples oxidized in air at 600 C for 100h. An oxidation mechanism is then proposed to understand the oxide scale growth in the temperature range 600 - 750 C. The second step of this study consists in improving the high temperature corrosion resistance of these steels without modifying their mechanical properties. Thus several solutions were investigated such as MOCVD coatings, pack cementation coatings, and tested in cycle conditions prior. (orig.)

On the Frequency Correction in Temperature-Modulated Differential Scanning Calorimetry of Glass Transition

DEFF Research Database (Denmark)

Guo, Xiaoju; Mauro, J.C.; Allan, D.C.

2012-01-01

Temperature-modulated differential scanning calorimetry (TMDSC) is based on conventional DSC but with a sinusoidally modulated temperature path. Simulations of TMDSC signals were performed for Corning EAGLE XG® glass over a wide range of modulation frequencies. Our results reveal that the frequency...... correction commonly used in the interpretation of TMDSC signals leads to a master nonreversing heat flow curve independent of modulation frequency, provided that sufficiently high frequencies are employed in the TMDSC measurement. A master reversing heat flow curve can also be generated through the frequency...

Novel High Temperature Materials for In-Situ Sensing Devices

Energy Technology Data Exchange (ETDEWEB)

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

In-situ investigation of the icosahedral Al-Cu-Fe phase formation in thin films

Energy Technology Data Exchange (ETDEWEB)

Haidara, F., E-mail: fanta.haidara@im2np.fr [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France); Duployer, B. [Universite Paul Sabatier CIRIMAT-LCMIE 2R1, 118, Route de Narbonne, 31062 Toulouse Cedex 09 (France); Mangelinck, D.; Record, M.-C. [IM2NP, UMR 6242 CNRS - Universite Aix-Marseille, Av. Escadrille Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France)

2012-09-05

Highlights: Black-Right-Pointing-Pointer We investigated the phase formation of i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} in thin films. Black-Right-Pointing-Pointer We characterized the samples by DSC and in-situ XRD and resistance measurements. Black-Right-Pointing-Pointer The resistivity value for i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5} was determined. - Abstract: This work is an investigation of the formation by reactive diffusion at high temperatures of the icosahedral phase, i-Al{sub 62.5}Cu{sub 25}Fe{sub 12.5}, in thin films. The samples were prepared by sputtering at room temperature. The elements Al, Cu and Fe were sequentially deposited onto oxidized silicon substrates. The two following stacking sequences, Al/Cu/Fe and Al/Fe/Cu, were investigated. The phase formation was studied using in situ resistivity, in situ X-ray Diffraction and Differential Scanning Calorimetry measurements. Whatever the stacking sequence, the sequences of phase formation evidenced during the heating treatment are similar. However the temperatures of formation for the first phases that are formed are different; they are higher in the case of the Al/Fe/Cu stacking sequence.

Effects of deposition temperature and in-situ annealing time on structure and magnetic properties of (001) orientation FePt films

International Nuclear Information System (INIS)

Yu, Yongsheng; George, T.A.; Li, Haibo; Sun, Daqian; Ren, Zhenan; Sellmyer, D.J.

2013-01-01

FePt films were prepared on (100) oriented single crystal MgO substrates at high temperature ranging from 620 until 800 °C and in-situ annealed for different times ranging from 0 to 60 min to obtain ordered FePt films. The structural analysis indicates that FePt films grow epitaxially on MgO (100) substrates. Both increasing deposition temperature and in-situ annealing time enhance the (001) texture and ordering of FePt films. The magnetic analysis shows that these L1 0 FePt films have perpendicular anisotropy and the easy magnetization c-axis is perpendicular to the film plane. Magnetization reversal is controlled by a rotational mechanism. The hard magnetic properties of the films are improved with increasing deposition temperature or in-situ annealing time. - Highlights: ► The paper reports the texture and magnetic evolution of FePt films deposited on MgO substrates. ► Increasing deposition temperature or annealing time enhanced the texture and ordering. ► The magnetic analysis shows L1 0 FePt films have perpendicular anisotropy.

Consecutive Short-Scan CT for Geological Structure Analog Models with Large Size on In-Situ Stage.

Science.gov (United States)

Yang, Min; Zhang, Wen; Wu, Xiaojun; Wei, Dongtao; Zhao, Yixin; Zhao, Gang; Han, Xu; Zhang, Shunli

2016-01-01

For the analysis of interior geometry and property changes of a large-sized analog model during a loading or other medium (water or oil) injection process with a non-destructive way, a consecutive X-ray computed tomography (XCT) short-scan method is developed to realize an in-situ tomography imaging. With this method, the X-ray tube and detector rotate 270° around the center of the guide rail synchronously by switching positive and negative directions alternately on the way of translation until all the needed cross-sectional slices are obtained. Compared with traditional industrial XCTs, this method well solves the winding problems of high voltage cables and oil cooling service pipes during the course of rotation, also promotes the convenience of the installation of high voltage generator and cooling system. Furthermore, hardware costs are also significantly decreased. This kind of scanner has higher spatial resolution and penetrating ability than medical XCTs. To obtain an effective sinogram which matches rotation angles accurately, a structural similarity based method is applied to elimination of invalid projection data which do not contribute to the image reconstruction. Finally, on the basis of geometrical symmetry property of fan-beam CT scanning, a whole sinogram filling a full 360° range is produced and a standard filtered back-projection (FBP) algorithm is performed to reconstruct artifacts-free images.

Design and performance of an ultra-high vacuum spin-polarized scanning tunneling microscope operating at 30 mK and in a vector magnetic field.

Science.gov (United States)

von Allwörden, Henning; Eich, Andreas; Knol, Elze J; Hermenau, Jan; Sonntag, Andreas; Gerritsen, Jan W; Wegner, Daniel; Khajetoorians, Alexander A

2018-03-01

We describe the design and performance of a scanning tunneling microscope (STM) that operates at a base temperature of 30 mK in a vector magnetic field. The cryogenics is based on an ultra-high vacuum (UHV) top-loading wet dilution refrigerator that contains a vector magnet allowing for fields up to 9 T perpendicular and 4 T parallel to the sample. The STM is placed in a multi-chamber UHV system, which allows in situ preparation and exchange of samples and tips. The entire system rests on a 150-ton concrete block suspended by pneumatic isolators, which is housed in an acoustically isolated and electromagnetically shielded laboratory optimized for extremely low noise scanning probe measurements. We demonstrate the overall performance by illustrating atomic resolution and quasiparticle interference imaging and detail the vibrational noise of both the laboratory and microscope. We also determine the electron temperature via measurement of the superconducting gap of Re(0001) and illustrate magnetic field-dependent measurements of the spin excitations of individual Fe atoms on Pt(111). Finally, we demonstrate spin resolution by imaging the magnetic structure of the Fe double layer on W(110).

Design and performance of an ultra-high vacuum spin-polarized scanning tunneling microscope operating at 30 mK and in a vector magnetic field

Science.gov (United States)

von Allwörden, Henning; Eich, Andreas; Knol, Elze J.; Hermenau, Jan; Sonntag, Andreas; Gerritsen, Jan W.; Wegner, Daniel; Khajetoorians, Alexander A.

2018-03-01

We describe the design and performance of a scanning tunneling microscope (STM) that operates at a base temperature of 30 mK in a vector magnetic field. The cryogenics is based on an ultra-high vacuum (UHV) top-loading wet dilution refrigerator that contains a vector magnet allowing for fields up to 9 T perpendicular and 4 T parallel to the sample. The STM is placed in a multi-chamber UHV system, which allows in situ preparation and exchange of samples and tips. The entire system rests on a 150-ton concrete block suspended by pneumatic isolators, which is housed in an acoustically isolated and electromagnetically shielded laboratory optimized for extremely low noise scanning probe measurements. We demonstrate the overall performance by illustrating atomic resolution and quasiparticle interference imaging and detail the vibrational noise of both the laboratory and microscope. We also determine the electron temperature via measurement of the superconducting gap of Re(0001) and illustrate magnetic field-dependent measurements of the spin excitations of individual Fe atoms on Pt(111). Finally, we demonstrate spin resolution by imaging the magnetic structure of the Fe double layer on W(110).

Effects of temperature and loading speed on interface-dominated strength in fibre/polymer composites: An evaluation for in-situ environment

International Nuclear Information System (INIS)

Sethi, Sanghamitra; Rathore, Dinesh Kumar; Ray, Bankim Chandra

2015-01-01

Graphical abstract: Some microcracks turn to potential cracks at low loading rates and cause significant reduction in interlaminar shear strength of the composite system while as the loading rate increases the time available to propagate the microcracks is less. This can be attributed to higher ILSS at higher loading rates at these above-ambient temperatures. - Highlights: • Effect of temperature and loading rate has been studied. • Three different types of fibres are used for fabrication. • Flexural and fractography behaviour were studied. • T g was affected by types of fibre and matrix used. - Abstract: The present investigation intends to study the influence of crosshead velocity and in-situ environmental conditioning i.e. high temperature and cryogenic temperature on micromechanical performance of glass fibre/epoxy, carbon fibre/epoxy and Kevlar fibre/epoxy polymer composites. 3-point short beam shear tests were conducted on the conditioned specimens to evaluate the interfacial properties and failure modes which are related to mechanical properties of the composites. The effect of crosshead velocity (within the range 1-10 3 mm/min) on the interlaminar shear strength (ILSS) of all the three composite systems at different temperatures was studied. The glass transition temperature (T g ) of conditioned samples were measured by differential scanning calorimetry (DSC) in the temperature range of 25 °C to 150 °C temperature. At 1 mm/min loading rate, for both glass/epoxy and carbon/epoxy composites maximum increase in ILSS value was about 85.72% with respect to ambient, while for Kevlar/epoxy composite 31.77% reduction in ILSS was observed at -100 °C temperature

Two-dimensional in situ metrology of X-ray mirrors using the speckle scanning technique

Energy Technology Data Exchange (ETDEWEB)

Wang, Hongchang, E-mail: hongchang.wang@diamond.ac.uk; Kashyap, Yogesh; Laundy, David; Sawhney, Kawal [Diamond Light Source Ltd, Harwell Science and Innovation Campus, Didcot OX11 0DE (United Kingdom)

2015-06-06

The two-dimensional slope error of an X-ray mirror has been retrieved by employing the speckle scanning technique, which will be valuable at synchrotron radiation facilities and in astronomical telescopes. In situ metrology overcomes many of the limitations of existing metrology techniques and is capable of exceeding the performance of present-day optics. A novel technique for precisely characterizing an X-ray bimorph mirror and deducing its two-dimensional (2D) slope error map is presented. This technique has also been used to perform fast optimization of a bimorph mirror using the derived 2D piezo response functions. The measured focused beam size was significantly reduced after the optimization, and the slope error map was then verified by using geometrical optics to simulate the focused beam profile. This proposed technique is expected to be valuable for in situ metrology of X-ray mirrors at synchrotron radiation facilities and in astronomical telescopes.

In situ investigation of the tensile deformation of laser welded Ti{sub 2}AlNb joints

Energy Technology Data Exchange (ETDEWEB)

Zhang, Kezhao; Ni, Longchang; Lei, Zhenglong, E-mail: leizhenglong@hit.edu.cn; Chen, Yanbin; Hu, Xue

2017-01-15

The tensile deformation behavior of laser welded Ti{sub 2}AlNb joints was investigated using in situ analysis methods. The fracture mode of the single-B2-phase fusion zone was quasi-cleavage at room temperature and intergranular at 650 °C, while that of base metal was microvoid coalescence at both room temperature and 650 °C. Tensile deformation at room temperature was observed using in situ SEM tensile testing. In base metal, microcracks nucleated and propagated mainly within the O phase or along O/B2 phase boundaries. While both the cross- and multi-slips were found in the single-B2-phase fusion zone, a confocal laser scanning microscopy was used to observe the crack initiation and propagation process in situ at 650 °C. Cracks mainly formed along the B2/O phase boundaries in base metal, along the fragile grain boundaries of B2 phase in the fusion zone. The thermal simulation experiment and following TEM analysis indicated that the precipitation of continuous O-phase films along the B2 grain boundaries resulted in the high temperature brittleness of laser welded Ti{sub 2}AlNb joints. - Highlights: •Cracks formed within O phase or along B2/O boundaries in the base metal. •Cross- and multi-slips relieved stress in the fusion zone at room temperature. •Cracks mainly formed along the B2/O boundaries at 650 °C. •In the fusion zone, intergranular cracks were in situ observed at 650 °C. •O-phase films along B2 grain boundaries caused the high temperature brittleness.

Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

Science.gov (United States)

Willa, K.; Diao, Z.; Campanini, D.; Welp, U.; Divan, R.; Hudl, M.; Islam, Z.; Kwok, W.-K.; Rydh, A.

2017-12-01

Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-δ crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

The interval high rate discharge behavior of Li3V2(PO4)3/C cathode based on in situ polymerization method

International Nuclear Information System (INIS)

Mao, Wen-feng; Yan, Ji; Xie, Hui; Tang, Zhi-yuan; Xu, Qiang

2013-01-01

An in situ polymerization assisted fast sol–gel method was introduced to synthesize high performance Li 3 V 2 PO 4 /C (LVP/C) cathode material. The crystal structure, surface morphology and electrochemical performances of the LVP/C samples sintered at different temperatures were investigated. The composite sintered at 750 °C exhibits the highest specific discharge capacity of 119.02 mAh g −1 (440.35 Wh g −1 ) at 10 C rate. The Li + diffusion coefficient ranges from 10 −6 to 10 −8 cm 2 s −1 based on different scanning rates and the electronic conductivity is about 10 −5 S cm −1 . For comparison, an ex situ polymerization method was also employed to obtain the LVP/C composite. A novel charge/discharge testing mode was designed to investigate the electrochemical behavior of the as-prepared LVP/C composite for practical application in electric vehicle cells. The obtained high power density and the special testing mode prove the LVP/C composite would be a promising candidate for the electric vehicle application and deserves further investigation

In situ tensile testing of individual Co nanowires inside a scanning electron microscope

International Nuclear Information System (INIS)

Zhang Dongfeng; Breguet, Jean-Marc; Clavel, Reymond; Phillippe, Laetitia; Utke, Ivo; Michler, Johann

2009-01-01

Uniaxial quasi-static tensile testing on individual nanocrystalline Co nanowires (NWs), synthesized by electrochemical deposition process (EDP) in porous templates, was performed inside a scanning electron microscope (SEM) using a microfabricated tensile stage consisting of a comb drive actuator and a clamped-clamped beam force sensor. A 'three-beam structure' was fabricated by focused ion beam induced deposition (FIBID) on the stage, from which the specimen elongation and the tensile force could be measured simultaneously from SEM images at high magnification. A novel strategy of modifying device topography, e.g. in the form of trenches and pillars, was proposed to facilitate in situ SEM pick-and-place nanomanipulation, which could achieve a high yield of about 80% and reduce the difficulties in specimen preparation for tensile testing at the nanoscale. The measured apparent Young's modulus (75.3 ± 14.6) GPa and tensile strength (1.6 ± 0.4) GPa are significantly lower than the bulk modulus and the theoretical strength of monocrystalline samples, respectively. This result is important for designing Co NW-based devices. The origins of these distinctions are discussed in terms of the stiffnesses of the soldering portions, specimen misalignment, microstructure of the NWs and the experimental measurement uncertainty.

Parallelism between gradient temperature raman spectroscopy and differential scanning calorimetry results

Science.gov (United States)

Temperature dependent Raman spectroscopy (TDR) applies the temperature gradients utilized in differential scanning calorimetry (DSC) to Raman spectroscopy, providing a straightforward technique to identify molecular rearrangements that occur just prior to phase transitions. Herein we apply TDR and D...

Structural stability of high entropy alloys under pressure and temperature

DEFF Research Database (Denmark)

Ahmad, Azkar S.; Su, Y.; Liu, S. Y.

2017-01-01

The stability of high-entropy alloys (HEAs) is a key issue before their selection for industrial applications. In this study, in-situ high-pressure and high-temperature synchrotron radiation X-ray diffraction experiments have been performed on three typical HEAs Ni20Co20Fe20Mn20Cr20, Hf25Nb25Zr25Ti...

Biocatalytic hydroxylation of n-butane with in situ cofactor regeneration at low temperature and under normal pressure

Directory of Open Access Journals (Sweden)

Svenja Staudt

2012-02-01

Full Text Available The hydroxylation of n-alkanes, which proceeds in the presence of a P450-monooxygenase advantageously at temperatures significantly below room temperature, is described. In addition, an enzymatic hydroxylation of the “liquid gas” n-butane with in situ cofactor regeneration, which does not require high-pressure conditions, was developed. The resulting 2-butanol was obtained as the only regioisomer, at a product concentration of 0.16 g/L.

Holocene Temperature Reconstructions from Arctic Lakes based on Alkenone Paleothermometry and Non-Destructive Scanning Techniques

Science.gov (United States)

D'Andrea, W. J.; Balascio, N. L.; Bradley, R. S.; Bakke, J.; Gjerde, M.; Kaufman, D. S.; Briner, J. P.; von Gunten, L.

2014-12-01

Generating continuous, accurate and quantitative Holocene temperature estimates from the Arctic is an ongoing challenge. In many Arctic regions, tree ring-based approaches cannot be used and lake sediments provide the most valuable repositories for extracting paleotemperature information. Advances in lacustrine alkenone paleothermometry now allow for quantitative reconstruction of lake-water temperature based on the UK37 values of sedimentary alkenones. In addition, a recent study demonstrated the efficacy of non-destructive scanning reflectance spectroscopy in the visible range (VIS-RS) for high-resolution quantitative temperature reconstruction from arctic lake sediments1. In this presentation, I will report a new UK37-based temperature reconstruction and a scanning VIS-RS record (using the RABD660;670 index as a measure of sedimentary chlorin content) from Kulusuk Lake in southeastern Greenland (65.6°N, 37.1°W). The UK37 record reveals a ~3°C increase in summer lake water temperatures between ~10ka and ~7ka followed by sustained warmth until ~4ka and a gradual (~3°C) cooling until ~400 yr BP. The strong correlation between UK37 and RABD660;670 measured in the same sediment core provides further evidence that in arctic lakes where temperature regulates primary productivity, and thereby sedimentary chlorin content, these proxies can be combined to develop high-resolution quantitative temperature records. The Holocene temperature history of Kulusuk Lake determined using this approach corresponds to changes in the size of the glaciers adjacent to the lake, as inferred from sediment minerogenic properties measured with scanning XRF. Glaciers retreated during early Holocene warming, likely disappeared during the period of mid-Holocene warmth, and advanced after 4ka. I will also discuss new UK37 and RABD660;670 reconstructions from northwestern Svalbard and the central Brooks Range of Alaska within the framework of published regional temperature reconstructions and

High-Speed Scanning Interferometer Using CMOS Image Sensor and FPGA Based on Multifrequency Phase-Tracking Detection

Science.gov (United States)

Ohara, Tetsuo

2012-01-01

A sub-aperture stitching optical interferometer can provide a cost-effective solution for an in situ metrology tool for large optics; however, the currently available technologies are not suitable for high-speed and real-time continuous scan. NanoWave s SPPE (Scanning Probe Position Encoder) has been proven to exhibit excellent stability and sub-nanometer precision with a large dynamic range. This same technology can transform many optical interferometers into real-time subnanometer precision tools with only minor modification. The proposed field-programmable gate array (FPGA) signal processing concept, coupled with a new-generation, high-speed, mega-pixel CMOS (complementary metal-oxide semiconductor) image sensor, enables high speed (>1 m/s) and real-time continuous surface profiling that is insensitive to variation of pixel sensitivity and/or optical transmission/reflection. This is especially useful for large optics surface profiling.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

International Nuclear Information System (INIS)

Iezzi, F; Todisco, M T

2015-01-01

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

Microstructure and high temperature oxidation resistance of in-situ synthesized TiN/Ti{sub 3}Al intermetallic composite coatings on Ti6Al4V alloy by laser cladding process

Energy Technology Data Exchange (ETDEWEB)

Liu, Hongxi, E-mail: piiiliuhx@sina.com; Zhang, Xiaowei; Jiang, Yehua; Zhou, Rong

2016-06-15

High temperature anti-oxidation TiN/Ti{sub 3}Al intermetallic composite coatings were fabricated with the powder and AlN powder on Ti6Al4V titanium alloy surface by 6 kW transverse-flow CO{sub 2} laser apparatus. The chemical composition, morphology and microstructure of the TiN/Ti{sub 3}Al composite coatings were characterized by optical microscopy (OM), scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectrometer (EDS). In order to evaluate the high temperature oxidation resistance of TiN/Ti{sub 3}Al coating, the isothermal oxidation test was performed in a high temperature resistance furnace at 600 °C and 800 °C, respectively. The result shows that the composite coating has a rapidly solidified fine microstructure consisting of TiN primary phase (granular-like, flake-like or dendrites), with an even distribution in Ti{sub 3}Al matrix. It indicates that a physical and chemical reaction between Ti powder and AlN powder has completely occurred under the laser irradiation condition. In addition, the microhardness of the TiN/Ti3Al intermetallic composite coating is 3.4 times higher than that of the Ti6Al4V alloy substrate and reaches 844 HV{sub 0.2}. The high temperature oxidation behavior test reveals that the high temperature oxidation resistance of TiN/Ti{sub 3}Al composite coating is much better than that of titanium alloy substrate. The excellent high temperature oxidation resistance of TiN/Ti{sub 3}Al intermetallic composite coating is attributed to the formation of reinforced phases TiN, Al{sub 2}O{sub 3} and TiO{sub 2}. The laser cladding TiN/Ti{sub 3}Al intermetallic composite coating is anticipated to be a promising high temperature oxidation resistance coating for Ti6Al4V alloy. - Highlights: • In-situ TiN/Ti{sub 3}Al composite coating was synthesized on Ti6Al4V alloy by laser cladding. • The influence of Ti and AlN molar ratio on the microstructure of the coating was studied. • The TiN/Ti{sub 3}Al intermetallic

Oxygen partial pressure control during in-situ high temperature X-ray diffraction on cerium dioxide

International Nuclear Information System (INIS)

Strach, M.; Belin, R.C.; Richaud, J-C.; Rogez, J.

2014-01-01

Cerium dioxide is widely used as a surrogate for plutonium dioxide in the studies of MOX type nuclear fuel. Thus, obtaining an accurate description of the structures present in this system in a range of temperatures is of importance to the development of fuel for the IV. generation of nuclear reactors. However, such a study requires appropriate scientific tools, in particular regarding the control and monitoring of the oxygen partial pressure (pO 2 ). Here we discuss several in-situ X-ray diffraction experiments performed to determine the phases present in the hypo-stoichiometric CeO 2-x region of the phase diagram and clearly demonstrate the need for controlling the pO 2 . (authors)

Measurement needs guided by synthetic radar scans in high-resolution model output

Science.gov (United States)

Varble, A.; Nesbitt, S. W.; Borque, P.

2017-12-01

Microphysical and dynamical process interactions within deep convective clouds are not well understood, partly because measurement strategies often focus on statistics of cloud state rather than cloud processes. While processes cannot be directly measured, they can be inferred with sufficiently frequent and detailed scanning radar measurements focused on the life cycleof individual cloud regions. This is a primary goal of the 2018-19 DOE ARM Cloud, Aerosol, and Complex Terrain Interactions (CACTI) and NSF Remote sensing of Electrification, Lightning, And Mesoscale/microscale Processes with Adaptive Ground Observations (RELAMPAGO) field campaigns in central Argentina, where orographic deep convective initiation is frequent with some high-impact systems growing into the tallest and largest in the world. An array of fixed and mobile scanning multi-wavelength dual-polarization radars will be coupled with surface observations, sounding systems, multi-wavelength vertical profilers, and aircraft in situ measurements to characterize convective cloud life cycles and their relationship with environmental conditions. While detailed cloud processes are an observational target, the radar scan patterns that are most ideal for observing them are unclear. They depend on the locations and scales of key microphysical and dynamical processes operating within the cloud. High-resolution simulations of clouds, while imperfect, can provide information on these locations and scales that guide radar measurement needs. Radar locations are set in the model domain based on planned experiment locations, and simulatedorographic deep convective initiation and upscale growth are sampled using a number of different scans involving RHIs or PPIs with predefined elevation and azimuthal angles that approximately conform with radar range and beam width specifications. Each full scan pattern is applied to output atsingle model time steps with time step intervals that depend on the length of time

In situ scanning tunnelling microscopy of redox molecules. Coherent electron transfer at large bias voltages

DEFF Research Database (Denmark)

Zhang, Jingdong; Kuznetsov, A.M.; Ulstrup, Jens

2003-01-01

Theories of in situ scanning tunnelling microscopy (STM) of molecules with redox levels near the substrate and tip Fermi levels point to 'spectroscopic' current-overpotential features. Prominent features require a narrow 'probing tip', i.e. a small bias voltage, eV(bias), compared...... a broad tunnelling current-overpotential range at a constant (large) bias voltage of +0.2 V. The current is found to be constant over a 0.25 V overpotential range, which covers roughly the range where the oxidised and reduced redox levels are located within the energy tip. STM contrast and apparent...... of previous theoretical work on in situ STM of redox molecules, to large bias voltages, \\eV(bias)\\ > E-r. Large bias voltages give tunnelling contrasts independent of the overpotential over a broad range, as both the oxidised and reduced redox levels are located within the 'energy tip' between the substrate...

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

Science.gov (United States)

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 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 recommended for long term, surface water monitoring.

A Silicon Carbide Wireless Temperature Sensing System for High Temperature Applications

Science.gov (United States)

Yang, Jie

2013-01-01

In this article, an extreme environment-capable temperature sensing system based on state-of-art silicon carbide (SiC) wireless electronics is presented. In conjunction with a Pt-Pb thermocouple, the SiC wireless sensor suite is operable at 450 °C while under centrifugal load greater than 1,000 g. This SiC wireless temperature sensing system is designed to be non-intrusively embedded inside the gas turbine generators, acquiring the temperature information of critical components such as turbine blades, and wirelessly transmitting the information to the receiver located outside the turbine engine. A prototype system was developed and verified up to 450 °C through high temperature lab testing. The combination of the extreme temperature SiC wireless telemetry technology and integrated harsh environment sensors will allow for condition-based in-situ maintenance of power generators and aircraft turbines in field operation, and can be applied in many other industries requiring extreme environment monitoring and maintenance. PMID:23377189

High pressure and high temperature EXAFS and diffraction study of AgI

International Nuclear Information System (INIS)

Yoshiasa, Akira; Arima, Hiroshi; Fukui, Hiroshi; Okube, Maki; Katayama, Yoshinori; Ohtaka, Osamu

2009-01-01

We have determined the precise P-T phase diagram of AgI by in-situ high-pressure high-temperature synchrotron experiments. X-ray diffraction and XAFS measurements were performed up to 6.0 GPa and 1100 K using a multi-anvil high-pressure device and synchrotron radiation from SPring-8. In the disordered rock-salt phase, Ag ions occupy both octahedral and tetrahedral sites and twenty percent of Ag ions occupy the tetrahedral site as a maximum value at 2 GPa. From the viewpoint of the local structure analyses, some sudden changes are recognized near broad phase transition point. Analysis of EXAFS Debye-Waller factor is useful because the force constant can be decided directly even at high pressure and high temperature. Pressure influences greatly the effective potential and anharmonicity decreases with increasing pressure. (author)

Small-size low-temperature scanning tunnel microscope

International Nuclear Information System (INIS)

Al'tfeder, I.B.; Khajkin, M.S.

1989-01-01

A small-size scanning tunnel microscope, designed for operation in transport helium-filled Dewar flasks is described. The microscope design contains a device moving the pin to the tested sample surface and a piezoelectric fine positioning device. High vibration protection of the microscope is provided by its suspension using silk threads. The small-size scanning tunnel microscope provides for atomic resolution

Design and performance of an in situ high vacuum STM in beam line at 15 UD pelletron accelerator

International Nuclear Information System (INIS)

Singh, J.P.; Tripathi, A.; Ahuja, R.; Dutt, R.N.; Kanjilal, D.; Mehta, G.K.; Raychoudhuri, A.K.

2000-01-01

The design, installation and performance of an in situ high vacuum STM in the materials science beam line of 15 UD tandem Pelletron accelerator, NSC are reported. The scanning tunneling microscope (STM) has imaged highly oriented pyrolytic graphite (HOPG) surfaces with atomic resolution. Local current-voltage spectroscopy has also been performed on p-type Si (111) samples. A band gap of 1.09 ± 0.1 eV was calculated. (author)

Visualising reacting single atoms under controlled conditions: Advances in atomic resolution in situ Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM)

Science.gov (United States)

Boyes, Edward D.; Gai, Pratibha L.

2014-02-01

Advances in atomic resolution Environmental (Scanning) Transmission Electron Microscopy (E(S)TEM) for probing gas-solid catalyst reactions in situ at the atomic level under controlled reaction conditions of gas environment and temperature are described. The recent development of the ESTEM extends the capability of the ETEM by providing the direct visualisation of single atoms and the atomic structure of selected solid state heterogeneous catalysts in their working states in real-time. Atomic resolution E(S)TEM provides a deeper understanding of the dynamic atomic processes at the surface of solids and their mechanisms of operation. The benefits of atomic resolution-E(S)TEM to science and technology include new knowledge leading to improved technological processes with substantial economic benefits, improved healthcare, reductions in energy needs and the management of environmental waste generation. xml:lang="fr"

Preparation of poly(vinyl alcohol)-grafted graphene oxide/poly(vinyl alcohol) nanocomposites via in-situ low-temperature emulsion polymerization and their thermal and mechanical characterization

Science.gov (United States)

Zhang, Shengchang; Liu, Pengqing; Zhao, Xiangsen; Xu, Jianjun

2017-02-01

An in-situ polymerization combined with chemical grafting modification method for preparing Poly(vinyl alcohol)-grafted graphene oxide/Poly(vinyl alcohol) (PVA-g-GO/PVA) nanocomposites was reported. Firstly, Poly(vinyl acetate)-grafted graphene oxide/Poly(vinyl acetate) nanocomposites were prepared, and then the PVA-g-GO/PVA nanocomposites could be obtained through alcoholysis reaction. X-ray photoelectron spectrometer and fourier-transform infrared spectrometer confirmed that the PVAc or PVA chains were successfully grafted to GO sheets during in-situ polymerization and alcoholysis. And the results from transmission electron microscopy, scanning electron microscopy and X-ray diffraction showed that the well compatibility and homogenous dispersion of PVA-g-GO in PVA matrix could be achieved. Differential scanning calorimetric, thermogravimetry analysis and tensile test were employed to study the thermal and mechanical properties of the PVA-g-GO/PVA nanocomposites. The results indicated that a 53% improvement of tensile strength and a 36% improvement of Young's modulus were achieved by addition of 0.5 wt% of GO sheets. And the glass transition temperature of PVA-g-GO/PVA nanocomposites was increased, and their thermal stability and crystallization degree were both decreased. Due to well dispersion of fillers and strong interfacial interactions at the filler-matrix interface, in-situ polymerization combined with chemical grafting modification was a good choice to prepare graphene/PVA nanocomposite with excellent mechanical properties.

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

International Nuclear Information System (INIS)

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

2015-01-01

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

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

Science.gov (United States)

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. © 2012 Society for Applied Microbiology and Blackwell Publishing Ltd.

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

International Nuclear Information System (INIS)

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

2014-01-01

Fresnoite Ba 2 TiSi 2 O 8 (BTS) thin films were grown and crystallized in situ using pulsed laser deposition (PLD) with CO 2 laser direct heating of the a-plane sapphire (1 1 0) substrates up to 1250 °C. Starting with 775 °C growth temperature, (0 0 1)- and (1 1 0)-textured BTS and BaTiO 3 phases, respectively, could be assigned in the films, and the typical fern-like BTS crystallization patterns appear. For higher process temperatures of 1100 to 1250 °C, atomically smooth, terraced surface of the films was found, accompanied by crystalline high-temperature phases of Ba–Ti–Si oxides. HAADF micrographs taken in both scanning transmission electron microscopy and energy-dispersive x-ray spectrometry mode show details of morphology and elemental distribution inside the films and at the interface. To balance the inherent Si deficiency of the BTS films, growth from glassy BTS × 2 SiO 2 and BTS × 2.5 SiO 2 targets was considered as well. The latter targets are ideal for PLD since the employed glasses possess 100% of the theoretical density and are homogeneous at the atomic scale. (paper)

Comparative study of lesions created by high-intensity focused ultrasound using sequential discrete and continuous scanning strategies.

Science.gov (United States)

Fan, Tingbo; Liu, Zhenbo; Zhang, Dong; Tang, Mengxing

2013-03-01

Lesion formation and temperature distribution induced by high-intensity focused ultrasound (HIFU) were investigated both numerically and experimentally via two energy-delivering strategies, i.e., sequential discrete and continuous scanning modes. Simulations were presented based on the combination of Khokhlov-Zabolotskaya-Kuznetsov (KZK) equation and bioheat equation. Measurements were performed on tissue-mimicking phantoms sonicated by a 1.12-MHz single-element focused transducer working at an acoustic power of 75 W. Both the simulated and experimental results show that, in the sequential discrete mode, obvious saw-tooth-like contours could be observed for the peak temperature distribution and the lesion boundaries, with the increasing interval space between two adjacent exposure points. In the continuous scanning mode, more uniform peak temperature distributions and lesion boundaries would be produced, and the peak temperature values would decrease significantly with the increasing scanning speed. In addition, compared to the sequential discrete mode, the continuous scanning mode could achieve higher treatment efficiency (lesion area generated per second) with a lower peak temperature. The present studies suggest that the peak temperature and tissue lesion resulting from the HIFU exposure could be controlled by adjusting the transducer scanning speed, which is important for improving the HIFU treatment efficiency.

Instrumentation for in situ flow electrochemical Scanning Transmission X-ray Microscopy (STXM)

Science.gov (United States)

Prabu, Vinod; Obst, Martin; Hosseinkhannazer, Hooman; Reynolds, Matthew; Rosendahl, Scott; Wang, Jian; Hitchcock, Adam P.

2018-06-01

We report the design and performance of a 3-electrode device for real time in situ scanning transmission X-ray microscopy studies of electrochemical processes under both static (sealed, non-flow) conditions and with a continuous flow of electrolytes. The device was made using a combination of silicon microfabrication and 3D printing technologies. The performance is illustrated by results of a study of copper deposition and stripping at a gold working electrode. X-ray absorption spectromicroscopy at the Cu 2p edge was used to follow the evolution as a function of potential and time of the spatial distributions of Cu(0) and Cu(i) species electro-deposited from an aqueous solution of copper sulphate. The results are interpreted in terms of competing mechanisms for the reduction of Cu(ii).

Determining pH at elevated pressure and temperature using in situ ¹³C NMR.

Science.gov (United States)

Surface, J Andrew; Wang, Fei; Zhu, Yanzhe; Hayes, Sophia E; Giammar, Daniel E; Conradi, Mark S

2015-02-03

We have developed an approach for determining pH at elevated pressures and temperatures by using (13)C NMR measurements of inorganic carbon species together with a geochemical equilibrium model. The approach can determine in situ pH with precision better than 0.1 pH units at pressures, temperatures, and ionic strengths typical of geologic carbon sequestration systems. A custom-built high pressure NMR probe was used to collect (13)C NMR spectra of (13)C-labeled CO2 reactions with NaOH solutions and Mg(OH)2 suspensions at pressures up to 107 bar and temperatures of 80 °C. The quantitative nature of NMR spectroscopy allows the concentration ratio [CO2]/[HCO3(-)] to be experimentally determined. This ratio is then used with equilibrium constants calculated for the specific pressure and temperature conditions and appropriate activity coefficients for the solutes to calculate the in situ pH. The experimentally determined [CO2]/[HCO3(-)] ratios agree well with the predicted values for experiments performed with three different concentrations of NaOH and equilibration with multiple pressures of CO2. The approach was then applied to experiments with Mg(OH)2 slurries in which the change in pH could track the dissolution of CO2 into solution, rapid initial Mg(OH)2 dissolution, and onset of magnesium carbonate precipitation.

Evaluation of the mechanical performance of silicon carbide in TRISO fuel at high temperatures

Energy Technology Data Exchange (ETDEWEB)

Rohbeck, Nadia, E-mail: nadia.rohbeck@manchester.ac.uk; Xiao, Ping, E-mail: p.xiao@manchester.ac.uk

2016-09-15

The HTR design envisions fuel operating temperatures of up to 1000 °C and in case of an accident even 1600 °C are conceivable. To ensure safety in all conditions a thorough understanding of the impact of an extreme temperature environment is necessary. This work assesses the high temperature mechanical performance of the silicon carbide (SiC) layer within the tristructural-isotropic (TRISO) fuel particle as it poses the main barrier against fission product release into the primary circuit. Therefore, simulated fuel was fabricated by fluidized bed chemical vapour deposition; varying the deposition conditions resulted in strongly differing SiC microstructures for the various samples. Subsequently the TRISO particles were annealed in inert atmosphere at temperatures ranging from 1600 °C up to 2200 °C. Scanning electron microscopy and Raman spectroscopy showed that strong disintegration of the SiC layer occurred from 2100 °C onwards, but initial signs of porosity formation were visible already at 1800 °C. Still, the elastic modulus and hardness as measured by nanoindentation were hardly impaired. After annealing stoichiometric SiC coatings showed a reduction in fracture strength as determined by a modified crush test, however the actual annealing temperature from 1600 °C to 2000 °C had no measureable effect. Furthermore, a technique was developed to measure the elastic modulus and hardness in situ up to 500 °C using a high temperature nanoindentation facility. This approach allows conducting tests while the specimen and indenter tip are heated to a specific measurement temperature, thus obtaining reliable values for the temperature dependent mechanical properties of the material. For the SiC layer in TRISO particles it was found that the elastic modulus decreased slightly from room temperature up to 500 °C, whereas the hardness was reduced more severely to approximately half of its ambient temperature value.

Evaluation of the mechanical performance of silicon carbide in TRISO fuel at high temperatures

International Nuclear Information System (INIS)

Rohbeck, Nadia; Xiao, Ping

2016-01-01

The HTR design envisions fuel operating temperatures of up to 1000 °C and in case of an accident even 1600 °C are conceivable. To ensure safety in all conditions a thorough understanding of the impact of an extreme temperature environment is necessary. This work assesses the high temperature mechanical performance of the silicon carbide (SiC) layer within the tristructural-isotropic (TRISO) fuel particle as it poses the main barrier against fission product release into the primary circuit. Therefore, simulated fuel was fabricated by fluidized bed chemical vapour deposition; varying the deposition conditions resulted in strongly differing SiC microstructures for the various samples. Subsequently the TRISO particles were annealed in inert atmosphere at temperatures ranging from 1600 °C up to 2200 °C. Scanning electron microscopy and Raman spectroscopy showed that strong disintegration of the SiC layer occurred from 2100 °C onwards, but initial signs of porosity formation were visible already at 1800 °C. Still, the elastic modulus and hardness as measured by nanoindentation were hardly impaired. After annealing stoichiometric SiC coatings showed a reduction in fracture strength as determined by a modified crush test, however the actual annealing temperature from 1600 °C to 2000 °C had no measureable effect. Furthermore, a technique was developed to measure the elastic modulus and hardness in situ up to 500 °C using a high temperature nanoindentation facility. This approach allows conducting tests while the specimen and indenter tip are heated to a specific measurement temperature, thus obtaining reliable values for the temperature dependent mechanical properties of the material. For the SiC layer in TRISO particles it was found that the elastic modulus decreased slightly from room temperature up to 500 °C, whereas the hardness was reduced more severely to approximately half of its ambient temperature value.

Scanning magnetic tunnel junction microscope for high-resolution imaging of remanent magnetization fields

Science.gov (United States)

Lima, E. A.; Bruno, A. C.; Carvalho, H. R.; Weiss, B. P.

2014-10-01

Scanning magnetic microscopy is a new methodology for mapping magnetic fields with high spatial resolution and field sensitivity. An important goal has been to develop high-performance instruments that do not require cryogenic technology due to its high cost, complexity, and limitation on sensor-to-sample distance. Here we report the development of a low-cost scanning magnetic microscope based on commercial room-temperature magnetic tunnel junction (MTJ) sensors that typically achieves spatial resolution better than 7 µm. By comparing different bias and detection schemes, optimal performance was obtained when biasing the MTJ sensor with a modulated current at 1.0 kHz in a Wheatstone bridge configuration while using a lock-in amplifier in conjunction with a low-noise custom-made preamplifier. A precision horizontal (x-y) scanning stage comprising two coupled nanopositioners controls the position of the sample and a linear actuator adjusts the sensor-to-sample distance. We obtained magnetic field sensitivities better than 150 nT/Hz1/2 between 0.1 and 10 Hz, which is a critical frequency range for scanning magnetic microscopy. This corresponds to a magnetic moment sensitivity of 10-14 A m2, a factor of 100 better than achievable with typical commercial superconducting moment magnetometers. It also represents an improvement in sensitivity by a factor between 10 and 30 compared to similar scanning MTJ microscopes based on conventional bias-detection schemes. To demonstrate the capabilities of the instrument, two polished thin sections of representative geological samples were scanned along with a synthetic sample containing magnetic microparticles. The instrument is usable for a diversity of applications that require mapping of samples at room temperature to preserve magnetic properties or viability, including paleomagnetism and rock magnetism, nondestructive evaluation of materials, and biological assays.

Scanning magnetic tunnel junction microscope for high-resolution imaging of remanent magnetization fields

International Nuclear Information System (INIS)

Lima, E A; Weiss, B P; Bruno, A C; Carvalho, H R

2014-01-01

Scanning magnetic microscopy is a new methodology for mapping magnetic fields with high spatial resolution and field sensitivity. An important goal has been to develop high-performance instruments that do not require cryogenic technology due to its high cost, complexity, and limitation on sensor-to-sample distance. Here we report the development of a low-cost scanning magnetic microscope based on commercial room-temperature magnetic tunnel junction (MTJ) sensors that typically achieves spatial resolution better than 7 µm. By comparing different bias and detection schemes, optimal performance was obtained when biasing the MTJ sensor with a modulated current at 1.0 kHz in a Wheatstone bridge configuration while using a lock-in amplifier in conjunction with a low-noise custom-made preamplifier. A precision horizontal (x–y) scanning stage comprising two coupled nanopositioners controls the position of the sample and a linear actuator adjusts the sensor-to-sample distance. We obtained magnetic field sensitivities better than 150 nT/Hz 1/2 between 0.1 and 10 Hz, which is a critical frequency range for scanning magnetic microscopy. This corresponds to a magnetic moment sensitivity of 10 –14  A m 2 , a factor of 100 better than achievable with typical commercial superconducting moment magnetometers. It also represents an improvement in sensitivity by a factor between 10 and 30 compared to similar scanning MTJ microscopes based on conventional bias-detection schemes. To demonstrate the capabilities of the instrument, two polished thin sections of representative geological samples were scanned along with a synthetic sample containing magnetic microparticles. The instrument is usable for a diversity of applications that require mapping of samples at room temperature to preserve magnetic properties or viability, including paleomagnetism and rock magnetism, nondestructive evaluation of materials, and biological assays. (paper)

Growth of room temperature ferromagnetic Ge1-xMnx quantum dots on hydrogen passivated Si (100) surfaces

Science.gov (United States)

Gastaldo, Daniele; Conta, Gianluca; Coïsson, Marco; Amato, Giampiero; Tiberto, Paola; Allia, Paolo

2018-05-01

A method for the synthesis of room-temperature ferromagnetic dilute semiconductor Ge1-xMnx (5 % < x < 8 %) quantum dots by molecular beam epitaxy by selective growth on hydrogen terminated silicon (100) surface is presented. The functionalized substrates, as well as the nanostructures, were characterized in situ by reflection high-energy electron diffraction. The quantum dots density and equivalent radius were extracted from field emission scanning electron microscope pictures, obtained ex-situ. Magnetic characterizations were performed by superconducting quantum interference device vibrating sample magnetometry revealing that ferromagnetic order is maintained up to room temperature: two different ferromagnetic phases were identified by the analysis of the field cooled - zero field cooled measurements.

High accuracy wavelength calibration for a scanning visible spectrometer

Energy Technology Data Exchange (ETDEWEB)

Scotti, Filippo; Bell, Ronald E. [Princeton Plasma Physics Laboratory, Princeton, New Jersey 08543 (United States)

2010-10-15

Spectroscopic applications for plasma velocity measurements often require wavelength accuracies {<=}0.2 A. An automated calibration, which is stable over time and environmental conditions without the need to recalibrate after each grating movement, was developed for a scanning spectrometer to achieve high wavelength accuracy over the visible spectrum. This method fits all relevant spectrometer parameters using multiple calibration spectra. With a stepping-motor controlled sine drive, an accuracy of {approx}0.25 A has been demonstrated. With the addition of a high resolution (0.075 arc sec) optical encoder on the grating stage, greater precision ({approx}0.005 A) is possible, allowing absolute velocity measurements within {approx}0.3 km/s. This level of precision requires monitoring of atmospheric temperature and pressure and of grating bulk temperature to correct for changes in the refractive index of air and the groove density, respectively.

A cryogenic scanning laser microscope for investigation of dynamical states in long Josephson junctions

DEFF Research Database (Denmark)

Holm, Jesper; Mygind, Jesper

1995-01-01

on measurements on different oscillator samples, performed with a novel Cryogenic Scanning Laser Microscope (CSLM) having a spatial resolution of less than ±2.5 μm over a 500 μm×50 μm wide scanning area in the temperature range 2 K-300 K. Even though the dynamical states are extremely sensitive to external noise...... tunnel current is one of the most important internal junction parameters which together with the boundary conditions determine the dynamics, it is of vital importance to experimentally determine the current density throughout the entire junction with high spatial resolution. Here we report...... this microscope enables us to make stable in-situ measurements on operating Josephson junctions. Recent results are presented and discussed....

Phosphoric acid distribution in the membrane electrode assembly of high temperature proton exchange membrane fuel cells

International Nuclear Information System (INIS)

Kwon, Kyungjung; Park, Jung Ock; Yoo, Duck Young; Yi, Jung S.

2009-01-01

The ionomer content in electrode is one of the most important parameters for the high performance of fuel cells. The high temperature PEMFC based on phosphoric acid (PA)-doped polymer membrane with unhumidified reactant gases has a difficulty in controlling the liquid state PA ionomer content in electrode. To evaluate the PA content in electrode, the three techniques of cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and acid-base titration (ABT) are carried out in situ or ex situ. The properties of membrane electrode assembly (MEA) such as electrochemical surface area (ESA), ohmic resistance, charge transfer resistance, double layer capacitance and the amount of PA in MEA components (anode, cathode and membrane) are extracted by each technique. Ex situ CV with the usage of dry gases has a limitation in assessing the reliable ESA of unhumidified PEMFC. While in situ EIS presents some informative values of resistance and capacitance for understanding the PA distribution in MEA, its sensitivity to the PA content in MEA components needs to be higher for detecting a subtle change in PA distribution. Ex situ ABT supplies a clear PA distribution in MEA at room temperature but does not seem to reflect the operating state well at high temperatures. However, it can be used as a detection tool for the loss of the initial acid content in membrane during a long-term MEA durability study.

Phosphoric acid distribution in the membrane electrode assembly of high temperature proton exchange membrane fuel cells

Energy Technology Data Exchange (ETDEWEB)

Kwon, Kyungjung [Fuel Cell Group, Energy Lab, SAIT, Samsung Electronics Co., Ltd., San 14-1, Nongseo-dong, Giheung-gu, Yongin-si, Gyeonggi-do, 446-712 (Korea, Republic of)], E-mail: kfromberk@gmail.com; Park, Jung Ock; Yoo, Duck Young; Yi, Jung S. [Fuel Cell Group, Energy Lab, SAIT, Samsung Electronics Co., Ltd., San 14-1, Nongseo-dong, Giheung-gu, Yongin-si, Gyeonggi-do, 446-712 (Korea, Republic of)

2009-11-01

The ionomer content in electrode is one of the most important parameters for the high performance of fuel cells. The high temperature PEMFC based on phosphoric acid (PA)-doped polymer membrane with unhumidified reactant gases has a difficulty in controlling the liquid state PA ionomer content in electrode. To evaluate the PA content in electrode, the three techniques of cyclic voltammetry (CV), electrochemical impedance spectroscopy (EIS) and acid-base titration (ABT) are carried out in situ or ex situ. The properties of membrane electrode assembly (MEA) such as electrochemical surface area (ESA), ohmic resistance, charge transfer resistance, double layer capacitance and the amount of PA in MEA components (anode, cathode and membrane) are extracted by each technique. Ex situ CV with the usage of dry gases has a limitation in assessing the reliable ESA of unhumidified PEMFC. While in situ EIS presents some informative values of resistance and capacitance for understanding the PA distribution in MEA, its sensitivity to the PA content in MEA components needs to be higher for detecting a subtle change in PA distribution. Ex situ ABT supplies a clear PA distribution in MEA at room temperature but does not seem to reflect the operating state well at high temperatures. However, it can be used as a detection tool for the loss of the initial acid content in membrane during a long-term MEA durability study.

Integration of a high-NA light microscope in a scanning electron microscope.

Science.gov (United States)

Zonnevylle, A C; Van Tol, R F C; Liv, N; Narvaez, A C; Effting, A P J; Kruit, P; Hoogenboom, J P

2013-10-01

We present an integrated light-electron microscope in which an inverted high-NA objective lens is positioned inside a scanning electron microscope (SEM). The SEM objective lens and the light objective lens have a common axis and focal plane, allowing high-resolution optical microscopy and scanning electron microscopy on the same area of a sample simultaneously. Components for light illumination and detection can be mounted outside the vacuum, enabling flexibility in the construction of the light microscope. The light objective lens can be positioned underneath the SEM objective lens during operation for sub-10 μm alignment of the fields of view of the light and electron microscopes. We demonstrate in situ epifluorescence microscopy in the SEM with a numerical aperture of 1.4 using vacuum-compatible immersion oil. For a 40-nm-diameter fluorescent polymer nanoparticle, an intensity profile with a FWHM of 380 nm is measured whereas the SEM performance is uncompromised. The integrated instrument may offer new possibilities for correlative light and electron microscopy in the life sciences as well as in physics and chemistry. © 2013 The Authors Journal of Microscopy © 2013 Royal Microscopical Society.

Improving image quality by accounting for changes in water temperature during a photoacoustic tomography scan.

Directory of Open Access Journals (Sweden)

Dominique Van de Sompel

Full Text Available The emerging field of photoacoustic tomography is rapidly evolving with many new system designs and reconstruction algorithms being published. Many systems use water as a coupling medium between the scanned object and the ultrasound transducers. Prior to a scan, the water is heated to body temperature to enable small animal imaging. During the scan, the water heating system of some systems is switched off to minimize the risk of bubble formation, which leads to a gradual decrease in water temperature and hence the speed of sound. In this work, we use a commercially available scanner that follows this procedure, and show that a failure to model intra-scan temperature decreases as small as 1.5°C leads to image artifacts that may be difficult to distinguish from true structures, particularly in complex scenes. We then improve image quality by continuously monitoring the water temperature during the scan and applying variable speed of sound corrections in the image reconstruction algorithm. While upgrading to an air bubble-free heating pump and keeping it running during the scan could also solve the changing temperature problem, we show that a software correction for the temperature changes provides a cost-effective alternative to a hardware upgrade. The efficacy of the software corrections was shown to be consistent across objects of widely varying appearances, namely physical phantoms, ex vivo tissue, and in vivo mouse imaging. To the best of our knowledge, this is the first study to demonstrate the efficacy of modeling temporal variations in the speed of sound during photoacoustic scans, as opposed to spatial variations as focused on by previous studies. Since air bubbles pose a common problem in ultrasonic and photoacoustic imaging systems, our results will be useful to future small animal imaging studies that use scanners with similarly limited heating units.

Microwave Wire Interrogation Method Mapping Pressure under High Temperatures

Directory of Open Access Journals (Sweden)

Xiaoyong Chen

2017-12-01

Full Text Available It is widely accepted that wireless reading for in-situ mapping of pressure under high-temperature environments is the most feasible method, because it is not subject to frequent heterogeneous jointing failures and electrical conduction deteriorating, or even disappearing, under heat load. However, in this article, we successfully demonstrate an in-situ pressure sensor with wire interrogation for high-temperature applications. In this proof-of-concept study of the pressure sensor, we used a microwave resonator as a pressure-sensing component and a microwave transmission line as a pressure characteristic interrogation tunnel. In the sensor, the line and resonator are processed into a monolith, avoiding a heterogeneous jointing failure; further, microwave signal transmission does not depend on electrical conduction, and consequently, the sensor does not suffer from the heat load. We achieve pressure monitoring under 400 °C when employing the sensor simultaneously. Our sensor avoids restrictions that exist in wireless pressure interrogations, such as environmental noise and interference, signal leakage and security, low transfer efficiency, and so on.

High-pressure, high-temperature magic angle spinning nuclear magnetic resonance devices and processes for making and using same

Science.gov (United States)

Hu, Jian Zhi; Hu, Mary Y.; Townsend, Mark R.; Lercher, Johannes A.; Peden, Charles H. F.

2015-10-06

Re-usable ceramic magic angle spinning (MAS) NMR rotors constructed of high-mechanic strength ceramics are detailed that include a sample compartment that maintains high pressures up to at least about 200 atmospheres (atm) and high temperatures up to about least about 300.degree. C. during operation. The rotor designs minimize pressure losses stemming from penetration over an extended period of time. The present invention makes possible a variety of in-situ high pressure, high temperature MAS NMR experiments not previously achieved in the prior art.

High-temperature absorbed dose measurements in the megagray range

International Nuclear Information System (INIS)

Balian, P.; Ardonceau, J.; Zuppiroli, L.

1988-01-01

Organic conductors of the tetraselenotetracene family have been tested as ''high-temperature'' absorbed dose dosimeters. They were heated up to 120 0 C and irradiated at this temperature with 1-MeV electrons in order to simulate, in a short time, a much longer γ-ray irradiation. The electric resistance increase of the crystal can be considered a good measurement of the absorbed dose in the range 10 6 Gy to a few 10 8 Gy and presumably one order of magnitude more. This dosimeter also permits on-line (in-situ) measurements of the absorbed dose without removing the sensor from the irradiation site. The respective advantages of organic and inorganic dosimeters at these temperature and dose ranges are also discussed. In this connection, we outline new, but negative, results concerning the possible use of silica as a high-temperature, high-dose dosimeter. (author)

Ex-situ X-ray tomography characterization of porosity during high-temperature creep in a Ni-based single-crystal superalloy: Toward understanding what is damage

Energy Technology Data Exchange (ETDEWEB)

Graverend, Jean-Briac le, E-mail: jblgpublications@gmail.com [Texas A& M University, Department of Aerospace Engineering and Materials Science Engineering, TAMU 3141, College Station, TX 77843 (United States); Adrien, Jérome [Université de Lyon, INSA-Lyon, MATEIS CNRS UMR5510, F-69621 Villeurbanne (France); Cormier, Jonathan [Institut Pprime, CNRS-ENSMA-Université de Poitiers, UPR CNRS 3346, Département Physique et Mécanique des Matériaux, ISAE-ENSMA, 1 avenue Clément Ader, BP 40109, F86961 Futuroscope Chasseneuil cedex (France)

2017-05-17

Creep damage by void nucleation and growth limits the lifetime of components subjected to mechanical loads at high temperatures. For the first time, the porosity of a Ni-based single crystal superalloy subjected to high temperature creep tests (T≥1000 °C) is followed by ex-situ X-ray computed tomography. A large experimental campaign consisting of nine temperature/stress conditions is carried out to determine the kinetics of the damage accumulation by voids. It is, indeed, essential to characterize their evolution to create internal variables describing properly the evolution of damage in a Continuum Damage Mechanics framework. Nonetheless, it is pointed out that the increase in the plastic strain rate during the tertiary creep stage is not necessarily related to the increase in the pore volume fraction for the alloy and temperature range explored (1000–1100 °C). Therefore, it seems that the changes in the microstructure, i.e. precipitation coarsening and γ/γ′ topological inversion, and the shearing of the γ′ particles have to be considered further to properly describe the damage evolution. Thus, the Continuum Damage Mechanics theory is undermined and should be replaced by a transformative paradigm taken into consideration microstructural evolutions in order to improve the predictability of further damage models.

High pressure-temperature polymorphism of 1,1-diamino-2,2-dinitroethylene

Science.gov (United States)

Bishop, M. M.; Chellappa, R. S.; Liu, Z.; Preston, D. N.; Sandstrom, M. M.; Dattelbaum, D. M.; Vohra, Y. K.; Velisavljevic, N.

2014-05-01

1,1-diamino-2,2-dinitroethylene (FOX-7) is a low sensitivity energetic material with performance comparable to commonly used secondary explosives such as RDX and HMX. At ambient pressure, FOX-7 exhibits complex polymorphism with at least three structurally distinct phases (α, β, and γ). In this study, we have investigated the high pressure-temperature stability of FOX-7 polymorphs using synchrotron mid-infrared (MIR) spectroscopy. At ambient pressure, our MIR spectra and corresponding differential scanning calorimetry (DSC) measurements confirmed the known α → β (~110 °C) and α → β (~160 °C) structural phase transitions; as well as, indicated an additional transition γ → (~210 °C), with the δ phase being stable up to ~251 °C prior to decomposition. In situ MIR spectra obtained during isobaric heating at 0.9 GPa, revealed a potential α → β transition that could occur as early as 180 °C, while β → β+δ phase transition shifted to ~300 °C with suppression of γ phase. Decomposition was observed slightly above 325 °C at 0.9 GPa.

In situ temperature relationships of biochemical and stomatal controls of photosynthesis in four lowland tropical tree species.

Science.gov (United States)

Slot, Martijn; Winter, Klaus

2017-12-01

Net photosynthetic carbon uptake of Panamanian lowland tropical forest species is typically optimal at 30-32 °C. The processes responsible for the decrease in photosynthesis at higher temperatures are not fully understood for tropical trees. We determined temperature responses of maximum rates of RuBP-carboxylation (V CMax ) and RuBP-regeneration (J Max ), stomatal conductance (G s ), and respiration in the light (R Light ) in situ for 4 lowland tropical tree species in Panama. G s had the lowest temperature optimum (T Opt ), similar to that of net photosynthesis, and photosynthesis became increasingly limited by stomatal conductance as temperature increased. J Max peaked at 34-37 °C and V CMax ~2 °C above that, except in the late-successional species Calophyllum longifolium, in which both peaked at ~33 °C. R Light significantly increased with increasing temperature, but simulations with a photosynthesis model indicated that this had only a small effect on net photosynthesis. We found no evidence for Rubisco-activase limitation of photosynthesis. T Opt of V CMax and J Max fell within the observed in situ leaf temperature range, but our study nonetheless suggests that net photosynthesis of tropical trees is more strongly influenced by the indirect effects of high temperature-for example, through elevated vapour pressure deficit and resulting decreases in stomatal conductance-than by direct temperature effects on photosynthetic biochemistry and respiration. © 2017 John Wiley & Sons Ltd.

Coalescence aspects of cobalt nanoparticles during in situ high-temperature annealing

NARCIS (Netherlands)

Palasantzas, G; Vystavel, T; Koch, SA; De Hosson, JTM

2006-01-01

In this work we investigate the coalescence aspects of Co nanoparticles. It was observed that nanoparticles in contact with the substrate are relatively immobile, whereas those on top of other Co particles can rearrange themselves during high-temperature annealing and further coalesce. Indeed,

Comparison of Fluorescence In Situ Hybridization and Chromogenic In Situ Hybridization for Low and High Throughput HER2 Genetic Testing

Science.gov (United States)

Poulsen, Tim S.; Espersen, Maiken L. M.; Kofoed, Vibeke; Dabetic, Tanja; Høgdall, Estrid; Balslev, Eva

2013-01-01

The purpose was to evaluate and compare 5 different HER2 genetic assays with different characteristics that could affect the performance to analyze the human epidermal growth factor 2 (HER2) gene copy number under low and high throughput conditions. The study included 108 tissue samples from breast cancer patients with HER2 immunohistochemistry (IHC) results scored as 0/1+, 2+, and 3+. HER2 genetic status was analysed using chromogenic in situ hybridization (CISH) and fluorescence in situ hybridization (FISH). Scoring results were documented through digital image analysis. The cancer region of interest was identified from a serial H&E stained slide following tissue cores were transferred to a tissue microarrays (TMA). When using TMA in a routine flow, all patients will be tested for HER2 status with IHC followed by CISH or FISH, thereby providing individual HER2 results. In conclusion, our results show that the differences between the HER2 genetic assays do not have an effect on the analytic performance and the CISH technology is superior to high throughput HER2 genetic testing due to scanning speed, while the IQ-FISH may still be a choice for fast low throughput HER2 genetic testing. PMID:24383005

Preparation of poly(vinyl alcohol)-grafted graphene oxide/poly(vinyl alcohol) nanocomposites via in-situ low-temperature emulsion polymerization and their thermal and mechanical characterization

Energy Technology Data Exchange (ETDEWEB)

Zhang, Shengchang; Liu, Pengqing, E-mail: liupq@scu.edu.cn; Zhao, Xiangsen; Xu, Jianjun, E-mail: xujj@scu.edu.cn

2017-02-28

Highlights: • In-situ emulsion polymerization and alcoholysis reaction is a good method to prepare GO/PVA nanocomposites. • Surface chemical grafting modification of GO with PVA chains was also carried out during the in-situ emulsion polymerization and alcoholysis reaction. • The surface chemical grafting modification of GO by in-situ polymerization and alcoholysis reaction could not only improve the dispersion of fillers in matrix, but also the interfacial interactions between fillers and matrix. • The thermal and mechanical properties of PVA-g-GO/PVA nanocompistes were also studied. - Abstract: An in-situ polymerization combined with chemical grafting modification method for preparing Poly(vinyl alcohol)-grafted graphene oxide/Poly(vinyl alcohol) (PVA-g-GO/PVA) nanocomposites was reported. Firstly, Poly(vinyl acetate)-grafted graphene oxide/Poly(vinyl acetate) nanocomposites were prepared, and then the PVA-g-GO/PVA nanocomposites could be obtained through alcoholysis reaction. X-ray photoelectron spectrometer and fourier-transform infrared spectrometer confirmed that the PVAc or PVA chains were successfully grafted to GO sheets during in-situ polymerization and alcoholysis. And the results from transmission electron microscopy, scanning electron microscopy and X-ray diffraction showed that the well compatibility and homogenous dispersion of PVA-g-GO in PVA matrix could be achieved. Differential scanning calorimetric, thermogravimetry analysis and tensile test were employed to study the thermal and mechanical properties of the PVA-g-GO/PVA nanocomposites. The results indicated that a 53% improvement of tensile strength and a 36% improvement of Young’s modulus were achieved by addition of 0.5 wt% of GO sheets. And the glass transition temperature of PVA-g-GO/PVA nanocomposites was increased, and their thermal stability and crystallization degree were both decreased. Due to well dispersion of fillers and strong interfacial interactions at the filler

Preparation of poly(vinyl alcohol)-grafted graphene oxide/poly(vinyl alcohol) nanocomposites via in-situ low-temperature emulsion polymerization and their thermal and mechanical characterization

International Nuclear Information System (INIS)

Zhang, Shengchang; Liu, Pengqing; Zhao, Xiangsen; Xu, Jianjun

2017-01-01

Highlights: • In-situ emulsion polymerization and alcoholysis reaction is a good method to prepare GO/PVA nanocomposites. • Surface chemical grafting modification of GO with PVA chains was also carried out during the in-situ emulsion polymerization and alcoholysis reaction. • The surface chemical grafting modification of GO by in-situ polymerization and alcoholysis reaction could not only improve the dispersion of fillers in matrix, but also the interfacial interactions between fillers and matrix. • The thermal and mechanical properties of PVA-g-GO/PVA nanocompistes were also studied. - Abstract: An in-situ polymerization combined with chemical grafting modification method for preparing Poly(vinyl alcohol)-grafted graphene oxide/Poly(vinyl alcohol) (PVA-g-GO/PVA) nanocomposites was reported. Firstly, Poly(vinyl acetate)-grafted graphene oxide/Poly(vinyl acetate) nanocomposites were prepared, and then the PVA-g-GO/PVA nanocomposites could be obtained through alcoholysis reaction. X-ray photoelectron spectrometer and fourier-transform infrared spectrometer confirmed that the PVAc or PVA chains were successfully grafted to GO sheets during in-situ polymerization and alcoholysis. And the results from transmission electron microscopy, scanning electron microscopy and X-ray diffraction showed that the well compatibility and homogenous dispersion of PVA-g-GO in PVA matrix could be achieved. Differential scanning calorimetric, thermogravimetry analysis and tensile test were employed to study the thermal and mechanical properties of the PVA-g-GO/PVA nanocomposites. The results indicated that a 53% improvement of tensile strength and a 36% improvement of Young’s modulus were achieved by addition of 0.5 wt% of GO sheets. And the glass transition temperature of PVA-g-GO/PVA nanocomposites was increased, and their thermal stability and crystallization degree were both decreased. Due to well dispersion of fillers and strong interfacial interactions at the filler

Evaluation of the Mechanical Performance of Silicon Carbide in TRISO Fuel at High Temperatures

International Nuclear Information System (INIS)

Rohbeck, N.; Xiao, P.

2014-01-01

The HTR design envisions fuel operating temperatures of up to 1000°C and in case of an accident even 1600°C are conceivable. To ensure safety in all conditions a thorough understanding of the impact of an extreme temperature environment is necessary. This work assesses the high temperature mechanical performance of the silicon carbide (SiC) layer within the tristructural-isotropic (TRISO) fuel particle as it poses the main barrier against fission product release into the primary circuit. Therefore simulated fuel was fabricated by fluidized bed chemical vapour deposition; varying the deposition conditions resulted in strongly differing SiC microstructures for the various samples. Subsequently the TRISO particles were annealed in inert atmosphere at temperatures ranging from 1600°C up to 2200°C. Scanning electron microscopy and Raman spectroscopy showed that strong disintegration of the SiC layer occurred from 2100°C onwards, but initial signs of porosity formation were visible already at 1800°C. Still, the elastic modulus and hardness as measured by nanoindentation were hardly impaired. After annealing stoichiometric SiC coatings showed a reduction in fracture strength as determined by a modified crush test, however the actual annealing temperature from 1600°C to 2000°C had no measureable effect. Furthermore, a technique was developed to measure the elastic modulus and hardness in-situ up to 500°C using a high temperature nanoindentation facility. This approach allows conducting numerous tests on small sample volumes and thus promises to improve our knowledge of irradiation effects on the mechanical properties. For the SiC layer in TRISO particles it was found that the elastic modulus decreased slightly from room temperature up to 500°C, whereas the hardness was reduced more severely to approximately half of its ambient temperature value. (author)

Temperature profiles by ground-based remote sensing and in situ measurements

Energy Technology Data Exchange (ETDEWEB)

Argentini, S; Pietroni, I; Conidi, A; Mastrantonio, G; Petenko, I; Viola, A [ISAC-CNR, Via del Fosso del Cavaliere, 100, 00133 Roma (Italy); Gariazzo, C; Pelliccioni, A; Amicarelli, A [ISPESL Dipartimento Insediamenti Produttivi e Interazione con l' Ambiente, Via Fontana Candida, 1, 00040 Monteporzio Catone (RM) (Italy)], E-mail: s.argentini@isac.cnr.it

2008-05-01

This study focuses on the accuracy of the temperature profiles measured with a Doppler Radio-Acoustic Sounding System and a Microwave Temperature Profiler during a period of about 3 months in winter 2007-2008. The experiment was carried on at the experimental facility of the Institute of Atmospheric Sciences and Climate (ISAC) of the Italian National Research Council (CNR). The temperature data measured with remote sensors were verified with in situ measurements on a mast as well as with tethered balloon data. The facsimile echograms obtained with the ISAC Doppler SODAR were analysed to understand to which extent the RASS and Radiometer temperature profiles behaviour can represent the real thermal structure of the atmosphere.

Temperature profiles by ground-based remote sensing and in situ measurements

International Nuclear Information System (INIS)

Argentini, S; Pietroni, I; Conidi, A; Mastrantonio, G; Petenko, I; Viola, A; Gariazzo, C; Pelliccioni, A; Amicarelli, A

2008-01-01

This study focuses on the accuracy of the temperature profiles measured with a Doppler Radio-Acoustic Sounding System and a Microwave Temperature Profiler during a period of about 3 months in winter 2007-2008. The experiment was carried on at the experimental facility of the Institute of Atmospheric Sciences and Climate (ISAC) of the Italian National Research Council (CNR). The temperature data measured with remote sensors were verified with in situ measurements on a mast as well as with tethered balloon data. The facsimile echograms obtained with the ISAC Doppler SODAR were analysed to understand to which extent the RASS and Radiometer temperature profiles behaviour can represent the real thermal structure of the atmosphere

Nanocalorimeter platform for in situ specific heat measurements and x-ray diffraction at low temperature

Energy Technology Data Exchange (ETDEWEB)

Willa, K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Diao, Z. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Laboratory of Mathematics, Physics and Electrical Engineering, Halmstad University, P.O. Box 823, SE-301 18 Halmstad, Sweden; Campanini, D. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Welp, U. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Divan, R. [Center for Nanoscale Materials, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Hudl, M. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden; Islam, Z. [X-ray Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Kwok, W. -K. [Materials Science Division, Argonne National Laboratory, 9700 South Cass Avenue, Argonne, Illinois 60439, USA; Rydh, A. [Department of Physics, Stockholm University, SE-106 91 Stockholm, Sweden

2017-12-01

Recent advances in electronics and nanofabrication have enabled membrane-based nanocalorimetry for measurements of the specific heat of microgram-sized samples. We have integrated a nanocalorimeter platform into a 4.5 T split-pair vertical-field magnet to allow for the simultaneous measurement of the specific heat and x-ray scattering in magnetic fields and at temperatures as low as 4 K. This multi-modal approach empowers researchers to directly correlate scattering experiments with insights from thermodynamic properties including structural, electronic, orbital, and magnetic phase transitions. The use of a nanocalorimeter sample platform enables numerous technical advantages: precise measurement and control of the sample temperature, quantification of beam heating effects, fast and precise positioning of the sample in the x-ray beam, and fast acquisition of x-ray scans over a wide temperature range without the need for time-consuming re-centering and re-alignment. Furthermore, on an YBa2Cu3O7-delta crystal and a copper foil, we demonstrate a novel approach to x-ray absorption spectroscopy by monitoring the change in sample temperature as a function of incident photon energy. Finally, we illustrate the new insights that can be gained from in situ structural and thermodynamic measurements by investigating the superheated state occurring at the first-order magneto-elastic phase transition of Fe2P, a material that is of interest for magnetocaloric applications.

High resolution, high speed ultrahigh vacuum microscopy

International Nuclear Information System (INIS)

Poppa, Helmut

2004-01-01

The history and future of transmission electron microscopy (TEM) is discussed as it refers to the eventual development of instruments and techniques applicable to the real time in situ investigation of surface processes with high resolution. To reach this objective, it was necessary to transform conventional high resolution instruments so that an ultrahigh vacuum (UHV) environment at the sample site was created, that access to the sample by various in situ sample modification procedures was provided, and that in situ sample exchanges with other integrated surface analytical systems became possible. Furthermore, high resolution image acquisition systems had to be developed to take advantage of the high speed imaging capabilities of projection imaging microscopes. These changes to conventional electron microscopy and its uses were slowly realized in a few international laboratories over a period of almost 40 years by a relatively small number of researchers crucially interested in advancing the state of the art of electron microscopy and its applications to diverse areas of interest; often concentrating on the nucleation, growth, and properties of thin films on well defined material surfaces. A part of this review is dedicated to the recognition of the major contributions to surface and thin film science by these pioneers. Finally, some of the important current developments in aberration corrected electron optics and eventual adaptations to in situ UHV microscopy are discussed. As a result of all the path breaking developments that have led to today's highly sophisticated UHV-TEM systems, integrated fundamental studies are now possible that combine many traditional surface science approaches. Combined investigations to date have involved in situ and ex situ surface microscopies such as scanning tunneling microscopy/atomic force microscopy, scanning Auger microscopy, and photoemission electron microscopy, and area-integrating techniques such as x-ray photoelectron

Plasma flow reactor for steady state monitoring of physical and chemical processes at high temperatures.

Science.gov (United States)

Koroglu, Batikan; Mehl, Marco; Armstrong, Michael R; Crowhurst, Jonathan C; Weisz, David G; Zaug, Joseph M; Dai, Zurong; Radousky, Harry B; Chernov, Alex; Ramon, Erick; Stavrou, Elissaios; Knight, Kim; Fabris, Andrea L; Cappelli, Mark A; Rose, Timothy P

2017-09-01

We present the development of a steady state plasma flow reactor to investigate gas phase physical and chemical processes that occur at high temperature (1000 flow injector). We have modeled the system using computational fluid dynamics simulations that are bounded by measured temperatures. In situ line-of-sight optical emission and absorption spectroscopy have been used to determine the structures and concentrations of molecules formed during rapid cooling of reactants after they pass through the plasma. Emission spectroscopy also enables us to determine the temperatures at which these dynamic processes occur. A sample collection probe inserted from the open end of the reactor is used to collect condensed materials and analyze them ex situ using electron microscopy. The preliminary results of two separate investigations involving the condensation of metal oxides and chemical kinetics of high-temperature gas reactions are discussed.

Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering.

Directory of Open Access Journals (Sweden)

Athanasios Ch Mitropoulos

Full Text Available Everett's theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a at a common point the system can reach in a finite (not an infinite number of ways, b a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM. Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed.

Scanning of Adsorption Hysteresis In Situ with Small Angle X-Ray Scattering

Science.gov (United States)

Mitropoulos, Athanasios Ch.; Favvas, Evangelos P.; Stefanopoulos, Konstantinos L.; Vansant, Etienne F.

2016-01-01

Everett’s theorem-6 of the domain theory was examined by conducting adsorption in situ with small angle x-ray scattering (SAXS) supplemented by the contrast matching technique. The study focuses on the spectrum differences of a point to which the system arrives from different scanning paths. It is noted that according to this theorem at a common point the system has similar macroscopic properties. Furthermore it was examined the memory string of the system. We concluded that opposite to theorem-6: a) at a common point the system can reach in a finite (not an infinite) number of ways, b) a correction for the thickness of the adsorbed film prior to capillary condensation is necessary, and c) the scattering curves although at high-Q values coincide, at low-Q values are different indicating different microscopic states. That is, at a common point the system holds different metastable states sustained by hysteresis effects. These metastable states are the ones which highlight the way of a system back to a return point memory (RPM). Entering the hysteresis loop from different RPMs different histories are implanted to the paths toward the common point. Although in general the memory points refer to relaxation phenomena, they also constitute a characteristic feature of capillary condensation. Analogies of the no-passing rule and the adiabaticity assumption in the frame of adsorption hysteresis are discussed. PMID:27741263

A High Rigidity and Precision Scanning Tunneling Microscope with Decoupled XY and Z Scans.

Science.gov (United States)

Chen, Xu; Guo, Tengfei; Hou, Yubin; Zhang, Jing; Meng, Wenjie; Lu, Qingyou

2017-01-01

A new scan-head structure for the scanning tunneling microscope (STM) is proposed, featuring high scan precision and rigidity. The core structure consists of a piezoelectric tube scanner of quadrant type (for XY scans) coaxially housed in a piezoelectric tube with single inner and outer electrodes (for Z scan). They are fixed at one end (called common end). A hollow tantalum shaft is coaxially housed in the XY -scan tube and they are mutually fixed at both ends. When the XY scanner scans, its free end will bring the shaft to scan and the tip which is coaxially inserted in the shaft at the common end will scan a smaller area if the tip protrudes short enough from the common end. The decoupled XY and Z scans are desired for less image distortion and the mechanically reduced scan range has the superiority of reducing the impact of the background electronic noise on the scanner and enhancing the tip positioning precision. High quality atomic resolution images are also shown.

A High Rigidity and Precision Scanning Tunneling Microscope with Decoupled XY and Z Scans

Directory of Open Access Journals (Sweden)

Xu Chen

2017-01-01

Full Text Available A new scan-head structure for the scanning tunneling microscope (STM is proposed, featuring high scan precision and rigidity. The core structure consists of a piezoelectric tube scanner of quadrant type (for XY scans coaxially housed in a piezoelectric tube with single inner and outer electrodes (for Z scan. They are fixed at one end (called common end. A hollow tantalum shaft is coaxially housed in the XY-scan tube and they are mutually fixed at both ends. When the XY scanner scans, its free end will bring the shaft to scan and the tip which is coaxially inserted in the shaft at the common end will scan a smaller area if the tip protrudes short enough from the common end. The decoupled XY and Z scans are desired for less image distortion and the mechanically reduced scan range has the superiority of reducing the impact of the background electronic noise on the scanner and enhancing the tip positioning precision. High quality atomic resolution images are also shown.

Bulk ultrasonic NDE of metallic components at high temperature using magnetostrictive transducers

Science.gov (United States)

Ashish, Antony Jacob; Rajagopal, Prabhu; Balasubramaniam, Krishnan; Kumar, Anish; Rao, B. Purnachandra; Jayakumar, Tammana

2017-02-01

Online ultrasonic NDE at high-temperature is of much interest to the power, process and automotive industries in view of possible savings in downtime. This paper describes a novel approach to developing ultrasonic transducers capable of high-temperature in-situ operation using the principle of magnetostriction. Preliminary design from previous research by the authors [1] is extended for operation at 1 MHz, and at elevated temperatures by amorphous metallic strips as the magnetostrictive core. Ultrasonic signals in pulse-echo mode are experimentally obtained from the ultrasonic transducer thus developed, in a simulated high-temperature environment of 350 °C for 10 hours. Advantages and challenges for practical deployment of this approach are discussed.

High-resolution fiber-optic microendoscopy for in situ cellular imaging.

Science.gov (United States)

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

2011-01-11

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

In Situ Elevated Temperature Testing of Fly Ash Based Geopolymer Composites

Science.gov (United States)

Vickers, Les; Pan, Zhu; Tao, Zhong; van Riessen, Arie

2016-01-01

In situ elevated temperature investigations using fly ash based geopolymers filled with alumina aggregate were undertaken. Compressive strength and short term creep tests were carried out to determine the onset temperature of viscous flow. Fire testing using the standard cellulose curve was performed. Applying a load to the specimen as the temperature increased reduced the temperature at which viscous flow occurred (compared to test methods with no applied stress). Compressive strength increased at the elevated temperature and is attributed to viscous flow and sintering forming a more compact microstructure. The addition of alumina aggregate and reduction of water content reduced the thermal conductivity. This led to the earlier onset and shorter dehydration plateau duration times. However, crack formation was reduced and is attributed to smaller thermal gradients across the fire test specimen. PMID:28773568

In Situ Elevated Temperature Testing of Fly Ash Based Geopolymer Composites

Directory of Open Access Journals (Sweden)

Les Vickers

2016-06-01

Full Text Available In situ elevated temperature investigations using fly ash based geopolymers filled with alumina aggregate were undertaken. Compressive strength and short term creep tests were carried out to determine the onset temperature of viscous flow. Fire testing using the standard cellulose curve was performed. Applying a load to the specimen as the temperature increased reduced the temperature at which viscous flow occurred (compared to test methods with no applied stress. Compressive strength increased at the elevated temperature and is attributed to viscous flow and sintering forming a more compact microstructure. The addition of alumina aggregate and reduction of water content reduced the thermal conductivity. This led to the earlier onset and shorter dehydration plateau duration times. However, crack formation was reduced and is attributed to smaller thermal gradients across the fire test specimen.

Energy Storage of Polyarylene Ether Nitriles at High Temperature

Science.gov (United States)

Tang, Xiaohe; You, Yong; Mao, Hua; Li, Kui; Wei, Renbo; Liu, Xiaobo

2018-03-01

Polyarylene ether nitrile (PEN) was synthesized and used as film capacitors for energy storage at high temperature. Scanning electron microscopy observation indicated that the films of PEN have pinholes at nanoscales which restricted the energy storage properties of the material. The pinhole shadowing effect through which the energy storage properties of PEN were effectively improved to be 2.3 J/cm3 was observed by using the overlapped film of PEN. The high glass transition temperature (T g) of PEN was as high as 216 °C and PEN film showed stable dielectric constant, breakdown strength and energy storage density before the T g. The PEN films will be a potential candidate as high performance electronic storage materials used at high temperature.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

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

Science.gov (United States)

Buchner, Othmar; Neuner, Gilbert

2011-11-01

Winter frost resistance (WFR), midwinter frost hardening and frost dehardening potential of Pinus cembra L. were determined in situ by means of a novel low-temperature freezing system at the alpine timberline ecotone (1950 m a.s.l., Mt Patscherkofel, Innsbruck, Austria). In situ liquid nitrogen (LN₂)-quenching experiments should check whether maximum WFR of P. cembra belonging to the frost hardiest conifer group, being classified in US Department of Agriculture climatic zone 1, suffices to survive dipping into LN₂ (-196 °C). Viability was assessed in a field re-growth test. Maximum in situ WFR (LT₅₀) of leaves was frost hardening treatment (12 days at -20 °C followed by 3 days at -50 °C) to induce maximum WFR. Temperature treatments applied in the field significantly affected the actual WFR. In January a frost hardening treatment (21 days at -20 °C) led to a significant increase of WFR (buds: -62 °C to frost dehardening (buds: -32.6 °C to -10.2 °C; leaves: -32.7 to -16.4 °C) followed by significantly earlier bud swelling and burst in late winter. Strikingly, both temperature treatments, either increased air temperature (+10.1 °C) or increased soil temperature (+6.5 °C), were similarly effective. This high readiness to frost harden and deharden in winter in the field must be considered to be of great significance for future winter survival of P. cembra. Determination of WFR in field re-growth tests appears to be a valuable tool for critically judging estimates of WFR obtained on detached twigs in an ecological context.

A combined scanning tunneling microscope-atomic layer deposition tool.

Science.gov (United States)

Mack, James F; Van Stockum, Philip B; Iwadate, Hitoshi; Prinz, Fritz B

2011-12-01

We have built a combined scanning tunneling microscope-atomic layer deposition (STM-ALD) tool that performs in situ imaging of deposition. It operates from room temperature up to 200 °C, and at pressures from 1 × 10(-6) Torr to 1 × 10(-2) Torr. The STM-ALD system has a complete passive vibration isolation system that counteracts both seismic and acoustic excitations. The instrument can be used as an observation tool to monitor the initial growth phases of ALD in situ, as well as a nanofabrication tool by applying an electric field with the tip to laterally pattern deposition. In this paper, we describe the design of the tool and demonstrate its capability for atomic resolution STM imaging, atomic layer deposition, and the combination of the two techniques for in situ characterization of deposition.

Immersion-scanning-tunneling-microscope for long-term variable-temperature experiments at liquid-solid interfaces

Science.gov (United States)

Ochs, Oliver; Heckl, Wolfgang M.; Lackinger, Markus

2018-05-01

Fundamental insights into the kinetics and thermodynamics of supramolecular self-assembly on surfaces are uniquely gained by variable-temperature high-resolution Scanning-Tunneling-Microscopy (STM). Conventionally, these experiments are performed with standard ambient microscopes extended with heatable sample stages for local heating. However, unavoidable solvent evaporation sets a technical limit on the duration of these experiments, hence prohibiting long-term experiments. These, however, would be highly desirable to provide enough time for temperature stabilization and settling of drift but also to study processes with inherently slow kinetics. To overcome this dilemma, we propose a STM that can operate fully immersed in solution. The instrument is mounted onto the lid of a hermetically sealed heatable container that is filled with the respective solution. By closing the container, both the sample and microscope are immersed in solution. Thereby solvent evaporation is eliminated and an environment for long-term experiments with utmost stable and controllable temperatures between room-temperature and 100 °C is provided. Important experimental requirements for the immersion-STM and resulting design criteria are discussed, the strategy for protection against corrosive media is described, the temperature stability and drift behavior are thoroughly characterized, and first long-term high resolution experiments at liquid-solid interfaces are presented.

In Situ UV-Visible Assessment of Iron-Based High-Temperature Water-Gas Shift Catalysts Promoted with Lanthana: An Extent of Reduction Study

Directory of Open Access Journals (Sweden)

Basseem B. Hallac

2018-02-01

Full Text Available The extent of reduction of unsupported iron-based high-temperature water-gas shift catalysts with small (<5 wt % lanthana contents was studied using UV-visible spectroscopy. Temperature- programmed reduction measurements showed that lanthana content higher than 0.5 wt % increased the extent of reduction to metallic Fe, while 0.5 wt % of lanthana facilitated the reduction to Fe3O4. In situ measurements on the iron oxide catalysts using mass and UV-visible spectroscopies permitted the quantification of the extent of reduction under temperature-programmed reduction and high-temperature water-gas shift conditions. The oxidation states were successfully calibrated against normalized absorbance spectra of visible light using the Kubelka-Munk theory. The normalized absorbance relative to the fully oxidized Fe2O3 increased as the extent of reduction increased. XANES suggested that the average bulk iron oxidation state during the water-gas shift reaction was Fe+2.57 for the catalyst with no lanthana and Fe+2.54 for the catalysts with 1 wt % lanthana. However, the UV-vis spectra suggest that the surface oxidation state of iron would be Fe+2.31 for the catalyst with 1 wt % lanthana if the oxidation state of iron in the catalyst with 0 wt % lanthana were Fe+2.57. The findings of this paper emphasize the importance of surface sensitive UV-visible spectroscopy for determining the extent of catalyst reduction during operation. The paper highlights the potential to use bench-scale UV-visible spectroscopy to study the surface chemistry of catalysts instead of less-available synchrotron X-ray radiation facilities.

Elevated temperature erosion studies on some materials for high temperature applications

International Nuclear Information System (INIS)

Zhou Jianren.

1991-01-01

The surface degradation of materials due to high temperature erosion or combined erosion corrosion is a serious problem in many industrial and aeronautical applications. As such, it has become an important design consideration in many situations. The materials investigated in the present studies are stainless steels, Ti-6Al-4V, alumina ceramics, with and without silicate glassy phase, and zirconia. These are some of the potential materials for use in the high temperature erosive-corrosive environments. The erosion or erosion-corrosion experiments were performed in a high temperature sand-blast type of test rig. The variables studied included the temperature, material composition, heat treatment condition, impingement velocity and angle, erodent concentration, etc. The morphological features of the eroded or eroded-corroded surfaces, substrate deformation, and oxide characteristics were studied by optical and scanning electron microscopy, X-ray diffraction, energy dispersive X-ray spectroscopy, thermogravimetric analysis. The scratch test, single ball impact, and indentation tests were used to understand the behavior of oxide film in particle impacts. Based on these studies, the understanding of the mechanisms involved in the mechanical or combined mechanical and chemical actions in erosion was developed

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

Science.gov (United States)

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

Microstructural characteristics of high-temperature oxidation in nickel-base superalloy

International Nuclear Information System (INIS)

Khalid, F.A.

1997-01-01

Superalloys are used for aerospace and nuclear applications where they can withstand high-temperature and severe oxidizing conditions. High-temperature oxidation behavior of a nickel-base superalloy is examined using optical and scanning electron microscopical techniques. The morphology of the oxide layers developed is examined, and EDX microanalysis reveals diffusion of the elements across the oxide-metal interface. Evidence of internal oxidation is presented, and the role of structural defects is considered. The morphology of the oxide-metal interface formed in the specimens exposed in steam and air is examined to elucidate the mechanism of high-temperature oxidation

In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

International Nuclear Information System (INIS)

Yun, Di; Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M.

2015-01-01

U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

In situ TEM and synchrotron characterization of U–10Mo thin specimen annealed at the fast reactor temperature regime

Energy Technology Data Exchange (ETDEWEB)

Yun, Di, E-mail: diyun1979@xjtu.edu.cn [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Xi' an Jiao Tong University, 28 Xian Ning West Road, Xi' an 710049 (China); Mo, Kun; Mohamed, Walid; Ye, Bei; Kirk, Marquis A.; Baldo, Peter; Xu, Ruqing; Yacout, Abdellatif M. [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

2015-12-15

U–Mo metallic alloys have been extensively used for the Reduced Enrichment for Research and Test Reactors (RERTR) program, which is now known as the Office of Material Management and Minimization under the Conversion Program. This fuel form has also recently been proposed as fast reactor metallic fuels in the recent DOE Ultra-high Burnup Fast Reactor project. In order to better understand the behavior of U–10Mo fuels within the fast reactor temperature regime, a series of annealing and characterization experiments have been performed. Annealing experiments were performed in situ at the Intermediate Voltage Electron Microscope (IVEM-Tandem) facility at Argonne National Laboratory (ANL). An electro-polished U–10Mo alloy fuel specimen was annealed in situ up to 700 °C. At an elevated temperature of about 540 °C, the U–10Mo specimen underwent a relatively slow microstructure transition. Nano-sized grains were observed to emerge near the surface. At the end temperature of 700 °C, the near-surface microstructure had evolved to a nano-crystalline state. In order to clarify the nature of the observed microstructure, Laue diffraction and powder diffraction experiments were carried out at beam line 34-ID of the Advanced Photon Source (APS) at ANL. Phases present in the as-annealed specimen were identified with both Laue diffraction and powder diffraction techniques. The U–10Mo was found to recrystallize due to thermally-induced recrystallization driven by a high density of pre-existing dislocations. A separate in situ annealing experiment was carried out with a Focused Ion Beam processed (FIB) specimen. A similar microstructure transition occurred at a lower temperature of about 460 °C with a much faster transition rate compared to the electro-polished specimen. - Highlights: • TEM annealing experiments were performed in situ at the IVEM facility up to fast reactor temperature. • At 540 °C, the U-10Mo specimen underwent a slow microstructure transition

Advantages of the in-situ LTP distortion profile test on high-heat-load mirrors and applications

International Nuclear Information System (INIS)

Qian, S.; Jark, W.; Sostero, G.; Gambitta, A.; Mazzolini, F.; Savoia, A.

1996-01-01

The first in-situ distortion profile measurement of a high heat load mirror by use of the penta-prism LTP is presented. A maximum height distortion of 0.47 micron in tangential direction over a length of 180 mm was measured for an internally water-cooled mirror of a undulator beam line at ELETTRA while exposed to a total emitted power of 600 W (undulator gap 30 mm and current 180 mA). The experiment has an accuracy and repeatability of 0.04 micron. The test schematic and the test equipment are presented. Two measuring methods to scan a penta-prism being installed either outside or inside the vacuum chamber are introduced. Advantages and some possible applications of adopting the penta-prism LTP to make the in-situ profile test are explained

High temperature structural and magnetic properties of cobalt nanorods

Energy Technology Data Exchange (ETDEWEB)

Ait Atmane, Kahina [Univ. Paris Diderot, Sorbonne Paris Cite, ITODYS, UMR CNRS 7086, 15 rue J.-A. de Baief, 75205 Paris Cedex 13 (France); Zighem, Fatih [Laboratoire Leon Brillouin, CEA CNRS UMR 12, IRAMIS, CEA-Saclay, 91191 Gif sur Yvette (France); Soumare, Yaghoub [Univ. Paris Diderot, Sorbonne Paris Cite, ITODYS, UMR CNRS 7086, 15 rue J.-A. de Baief, 75205 Paris Cedex 13 (France); Ibrahim, Mona; Boubekri, Rym [Universite de Toulouse, LPCNO, INSA CNRS UMR 5215, 135 av. de Rangueil, 31077 Toulouse Cedex 4 (France); Maurer, Thomas [Laboratoire Leon Brillouin, CEA CNRS UMR 12, IRAMIS, CEA-Saclay, 91191 Gif sur Yvette (France); Margueritat, Jeremie [Univ. Paris Diderot, Sorbonne Paris Cite, ITODYS, UMR CNRS 7086, 15 rue J.-A. de Baief, 75205 Paris Cedex 13 (France); Piquemal, Jean-Yves, E-mail: jean-yves.piquemal@univ-paris-diderot.fr [Univ. Paris Diderot, Sorbonne Paris Cite, ITODYS, UMR CNRS 7086, 15 rue J.-A. de Baief, 75205 Paris Cedex 13 (France); Ott, Frederic; Chaboussant, Gregory [Laboratoire Leon Brillouin, CEA CNRS UMR 12, IRAMIS, CEA-Saclay, 91191 Gif sur Yvette (France); Schoenstein, Frederic; Jouini, Noureddine [LSPM, CNRS UPR 9001, Universite Paris XIII, Institut Galilee, 99 av. J.-B. Clement, 93430 Villetaneuse (France); Viau, Guillaume, E-mail: gviau@insa-toulouse.fr [Universite de Toulouse, LPCNO, INSA CNRS UMR 5215, 135 av. de Rangueil, 31077 Toulouse Cedex 4 (France)

2013-01-15

We present in this paper the structural and magnetic properties of high aspect ratio Co nanoparticles ({approx}10) at high temperatures (up to 623 K) using in-situ X ray diffraction (XRD) and SQUID characterizations. We show that the anisotropic shapes, the structural and texture properties are preserved up to 500 K. The coercivity can be modelled by {mu}{sub 0}H{sub C}=2(K{sub MC}+K{sub shape})/M{sub S} with K{sub MC} the magnetocrystalline anisotropy constant, K{sub shape} the shape anisotropy constant and M{sub S} the saturation magnetization. H{sub C} decreases linearly when the temperature is increased due to the loss of the Co magnetocrystalline anisotropy contribution. At 500 K, 50% of the room temperature coercivity is preserved corresponding to the shape anisotropy contribution only. We show that the coercivity drop is reversible in the range 300-500 K in good agreement with the absence of particle alteration. Above 525 K, the magnetic properties are irreversibly altered either by sintering or by oxidation. - Graphical abstract: We present in this paper the structural and magnetic properties of high aspect ratio Co nanorods ({approx}10) at high temperatures (up to 623 K) using in-situ X-ray diffraction and SQUID characterizations. We show that the anisotropic shapes, the structural and texture properties are preserved up to 500 K. Above 525 K, the magnetic properties are irreversibly altered either by sintering or by oxidation. Highlights: Black-Right-Pointing-Pointer Ferromagnetic Co nanorods are prepared using the polyol process. Black-Right-Pointing-Pointer The structural and texture properties of the Co nanorods are preserved up to 500 K. Black-Right-Pointing-Pointer The magnetic properties of the Co nanorods are irreversibly altered above 525 K.

Beamline electrostatic levitator for in situ high energy x-ray diffraction studies of levitated solids and liquids

Energy Technology Data Exchange (ETDEWEB)

Gangopadhyay, A.K.; Lee, G.W.; Kelto, K.F.; Rogers, J.R.; Goldman, A.I.; Robinson, D.S.; Rathz, T.J.; Hyers, R.W. (WU); (UAB); (NASA); (UMASS, Amherst)

2010-07-19

Determinations of the phase formation sequence, crystal structures and the thermo-physical properties of materials at high temperatures are hampered by contamination from the sample container and environment. Containerless processing techniques, such as electrostatic (ESL), electromagnetic, aerodynamic, and acoustic levitation, are most suitable for these studies. An adaptation of ESL for in situ structural studies of a wide range of materials using high energy (30-130 keV) x rays at a synchrotron source is described here. This beamline ESL (BESL) allows the in situ determination of the atomic structures of equilibrium solid and liquid phases, undercooled liquids and time-resolved studies of solid-solid and liquid-solid phase transformations. The use of area detectors enables the rapid acquisition of complete diffraction patterns over a wide range (0.5-14 {angstrom}{sup -1}) of reciprocal space. The wide temperature range (300-2500 K), containerless processing environment under high vacuum (10{sup -7}-10{sup -8} Torr), and fast data acquisition capability, make BESL particularly well suited for phase stability studies of high temperature solids and liquids. An additional, but important, feature of BESL is the capability for simultaneous measurements of a host of thermo-physical properties including the specific heat, enthalpy of transformation, solidus and liquidus temperatures, density, viscosity, and surface tension, all on the same sample during the structural measurements.

Transformations of gold nanoparticles investigated using variable temperature high-resolution transmission electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Young, N.P. [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom); Huis, M.A. van; Zandbergen, H.W. [Kavli Institute of Nanoscience, Delft University of Technolgy, Lorentzweg 1, NL-2628CJ, Delft, The Netherlands. (Netherlands); Xu, H. [Department of Geology and Geophysics, and Materials Science Program, University of Wisconsin-Madison, Madison, WI (United States); Kirkland, A.I., E-mail: angus.kirkland@materials.ox.ac.uk [Department of Materials, University of Oxford, Parks Road, Oxford OX1 3PH (United Kingdom)

2010-04-15

Recently designed advanced in-situ specimen holders for transmission electron microscopy (TEM) have been used in studies of gold nanoparticles. We report results of variable temperature TEM experiments in which structural transformations have been correlated with specimen temperature, allowing general trends to be identified. Transformation to a decahedral morphology for particles in the size range 5-12 nm was observed for the majority of particles regardless of their initial structure. Following in-situ annealing, decahedra were found to be stable at room temperature, confirming this as the equilibrium morphology, in agreement with recently calculated phase diagrams. Other transitions at low temperature in addition to surface roughening have also been observed and correlated with the same nanoscale phase diagram. Investigations of gold particles at high temperature have revealed evidence for co-existing solid and liquid phases. Overall, these results are important in a more precise understanding of the structure and action of catalytic gold nanoparticles and in the experimental verification of theoretical calculations.

In situ observation of stress relaxation in epitaxial graphene

International Nuclear Information System (INIS)

N'Diaye, Alpha T; Coraux, Johann; Busse, Carsten; Michely, Thomas; Gastel, Raoul van; Poelsema, Bene; MartInez-Galera, Antonio J; Gomez-RodrIguez, Jose M; Hattab, Hichem; Wall, Dirk; Heringdorf, Frank-J Meyer zu; Hoegen, Michael Horn-von

2009-01-01

Upon cooling, branched line defects develop in epitaxial graphene grown at high temperature on Pt(111) and Ir(111). Using atomically resolved scanning tunneling microscopy, we demonstrate that these defects are wrinkles in the graphene layer, i.e. stripes of partially delaminated graphene. With low energy electron microscopy (LEEM), we investigate the wrinkling phenomenon in situ. Upon temperature cycling, we observe hysteresis in the appearance and disappearance of the wrinkles. Simultaneously with wrinkle formation a change in bright field imaging intensity of adjacent areas and a shift in the moire spot positions for micro diffraction of such areas takes place. The stress relieved by wrinkle formation results from the mismatch in thermal expansion coefficients of graphene and the substrate. A simple one-dimensional model taking into account the energies related to strain, delamination and bending of graphene is in qualitative agreement with our observations.

Multipurpose high-pressure high-temperature diamond-anvil cell with a novel high-precision guiding system and a dual-mode pressurization device

Science.gov (United States)

Pippinger, Thomas; Miletich, Ronald; Burchard, Michael

2011-09-01

A novel diamond-anvil cell (DAC) design has been constructed and tested for in situ applications at high-pressure (HP) operations and has proved to be suitable even for HP sample environments at non-ambient temperature conditions. The innovative high-precision guiding mechanism, comparable to a dog clutch, consists of perpendicular planar sliding-plane elements and is integrated directly into the base body of the cylindrically shaped DAC. The combination of two force-generating devices, i.e., mechanical screws and an inflatable gas membrane, allows the user to choose independently between, and to apply individually, two different forcing mechanisms for pressure generation. Both mechanisms are basically independent of each other, but can also be operated simultaneously. The modularity of the DAC design allows for an easy exchange of functional core-element groups optimized not only for various analytical in situ methods but also for HP operation with or without high-temperature (HT) application. For HP-HT experiments a liquid cooling circuit inside the specific inner modular groups has been implemented to obtain a controlled and limited heat distribution within the outer DAC body.

High-Temperature Surface-Acoustic-Wave Transducer

Science.gov (United States)

Zhao, Xiaoliang; Tittmann, Bernhard R.

2010-01-01

Aircraft-engine rotating equipment usually operates at high temperature and stress. Non-invasive inspection of microcracks in those components poses a challenge for the non-destructive evaluation community. A low-profile ultrasonic guided wave sensor can detect cracks in situ. The key feature of the sensor is that it should withstand high temperatures and excite strong surface wave energy to inspect surface/subsurface cracks. As far as the innovators know at the time of this reporting, there is no existing sensor that is mounted to the rotor disks for crack inspection; the most often used technology includes fluorescent penetrant inspection or eddy-current probes for disassembled part inspection. An efficient, high-temperature, low-profile surface acoustic wave transducer design has been identified and tested for nondestructive evaluation of structures or materials. The development is a Sol-Gel bismuth titanate-based surface-acoustic-wave (SAW) sensor that can generate efficient surface acoustic waves for crack inspection. The produced sensor is very thin (submillimeter), and can generate surface waves up to 540 C. Finite element analysis of the SAW transducer design was performed to predict the sensor behavior, and experimental studies confirmed the results. One major uniqueness of the Sol-Gel bismuth titanate SAW sensor is that it is easy to implement to structures of various shapes. With a spray coating process, the sensor can be applied to surfaces of large curvatures. Second, the sensor is very thin (as a coating) and has very minimal effect on airflow or rotating equipment imbalance. Third, it can withstand temperatures up to 530 C, which is very useful for engine applications where high temperature is an issue.

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

Science.gov (United States)

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

2017-02-01

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

Narrow, highly P-doped, planar wires in silicon created by scanning probe microscopy

Energy Technology Data Exchange (ETDEWEB)

Ruess, F J [Australian Research Council Centre of Excellence for Quantum Computer Technology, University of New South Wales, Sydney, NSW 2052 (Australia); Goh, K E J [Australian Research Council Centre of Excellence for Quantum Computer Technology, University of New South Wales, Sydney, NSW 2052 (Australia); Butcher, M J [School of Physics, University of New South Wales, Sydney, NSW 2052 (Australia); Reusch, T C G [Australian Research Council Centre of Excellence for Quantum Computer Technology, University of New South Wales, Sydney, NSW 2052 (Australia); Oberbeck, L [Australian Research Council Centre of Excellence for Quantum Computer Technology, University of New South Wales, Sydney, NSW 2052 (Australia); Weber, B [School of Physics, University of New South Wales, Sydney, NSW 2052 (Australia); Hamilton, A R [School of Physics, University of New South Wales, Sydney, NSW 2052 (Australia); Simmons, M Y [Australian Research Council Centre of Excellence for Quantum Computer Technology, University of New South Wales, Sydney, NSW 2052 (Australia)

2007-01-31

We demonstrate the use of a scanning tunnelling microscope (STM) to pattern buried, highly planar phosphorus-doped silicon wires with widths down to the sub-10 nm level. We confirm the structural integrity of these wires using both buried dopant imaging techniques and ex situ electrical characterization. Four terminal I-V characteristics at 4 K show ohmic behaviour for all wires with resistivities between 1 and 24 x 10{sup -8} {omega} cm. Magnetotransport measurements reveal that conduction is dominated by disordered scattering with quantum corrections consistent with 2D weak localization theory. Our results show that these quantum corrections become more pronounced as the electron phase coherence length approaches the width of the wire.

High-temperature elastic properties of in situ-reinforced Si3N4

International Nuclear Information System (INIS)

Swift, Geoffrey A.; Uestuendag, Ersan; Clausen, Bjoern; Bourke, Mark A.M.; Lin, H.-T.

2003-01-01

A high-temperature tensile stress study of a monolithic silicon nitride (Si 3 N 4 ) was performed with time-of-flight neutron diffraction. A dedicated engineering diffractometer was employed at temperatures reaching 1375 deg. C. Rietveld refinements of diffraction spectra allowed the determination of (1) the coefficient of thermal expansion tensor during heating and (2) lattice strains during loading. The stress-strain response of individual lattice reflections was used to calculate the single-crystal elastic stiffness tensor of Si 3 N 4 at 1375 deg. C via a self-consistent model

Six-axis multi-anvil press for high-pressure, high-temperature neutron diffraction experiments

Energy Technology Data Exchange (ETDEWEB)

Sano-Furukawa, A., E-mail: sano.asami@jaea.go.jp; Hattori, T. [Quantum Beam Science Center, Japan Atomic Energy Agency, Ibaraki 319-1195 (Japan); J-PARC Center, Japan Atomic Energy Agency, Ibaraki 319-1195 (Japan); Arima, H. [Institute for Materials Research, Tohoku University, Sendai 980-8577 (Japan); Yamada, A. [The University of Shiga Prefecture, Shiga 522-8533 (Japan); Tabata, S.; Kondo, M.; Nakamura, A. [Sumitomo Heavy Industries Co., Ltd., Ehime 792-0001 (Japan); Kagi, H.; Yagi, T. [Geochemical Research Center, Graduate School of Science, The University of Tokyo, Tokyo 113-0033 (Japan)

2014-11-15

We developed a six-axis multi-anvil press, ATSUHIME, for high-pressure and high-temperature in situ time-of-flight neutron powder diffraction experiments. The press has six orthogonally oriented hydraulic rams that operate individually to compress a cubic sample assembly. Experiments indicate that the press can generate pressures up to 9.3 GPa and temperatures up to 2000 K using a 6-6-type cell assembly, with available sample volume of about 50 mm{sup 3}. Using a 6-8-type cell assembly, the available conditions expand to 16 GPa and 1273 K. Because the six-axis press has no guide blocks, there is sufficient space around the sample to use the aperture for diffraction and place an incident slit, radial collimators, and a neutron imaging camera close to the sample. Combination of the six-axis press and the collimation devices realized high-quality diffraction pattern with no contamination from the heater or the sample container surrounding the sample. This press constitutes a new tool for using neutron diffraction to study the structures of crystals and liquids under high pressures and temperatures.

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

International Nuclear Information System (INIS)

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

2014-01-01

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

Tritium Removal from JET and TFTR Tiles by a Scanning Laser

International Nuclear Information System (INIS)

Skinner, C.H.; Bekris, N.; Coad, J.P.; Gentile, C.A.; Glugla, M.

2002-01-01

Fast and efficient tritium removal is needed for future D-T machines with carbon plasma-facing components. A novel method for tritium release has been demonstrated on co-deposited layers on tiles retrieved from the Tokamak Fusion Test Reactor (TFTR) and from the Joint European Torus (JET). A scanning continuous wave neodymium laser beam was focused to =100 W/mm2 and scanned at high speed over the co-deposits, heating them to temperatures =2000 C for about 10 ms in either air or argon atmospheres. Fiber optic coupling between the laser and scanner was implemented. Up to 87% of the co-deposited tritium was thermally desorbed from the JET and TFTR samples. This technique appears to be a promising in-situ method for tritium removal in a next-step D-T device as it avoids oxidation, the associated de-conditioning of the plasma-facing surfaces, and the expense of processing large quantities of tritium oxide

High pressure-temperature polymorphism of 1,1-diamino-2,2-dinitroethylene

International Nuclear Information System (INIS)

Bishop, M M; Dattelbaum, D M; Velisavljevic, N; Chellappa, R S; Liu, Z; Preston, D N; Sandstrom, M M; Vohra, Y K

2014-01-01

1,1-diamino-2,2-dinitroethylene (FOX-7) is a low sensitivity energetic material with performance comparable to commonly used secondary explosives such as RDX and HMX. At ambient pressure, FOX-7 exhibits complex polymorphism with at least three structurally distinct phases (α, β, and γ). In this study, we have investigated the high pressure-temperature stability of FOX-7 polymorphs using synchrotron mid-infrared (MIR) spectroscopy. At ambient pressure, our MIR spectra and corresponding differential scanning calorimetry (DSC) measurements confirmed the known α → β (∼110 °C) and α → β (∼160 °C) structural phase transitions; as well as, indicated an additional transition γ → (∼210 °C), with the δ phase being stable up to ∼251 °C prior to decomposition. In situ MIR spectra obtained during isobaric heating at 0.9 GPa, revealed a potential α → β transition that could occur as early as 180 °C, while β → β+δ phase transition shifted to ∼300 °C with suppression of γ phase. Decomposition was observed slightly above 325 °C at 0.9 GPa.

Analysis on High Temperature Aging Property of Self-brazing Aluminum Honeycomb Core at Middle Temperature

Directory of Open Access Journals (Sweden)

ZHAO Huan

2016-11-01

Full Text Available Tension-shear test was carried out on middle temperature self-brazing aluminum honeycomb cores after high temperature aging by micro mechanical test system, and the microstructure and component of the joints were observed and analyzed using scanning electron microscopy and energy dispersive spectroscopy to study the relationship between brazing seam microstructure, component and high temperature aging properties. Results show that the tensile-shear strength of aluminum honeycomb core joints brazed by 1060 aluminum foil and aluminum composite brazing plate after high temperature aging(200℃/12h, 200℃/24h, 200℃/36h is similar to that of as-welded joints, and the weak part of the joint is the base metal which is near the brazing joint. The observation and analysis of the aluminum honeycomb core microstructure and component show that the component of Zn, Sn at brazing seam is not much affected and no compound phase formed after high temperature aging; therefore, the main reason for good high temperature aging performance of self-brazing aluminum honeycomb core is that no obvious change of brazing seam microstructure and component occurs.

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

DEFF Research Database (Denmark)

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

2014-01-01

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

High-resolution spectroscopy of gases at elevated temperatures for industrial applications

DEFF Research Database (Denmark)

measurements have to be done in a very aggressive and unstable in time hot gas environment which is realized, for example, in boilers, gasifires and engines. An optically based technique is beneficial because it is non-intrusive, accurate, fast and can be performed in situ for various extremely hard conditions....... The quality of the in situ gas composition measurements depends, among other things, on the quality of reference data (i.e. partial absorption spectra gases of interest) which are in general highly temperature dependent. Existing databases (e.g. HITRAN, HITEMP or CDSD) can normally be used for absorption...

Voltammetry and in situ scanning tunnelling spectroscopy of osmium, iron, and ruthenium complexes of 2,2′:6′,2′′-terpyridine covalently linked to Au(111)-electrodes

DEFF Research Database (Denmark)

Salvatore, Princia; Hansen, Allan Glargaard; Moth-Poulsen, Kasper

2011-01-01

prepared in situ by first linking the terpy ligand to the surface via the S-atom, followed by addition of suitable metal compounds. The metal-terpy SAMs were studied by cyclic voltammetry (CV), and in situ scanning tunnelling microscopy with full electrochemical potential control of substrate and tip (in...

High-temperature stability of yttria-stabilized zirconia thermal barrier ...

Indian Academy of Sciences (India)

The coatings before and after IR heating were investigated by scanning electron microscopy, X-ray diffraction, electron probe microanalysis, microhardness and residual stress measurements in order to understand the effect of thermal shock on the properties of the TBC. On account of these high-temperature properties, ...

In situ observation and neutron diffraction of NiTi powder sintering

International Nuclear Information System (INIS)

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

2014-01-01

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

N-Vinylcarbazole: As an Additive for Thermal Polymerization at Room Temperature with in situ Formation of Ag(0 Nanoparticules

Directory of Open Access Journals (Sweden)

Mohamad-Ali Tehfe

2015-08-01

Full Text Available N-vinylcarbazole (NVK is proposed as an additive for acrylates thermal free radical polymerization (FRP and epoxy thermal ring opening polymerization (ROP at room temperature. The new initiating systems are based on a silane/silver salt/N-vinylcarbazole interaction, which ensures good to excellent polymerization. Moreover, the polymerization is much more efficient under air than under argon. The effects of the N-vinylcarbazole, silane, silver salt and monomer structures are investigated. Interestingly, silver nanoparticles Ag(0 are formed in situ. The as-synthesized nanocomposite materials contained spherical nanoparticles homogeneously dispersed in the polymer matrices. Polymers and nanoparticles were characterized by Differential Scanning Calorimetry (DSC, Transmission Electron Microscopy (TEM, Energy-Dispersive X-ray Spectrometry (EDS, Fourier Transform Infrared Spectroscopy (FTIR, and UV-vis spectroscopy. A coherent picture of the involved chemical mechanisms is presented.

Calibration Transfer Between a Bench Scanning and a Submersible Diode Array Spectrophotometer for In Situ Wastewater Quality Monitoring in Sewer Systems.

Science.gov (United States)

Brito, Rita S; Pinheiro, Helena M; Ferreira, Filipa; Matos, José S; Pinheiro, Alexandre; Lourenço, Nídia D

2016-03-01

Online monitoring programs based on spectroscopy have a high application potential for the detection of hazardous wastewater discharges in sewer systems. Wastewater hydraulics poses a challenge for in situ spectroscopy, especially when the system includes storm water connections leading to rapid changes in water depth, velocity, and in the water quality matrix. Thus, there is a need to optimize and fix the location of in situ instruments, limiting their availability for calibration. In this context, the development of calibration models on bench spectrophotometers to estimate wastewater quality parameters from spectra acquired with in situ instruments could be very useful. However, spectra contain information not only from the samples, but also from the spectrophotometer generally invalidating this approach. The use of calibration transfer methods is a promising solution to this problem. In this study, calibration models were developed using interval partial least squares (iPLS), for the estimation of total suspended solids (TSS) and chemical oxygen demand (COD) in sewage from Ultraviolet-visible spectra acquired in a bench scanning spectrophotometer. The feasibility of calibration transfer to a submersible, diode array equipment, to be subsequently operated in situ, was assessed using three procedures: slope and bias correction (SBC); single wavelength standardization (SWS) on mean spectra; and local centering (LC). The results showed that SBC was the most adequate for the available data, adding insignificant error to the base model estimates. Single wavelength standardization was a close second best, potentially more robust, and independent of the base iPLS model. Local centering was shown to be inadequate for the samples and instruments used. © The Author(s) 2016.

Ratiometric Afterglow Nanothermometer for Simultaneous in Situ Bioimaging and Local Tissue Temperature Sensing

NARCIS (Netherlands)

Yang, J.; Liu, Y.; Zhao, Y.; Gong, Z.; Zhang, M.; Yan, D.; Zhu, H.; Liu, C.; Xu, C.; Zhang, H.

2017-01-01

Simultaneous in situ bioimage tracing and temperature sensing have been two of the foci of modern biomedicine that have given birth to designing novel luminescent nanothermometers with dual functions. To minimize the disadvantages of existing approaches, like the surface effect of nanoparticles,

A low temperature situ precipitation route to designing Zn-doped SnO2 photocatalyst with enhanced photocatalytic performance

International Nuclear Information System (INIS)

Jia, Xiaohua; Liu, Yingying; Wu, Xiangyang; Zhang, Zhen

2014-01-01

Highlights: • A new Zn doped SnO 2 photocatalyst was successfully achieved and characterized. • The Zn doped SnO 2 photocatalyst exhibited excellent photocatalytic activity and stability for the photodegradation RhB. • Photocatalytic mechanisms both under visible and UV–vis light irradiation were proposed. - Abstract: Zn doped SnO 2 nanoparticles have been fabricated through the low temperature situ precipitation technique. The morphology, structure and chemical composition of the nanoparticles are characterized using field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), UV–vis diffuse reflectance spectroscopy (DRS), Thermogravimetric-differential scanning calorimetry (TG–DSC) and UV–vis absorption spectroscopy. The products were also characterized by X-ray diffraction (XRD) and X-photoelectron spectrum (XPS), and the results indicated that Sn 4+ ions were successfully substituted by Zn 2+ . Their photocatalytic activities were evaluated using rhodamine B (RhB) as a decomposition objective. The results show that the Zn doped SnO 2 display higher photocatalytic activities in the degradation of RhB than pure ZnO products by exposure to UV irradiation. A possible reason of the increased photocatalytic activity of Zn doped SnO 2 is attributed to intrinsic oxygen vacancies in nanoparticles and extrinsic defect due to Zn hole doping

In situ response time measurements of RTD temperature sensors

International Nuclear Information System (INIS)

Goncalves, I.M.P.

1985-01-01

The loop-current-step-response test provides a mean for determining the time constant of resistence thermometers. The test consist in heating the sensor a few degrees above ambient temperature by causing a step pertubation in the electric current that flows through the sensor leads. The developed mathematical transformation permits to use data collected during the internal heating transient to predict the sensor response to perturbations in fluid temperature. Experimental data obtained show that the time constant determined by method is within 15 percent of true value. The loop-current-step-response test is a remote in situ test, which can be performed with the sensor installed in the process. Consequently it takes account the local heat transfer conditions, and appropriated for nuclear power plants, where sensors are installed in points of difficult access. (author) [pt

Two-Dimensional Cysteine and Cystine Cluster Networks on Au(111) Disclosed by Voltammetry and in Situ Scanning Tunneling Microscopy

DEFF Research Database (Denmark)

Zhang, Jingdong; Chi, Qijin; Nielsen, Jens Ulrik

2000-01-01

Microscopic structures for molecular monolayers of L-cysteine and L-cystine assembled on Au(111) have been disclosed by employing electrochemistry and in situ scanning tunneling microscopy (STM). HighresolutionSTMimages show that the adlayers of both cyteine and cystine exhibit highly......-ordered networklike clusters with (3x3 6)R30° structure. By combining the surface coverage estimated from voltammetric data, each cluster is demonstrated to include six individual cysteine molecules or three cystine molecules. As a comparison, no cluster structure is observed for the 1-butanethiol adlayer prepared...... and examined under the same conditions as those for cysteine and cystine. This suggests that intermolecular and intramolecular hydrogen bonds among adsorbed cysteine or cystine molecules could be responsible for the origin of the cluster-network structures for the adlayers. Several models are proposed and used...

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

Science.gov (United States)

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

2018-05-23

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

In situ TEM observation of solid-gas reactions

International Nuclear Information System (INIS)

Kishita, K; Kamino, T; Watabe, A; Kuroda, K; Saka, H

2008-01-01

Under a gaseous atmosphere at high temperatures, almost all the materials (metal, catalysts, etc.) change their structures and properties. For the research and development of materials, it is of vital importance to clarify mechanisms of solid-gas and liquid-gas reactions. Recently an in situ TEM system combined with an environmental holder, which has a gas injection nozzle close to a specimen-heating element, has been developed. The gas injection nozzle permits gas to flow around the specimens sitting on the heating element made of a fine W filament. The newly developed in situ TEM has a differential pumping system; therefore, the pressure in the specimen chamber is maintained in the range of higher than 1 Pa, while the pressure in the electron gun chamber can be kept in the range of 10 -5 Pa. This system was applied to in situ observation of chemical reactions of metals with gases: Observation of oxidation and reduction under a gas pressure ranging from 10 -5 Pa to 1 Pa at high temperatures (room temperature to ∼1473 K) were successfully carried out on pure metal and rare metal catalysts at near-atomic resolution. This in situ environmental TEM system is promising for clarifying mechanisms of many solid-gas and liquid-gas reactions that take place at high temperatures under a gas atmosphere.

Polymer nanocomposites for high-temperature composite repair

Energy Technology Data Exchange (ETDEWEB)

Sheng, Xia [Iowa State Univ., Ames, IA (United States)

2008-01-01

A novel repair agent for resin-injection repair of advanced high temperature composites was developed and characterized. The repair agent was based on bisphenol E cyanate ester (BECy) and reinforced with alumina nanoparticles. To ensure good dispersion and compatibility with the BECy matrix in nanocomposites, the alumina nanoparticles were functionalized with silanes. The BECy nanocomposites, containing bare and functionalized alumina nanoparticles, were prepared and evaluated for their thermal, mechanical, rheological, and viscoelastic properties. The monomer of BECy has an extremely low viscosity at ambient temperature, which is good for processability. The cured BECy polymer is a highly cross-linked network with excellent thermal mechanical properties, with a high glass transition temperature (T_g) of 270 C and decomposition temperature above 350 C. The incorporation of alumina nanoparticles enhances the mechanical and rheological properties of the BECy nanocomposites. Additionally, the alumina nanoparticles are shown to catalyze the cure of BECy. Characterization of the nanocomposites included dynamic mechanical analysis, differential scanning calorimetry, thermogravimetric analysis, rheological and rheokinetic evaluation, and transmission electron microscopy. The experimental results show that the BECy nanocomposite is a good candidate as repair agent for resin-injection repair applications.

In Situ Characterization of Inconel 718 Post-Dynamic Recrystallization within a Scanning Electron Microscope

Directory of Open Access Journals (Sweden)

Meriem Zouari

2017-11-01

Full Text Available Microstructure evolution within the post-dynamic regime following hot deformation was investigated in Inconel 718 samples with different dynamically recrystallized volume fractions and under conditions such that no δ-phase particles were present. In situ annealing treatments carried out to mimic post-dynamic conditions inside the Scanning Electron Microscope (SEM chamber suggest the occurrence of both metadynamic and static recrystallization mechanisms. Static recrystallization was observed in addition to metadynamic recrystallization, only when the initial dynamically recrystallized volume fraction was very small. The initial volume fraction of dynamically recrystallized grains appears to be decisive for subsequent microstructural evolution mechanisms and kinetics. In addition, the formation of annealing twins is observed along with the growth of recrystallized grains, but then the twin density decreases as the material enters the capillarity-driven grain growth regime.

Tritium Removal from JET and TFTR Tiles by a Scanning Laser; TOPICAL

International Nuclear Information System (INIS)

C.H. Skinner; N. Bekris; J.P. Coad; C.A. Gentile; M. Glugla

2002-01-01

Fast and efficient tritium removal is needed for future D-T machines with carbon plasma-facing components. A novel method for tritium release has been demonstrated on co-deposited layers on tiles retrieved from the Tokamak Fusion Test Reactor (TFTR) and from the Joint European Torus (JET). A scanning continuous wave neodymium laser beam was focused to=100 W/mm2 and scanned at high speed over the co-deposits, heating them to temperatures=2000 C for about 10 ms in either air or argon atmospheres. Fiber optic coupling between the laser and scanner was implemented. Up to 87% of the co-deposited tritium was thermally desorbed from the JET and TFTR samples. This technique appears to be a promising in-situ method for tritium removal in a next-step D-T device as it avoids oxidation, the associated de-conditioning of the plasma-facing surfaces, and the expense of processing large quantities of tritium oxide

In Situ Solid-State Reactions Monitored by X-ray Absorption Spectroscopy: Temperature-Induced Proton Transfer Leads to Chemical Shifts.

Science.gov (United States)

Stevens, Joanna S; Walczak, Monika; Jaye, Cherno; Fischer, Daniel A

2016-10-24

The dramatic colour and phase alteration with the solid-state, temperature-dependent reaction between squaric acid and 4,4'-bipyridine has been probed in situ with X-ray absorption spectroscopy. The electronic and chemical sensitivity to the local atomic environment through chemical shifts in the near-edge X-ray absorption fine structure (NEXAFS) revealed proton transfer from the acid to the bipyridine base through the change in nitrogen protonation state in the high-temperature form. Direct detection of proton transfer coupled with structural analysis elucidates the nature of the solid-state process, with intermolecular proton transfer occurring along an acid-base chain followed by a domino effect to the subsequent acid-base chains, leading to the rapid migration along the length of the crystal. NEXAFS thereby conveys the ability to monitor the nature of solid-state chemical reactions in situ, without the need for a priori information or long-range order. © 2016 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

New design of a variable-temperature ultrahigh vacuum scanning tunneling microscope

NARCIS (Netherlands)

Mugele, Friedrich Gunther; Rettenberger, A.; Boneberg, J.; Leiderer, P.

1998-01-01

We present the design of a variable-temperature ultrahigh vacuum (UHV) scanning tunneling microscope which can be operated between 20 and 400 K. The microscope is mounted directly onto the heat exchanger of a He continuous flow cryostat without vibration isolation inside the UHV chamber. The coarse

NCTM of liquids at high temperatures using polarization techniques

Science.gov (United States)

Krishnan, Shankar; Weber, J. K. Richard; Nordine, Paul C.; Schiffman, Robert A.

1990-01-01

Temperature measurement and control is extremely important in any materials processing application. However, conventional techniques for non-contact temperature measurement (mainly optical pyrometry) are very uncertain because of unknown or varying surface emittance. Optical properties like other properties change during processing. A dynamic, in-situ measurement of optical properties including the emittance is required. Intersonics is developing new technologies using polarized laser light scattering to determine surface emittance of freely radiating bodies concurrent with conventional optical pyrometry. These are sufficient to determine the true surface temperature of the target. Intersonics is currently developing a system called DAPP, the Division of Amplitude Polarimetric Pyrometer, that uses polarization information to measure the true thermodynamic temperature of freely radiating objects. This instrument has potential use in materials processing applications in ground and space based equipment. Results of thermophysical and thermodynamic measurements using laser reflection as a temperature measuring tool are presented. The impact of these techniques on thermophysical property measurements at high temperature is discussed.

Eight-fold quantum states blossom in a high-temperature superconductor

CERN Multimedia

2003-01-01

"Researchers based at Lawrence Berkeley National Laboratory and the University of California at Berkeley have used a scanning tunneling microscope (STM) to reveal eight-fold patterns of quasiparticle interference in the high-temperature superconductor Bi-2212 (bismuth strontium calcium copper oxide)" (2 pages).

Evolution of sputtered tungsten coatings at high temperature

Energy Technology Data Exchange (ETDEWEB)

Stelmakh, Veronika; Rinnerbauer, Veronika; Joannopoulos, John D.; Soljačić, Marin; Celanovic, Ivan; Senkevich, Jay J. [Institute for Soldier Nanotechnologies, Massachusetts Institute of Technology, Cambridge, Massachusetts 02139 (United States); Tucker, Charles; Ives, Thomas; Shrader, Ronney [Materion Corporation, Buellton, California 93427 (United States)

2013-11-15

Sputtered tungsten (W) coatings were investigated as potential high temperature nanophotonic material to replace bulk refractory metal substrates. Of particular interest are materials and coatings for thermophotovoltaic high-temperature energy conversion applications. For such applications, high reflectance of the substrate in the infrared wavelength range is critical in order to reduce losses due to waste heat. Therefore, the reflectance of the sputtered W coatings was characterized and compared at different temperatures. In addition, the microstructural evolution of sputtered W coatings (1 and 5 μm thick) was investigated as a function of anneal temperature from room temperature to 1000 °C. Using in situ x-ray diffraction analysis, the microstrain in the two samples was quantified, ranging from 0.33% to 0.18% for the 1 μm sample and 0.26% to 0.20% for the 5 μm sample, decreasing as the temperature increased. The grain growth could not be as clearly quantified due to the dominating presence of microstrain in both samples but was in the order of 20 to 80 nm for the 1 μm sample and 50 to 100 nm for the 5 μm sample, as deposited. Finally, the 5 μm thick layer was found to be rougher than the 1 μm thick layer, with a lower reflectance at all wavelengths. However, after annealing the 5 μm sample at 900 °C for 1 h, its reflectance exceeded that of the 1 μm sample and approached that of bulk W found in literature. Overall, the results of this study suggest that thick coatings are a promising alternative to bulk substrates as a low cost, easily integrated platform for nanostructured devices for high-temperature applications, if the problem of delamination at high temperature can be overcome.

Rapid Separation of Copper Phase and Iron-Rich Phase From Copper Slag at Low Temperature in a Super-Gravity Field

Science.gov (United States)

Lan, Xi; Gao, Jintao; Huang, Zili; Guo, Zhancheng

2018-06-01

A novel approach for quickly separating a metal copper phase and iron-rich phase from copper slag at low temperature is proposed based on a super-gravity method. The morphology and mineral evolution of the copper slag with increasing temperature were studied using in situ high-temperature confocal laser scanning microscopy and ex situ scanning electron microscopy and X-ray diffraction methods. Fe3O4 particles dispersed among the copper slag were transformed into FeO by adding an appropriate amount of carbon as a reducing agent, forming the slag melt with SiO2 at low temperature and assisting separation of the copper phase from the slag. Consequently, in a super-gravity field, the metallic copper and copper matte were concentrated as the copper phase along the super-gravity direction, whereas the iron-rich slag migrated in the opposite direction and was quickly separated from the copper phase. Increasing the gravity coefficient (G) significantly enhanced the separation efficiency. After super-gravity separation at G = 1000 and 1473 K (1200 °C) for 3 minutes, the mass fraction of Cu in the separated copper phase reached 86.11 wt pct, while that in the separated iron-rich phase was reduced to 0.105 wt pct. The recovery ratio of Cu in the copper phase was as high as up to 97.47 pct.

In situ observation of the role of alumina particles on the crystallization behavior of slags

Energy Technology Data Exchange (ETDEWEB)

Orrling, C.

2000-09-01

The confocal laser scanning microscope (CLSM) allows crystallization behavior in liquid slags to he observed in situ at high temperatures. Slags in the lime-silica-alumina-magnesia system are easily tinder cooled and it is possible to construct time temperature transformation (TTT) diagrams for this system. The presence of solid alumina particles its these liquid slags was studied to determine if these particles act as heterogeneous nucleation sites that cause she precipitation of solid material within slags. The introduction of alumina particles reduced the incubation time for the onset of crystallization and increased the temperature at which crystallization was observed in the slags to close to the liquidus temperature for the slag. Crystal growth rates are in a good agreement with Ivantsov's solution of the problem of diffusion controlled dendritic growth. Alumina appears to be a potent nucleating agent in the slag systems that were studied. (author)

In-situ fabrication of MoSi{sub 2}/SiC–Mo{sub 2}C gradient anti-oxidation coating on Mo substrate and the crucial effect of Mo{sub 2}C barrier layer at high temperature

Energy Technology Data Exchange (ETDEWEB)

Liu, Jun [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Key Laboratory for Advanced Materials Processing Technology, Ministry of Education, Beijing 100084 (China); State Key Laboratory of New Ceramics and Fine Processing, Beijing 100084 (China); Gong, Qianming, E-mail: gongqianming@mail.tsinghua.edu.cn [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Key Laboratory for Advanced Materials Processing Technology, Ministry of Education, Beijing 100084 (China); State Key Laboratory of New Ceramics and Fine Processing, Beijing 100084 (China); Shao, Yang; Zhuang, Daming [School of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Key Laboratory for Advanced Materials Processing Technology, Ministry of Education, Beijing 100084 (China); State Key Laboratory of New Ceramics and Fine Processing, Beijing 100084 (China); Liang, Ji [Key Laboratory for Advanced Materials Processing Technology, Ministry of Education, Beijing 100084 (China); Department of Mechanical Engineering, Tsinghua University, Beijing 100084 (China)

2014-07-01

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

Atomic species recognition on oxide surfaces using low temperature scanning probe microscopy

Energy Technology Data Exchange (ETDEWEB)

Ma, Zong Min, E-mail: mzmncit@163.com [National Key Laboratory for Electronic Measurement Technology, North University of China, Taiyuan, 030051 (China); Key Laboratory of Instrumentation Science & Dynamic Measurement, North University of China, Ministry of Education, Taiyuan, 030051 (China); School of Instrument and Electronics, North University of China, Taiyuan, 030051 (China); Shi, Yun Bo; Mu, Ji Liang; Qu, Zhang; Zhang, Xiao Ming; Qin, Li [National Key Laboratory for Electronic Measurement Technology, North University of China, Taiyuan, 030051 (China); Key Laboratory of Instrumentation Science & Dynamic Measurement, North University of China, Ministry of Education, Taiyuan, 030051 (China); School of Instrument and Electronics, North University of China, Taiyuan, 030051 (China); Liu, Jun, E-mail: liuj@nuc.edu.cn [National Key Laboratory for Electronic Measurement Technology, North University of China, Taiyuan, 030051 (China); Key Laboratory of Instrumentation Science & Dynamic Measurement, North University of China, Ministry of Education, Taiyuan, 030051 (China); School of Instrument and Electronics, North University of China, Taiyuan, 030051 (China)

2017-02-01

Highlights: • The coexisted phase of p(2 × 1)and c(6 × 2) on Cu(110)-O surface using AFM under UHV at low temperature. • Two different c(6 × 2) phase depending on the status of the tip apex. • Electronic state of tip seriously effect the resolution and stability of the sample surface. - Abstract: In scanning probe microscopy (SPM), the chemical properties and sharpness of the tips of the cantilever greatly influence the scanning of a sample surface. Variation in the chemical properties of the sharp tip apex can induce transformation of the SPM images. In this research, we explore the relationship between the tip and the structure of a sample surface using dynamic atomic force microscopy (AFM) on a Cu(110)-O surface under ultra-high vacuum (UHV) at low temperature (78 K). We observed two different c(6 × 2) phase types in which super-Cu atoms show as a bright spot when the tip apex is of O atoms and O atoms show as a bright spot when the tip apex is of Cu atoms. We also found that the electronic state of the tip has a serious effect on the resolution and stability of the sample surface, and provide an explanation for these phenomena. This technique can be used to identify atom species on sample surfaces, and represents an important development in the SPM technique.

The refrigeration of high temperature superconductors between 25K and 65K

International Nuclear Information System (INIS)

Richardson, R.N.; Scurlock, R.G.; Tavner, A.C.R.

1996-01-01

The present state of the art indicates that acceptable j - H characteristics for power applications of the new high Tc superconductors will only be achieved using materials at temperatures below liquid nitrogen temperature. A boiling point of 27.1K and high specific cooling capacity make neon an eminently suitable choice of refrigerant at these temperatures. A cryostat has been constructed which employs a two stage Gifford-McMahon cooler to liquefy neon gas. The cryostat contains up to 5 litres of liquid neon which can be used for open-quote in-situ close-quote experiments or transfer to another cryostat. Another set of cryostats are being used with liquid nitrogen/oxygen mixtures at reduced pressure for temperatures down to 50K. All these cryostats provide a core facility for characterising and operating high T c superconductors at Southampton

Sea surface temperature measurements by the along-track scanning radiometer on the ERS 1 satellite: Early results

Science.gov (United States)

Mutlow, C. T.; ZáVody, A. M.; Barton, I. J.; Llewellyn-Jones, D. T.

1994-11-01

The along-track scanning radiometer (ATSR) was launched in July 1991 on the European Space Agency's first remote sensing satellite, ERS 1. An initial analysis of ATSR data demonstrates that the sea surface temperature (SST) can be measured from space with very high accuracy. Comparison of simultaneous measurements of SST made from ATSR and from a ship-borne radiometer show that they agree to within 0.3°C. To assess data consistency, a complementary analysis of SST data from ATSR was also carried out. The ATSR global SST field was compared on a daily basis with daily SST analysis of the United Kingdom Meteorological Office (UKMO). The ATSR global field is consistently within 1.0°C of the UKMO analysis. Also, to demonstrate the benefits of along-track scanning SST determination, the ATSR SST data were compared with high-quality bulk temperature observations from drifting buoys. The likely causes of the differences between ATSR and the bulk temperature data are briefly discussed. These results provide early confidence in the quantitative benefit of ATSR's two-angle view of the Earth and its high radiometric performance and show a significant advance on the data obtained from other spaceborne sensors. It should be noted that these measurements were made at a time when the atmosphere was severely contaminated with volcanic aerosol particles, which degrade infrared measurements of the Earth's surface made from space.

In situ XRD study of C60 polymerisation above pressures of 9 GPa and temperatures up to 830K

International Nuclear Information System (INIS)

Talyzin, A.V.; Jansson, U.; Dubrovinsky, L.S.; Oden, M.; Le Bihan, T.

2002-01-01

The C60 polymerization was studied by X-ray diffraction in situ in the pressure range 13-18 GPa and at temperatures up to 830 K. The results of the high pressure high temperature treatment are strongly dependent from the history of the sample and stress. At certain conditions no elliptical diffraction patterns were observed at 13 GPa and 830K. Samples with a relatively low internal stress showed a transformation to new phase. It is suggested that this phase is three-dimensional polymer with each C60 molecule bonded to eight neighbors. This phase showed an increased hardness (about 37 GPa) and a Raman spectrum distinctly different from previously known polymeric phases

In situ observation · analytical technologies of high temperature superconductor for fusion reactor at ultra low temperature

International Nuclear Information System (INIS)

Kimoto, Takayoshi; Sun, Wei; Fukutomi, Katsuo; Togano, Kazumasa; Saito, Tetsuya; Hiraga, Kenji; Takeda, Toshiyuki

1998-01-01

An image installation program of SPARK station 20 was accomplished. It can induce continuously 2.1 MB TEM image at 5 sheet/sec until 160 sheets. An image processing (shift addition) program was developed at first in the world. The program can overlap many sheet of TEM images by shifting them to the correct position. Other image processing programs such as flatfielding and reducing noise processing were developed. High temperature lattice fringe image of superconductive oxide Bi2223 in the drift chamber can be observed at low temperature by using the above image processing programs. New type laser device for filament radiation which consists of argon ion laser was developed as the first step of development of high brightness electron gun. Bi2212 single crystal was determined by the large angle convergent beam electron diffraction. The results showed the crystal structure belonged to Bbmb. (S.Y.)

In Situ Study of Live Specimens in an Environmental Scanning Electron Microscope

Czech Academy of Sciences Publication Activity Database

Tihlaříková, Eva; Neděla, Vilém; Shiojiri, M.

2013-01-01

Roč. 19, č. 4 (2013), s. 914-918 ISSN 1431-9276 R&D Projects: GA ČR GAP102/10/1410 Institutional support: RVO:68081731 Keywords : live biological sample * high-pressure environment * hydration system * in situ observation * Monte Carlo simulation * methodology Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 1.757, year: 2013

Mechanochemical preparation of nanocrystalline TiO2 powders and their behavior at high temperatures

International Nuclear Information System (INIS)

Gajovic, A.; Furic, K.; Tomasic, N.; Popovic, S.; Skoko, Z.; Music, S.

2005-01-01

Nanocrystalline TiO 2 powders were prepared by high-energy ball-milling using zirconia vial and balls. The changes of microstructure caused by material processing were studied using Raman spectroscopy, X-ray powder diffraction (XRD), transmission electron microscopy (TEM) and selected area electron diffraction (SAED). The milling of the starting TiO 2 powder (anatase + rutile in traces) induced phase transitions to high-pressure polymorph, TiO 2 II, and rutile. We found that the phase transition to TiO 2 II was initiated at the surface of the small particles, while transition to rutile started in their center. Changes in crystallite size during milling process were obtained by the Scherrer method, while the particle size changes were monitored by TEM. The kinetics of phase changes, a decrease in crystallite/particle size, as well as zirconia contamination depended on the powder-to-ball weight ratio. The starting powder and some selected ball-milled samples were investigated in situ by Raman spectroscopy and XRD at high temperatures (up to 1300 deg. C) to examine their behavior during the sintering process. A difference in the results obtained by these two techniques was explained in frame of basic physical properties characterizing both methods. The morphology of the final sinters was monitored by scanning electron microscopy (SEM)

Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

International Nuclear Information System (INIS)

Bindi, Luca

2009-01-01

The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: α a = 1.5 x 10 -5 K -1 , α b = 3.0 x 10 -5 K -1 , α c = 2.2 x 10 -5 K -1 , and the bulk thermal expansion coefficient α V is 5.4 x 10 -5 K -1 for the temperature range 298-463 K

Experimental study of carbon materials behavior under high temperature and VUV radiation: Application to Solar Probe+ heat shield

International Nuclear Information System (INIS)

Eck, J.; Sans, J.-L.; Balat-Pichelin, M.

2011-01-01

The aim of the Solar Probe Plus (SP+) mission is to understand how the solar corona is heated and how the solar wind is accelerated. To achieve these goals, in situ measurements are necessary and the spacecraft has to approach the Sun as close as 9.5 solar radii. This trajectory induces extreme environmental conditions such as high temperatures and intense Vacuum Ultraviolet radiation (VUV). To protect the measurement and communication instruments, a heat shield constituted of a carbon material is placed on the top of the probe. In this study, the physical and chemical behavior of carbon materials is experimentally investigated under high temperatures (1600-2100 K), high vacuum (10 -4 Pa) and VUV radiation in conditions near those at perihelion for SP+. Thanks to several in situ and ex situ characterizations, it was found that VUV radiation induced modification of outgassing and of mass loss rate together with alteration of microstructure and morphology.

In-situ transmission electron microscopy study of ion-irradiated copper : comparison of the temperature dependence of cascade collapse in FCC- and BCC- metals.

Energy Technology Data Exchange (ETDEWEB)

Daulton, T. L.

1998-10-23

The kinetics which drive cascade formation and subsequent collapse into point-defect clusters is investigated by analyzing the microstructure produced in situ by low fluence 100 keV Kr ion irradiations of fcc-Cu over a wide temperature range (18-873 K). The yield of collapsed point-defect clusters is demonstrated unequivocally to be temperature dependent, remaining approximately constant up to lattice temperatures of 573 K and then abruptly decreasing with increasing temperature. This drop in yield is not caused by defect loss during or following ion irradiation. This temperature dependence can be explained by a thermal spike effect. These in-situ yield measurements are compared to previous ex-situ yield measurements in fcc-Ni and bcc-Mo.

Scanning transmission X-ray microscopy probe for in situ mechanism study of graphene-oxide-based resistive random access memory.

Science.gov (United States)

Nho, Hyun Woo; Kim, Jong Yun; Wang, Jian; Shin, Hyun-Joon; Choi, Sung-Yool; Yoon, Tae Hyun

2014-01-01

Here, an in situ probe for scanning transmission X-ray microscopy (STXM) has been developed and applied to the study of the bipolar resistive switching (BRS) mechanism in an Al/graphene oxide (GO)/Al resistive random access memory (RRAM) device. To perform in situ STXM studies at the C K- and O K-edges, both the RRAM junctions and the I0 junction were fabricated on a single Si3N4 membrane to obtain local XANES spectra at these absorption edges with more delicate I0 normalization. Using this probe combined with the synchrotron-based STXM technique, it was possible to observe unique chemical changes involved in the BRS process of the Al/GO/Al RRAM device. Reversible oxidation and reduction of GO induced by the externally applied bias voltages were observed at the O K-edge XANES feature located at 538.2 eV, which strongly supported the oxygen ion drift model that was recently proposed from ex situ transmission electron microscope studies.

In situ high-resolution transmission electron microscopy synthesis observation of nanostructured carbon coated LiFePO 4

Science.gov (United States)

Trudeau, M. L.; Laul, D.; Veillette, R.; Serventi, A. M.; Mauger, A.; Julien, C. M.; Zaghib, K.

In situ high-resolution transmission electron microscopy (HRTEM) studies of the structural transformations that occur during the synthesis of carbon-coated LiFePO 4 (C-LiFePO 4) and heat treatment to elevated temperatures were conducted in two different electron microscopes. Both microscopes have sample holders that are capable of heating up to 1500 °C, with one working under high vacuum and the other capable of operating with the sample surrounded by a low gaseous environment. The C-LiFePO 4 samples were prepared using three different compositions of precursor materials with Fe(0), Fe(II) or Fe(III), a Li-containing salt and a polyethylene- block-poly(ethylene glycol)-50% ethylene oxide or lactose. The in situ TEM studies suggest that low-cost Fe(0) and a low-cost carbon-containing compound such as lactose are very attractive precursors for mass production of C-LiFePO 4, and that 700 °C is the optimum synthesis temperature. At temperatures higher than 800 °C, LiFePO 4 has a tendency to decompose. The same in situ measurements have been made on particles without carbon coat. The results show that the homogeneous deposit of the carbon deposit at 700 °C is the result of the annealing that cures the disorder of the surface layer of bare LiFePO 4. Electrochemical tests supported the conclusion that the C-LiFePO 4 derived from Fe(0) is the most attractive for mass production.

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

International Nuclear Information System (INIS)

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

2017-01-01

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

Testing of Sapphire Optical Fiber and Sensors in Intense Radiation Fields When Subjected to Very High Temperatures

Energy Technology Data Exchange (ETDEWEB)

Blue, Thomas [The Ohio State Univ., Columbus, OH (United States); Windl, Wolfgang [The Ohio State Univ., Columbus, OH (United States)

2017-12-15

The primary objective of this project was to determine the optical attenuation and signal degradation of sapphire optical fibers & sensors (temperature & strain), in-situ, operating at temperatures up to 1500°C during reactor irradiation through experiments and modeling. The results will determine the feasibility of extending sapphire optical fiber-based instrumentation to extremely high temperature radiation environments. This research will pave the way for future testing of sapphire optical fibers and fiber-based sensors under conditions expected in advanced high temperature reactors.

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

Science.gov (United States)

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.

In-situ monitoring of etching of bovine serum albumin using low-temperature atmospheric plasma jet

Science.gov (United States)

Kousal, J.; Shelemin, A.; Kylián, O.; Slavínská, D.; Biederman, H.

2017-01-01

Bio-decontamination of surfaces by means of atmospheric pressure plasma is nowadays extensively studied as it represents promising alternative to commonly used sterilization/decontamination techniques. The non-equilibrium atmospheric pressure plasmas were already reported to be highly effective in removal of a wide range of biological residual from surfaces. Nevertheless the kinetics of removal of biological contamination from surfaces is still not well understood as the majority of performed studies were based on ex-situ evaluation of etching rates, which did not allow investigating details of plasma action on biomolecules. This study therefore presents a real-time, in-situ ellipsometric characterization of removal of bovine serum albumin (BSA) from surfaces by low-temperature atmospheric plasma jet operated in argon. Non-linear and at shorter distances between treated samples and nozzle of the plasma jet also non-monotonic dependence of the removal rate on the treatment duration was observed. According to additional measurements focused on the determination of chemical changes of treated BSA as well as temperature measurements, the observed behavior is most likely connected with two opposing effects: the formation of a thin layer on the top of BSA deposit enriched in inorganic compounds, whose presence causes a gradual decrease of removal efficiency, and slight heating of BSA that facilitates its degradation and volatilization induced by chemically active radicals produced by the plasma.

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

Energy Technology Data Exchange (ETDEWEB)

Bisson, R., E-mail: regis.bisson@univ-amu.fr [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France); Markelj, S. [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France); Jožef Stefan Institute, Jamova cesta 39, 1000 Ljubljana (Slovenia); Mourey, O.; Ghiorghiu, F. [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France); Achkasov, K. [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France); CEA, IRFM, F-13108 Saint-Paul-lez-Durance (France); Layet, J.-M.; Roubin, P.; Cartry, G. [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France); Grisolia, C. [CEA, IRFM, F-13108 Saint-Paul-lez-Durance (France); Angot, T. [Aix Marseille Université, CNRS, PIIM UMR 7345, 13397 Marseille (France)

2015-12-15

Retention of deuterium ion implanted in polycrystalline tungsten samples is studied in situ in an ultra-high vacuum apparatus equipped with a low-flux ion source and a high sensitivity thermo-desorption setup. Retention as a function of ion fluence was measured in the 10{sup 17}–10{sup 21} D{sup +}·m{sup −2} range. By combining this new fluence range with the literature in situ experimental data, we evidence the existence of a retention ∝ fluence{sup 0.645±0.025} relationship which describes deuterium retention behavior on polycrystalline tungsten on 8 orders of magnitude of fluence. Evolution of deuterium retention as a function of the sample storage time in vacuum at room temperature was followed. A loss of 50% of the retained deuterium is observed when the storage time is increased from 2 h to 135 h. The role of the surface and of natural bulk defects on the deuterium retention/release in polycrystalline tungsten is discussed in light of the behavior of the single desorption peak obtained with Temperature Programmed Desorption.

High temperature dielectric function of silicon, germanium and GaN

Energy Technology Data Exchange (ETDEWEB)

Leyer, Martin; Pristovsek, Markus; Kneissl, Michael [Technische Universitaet Berlin (Germany). Institut fuer Festkoerperphysik

2010-07-01

In the last few years accurate values for the optical properties of silicon, germanium and GaN at high temperatures have become important as a reference for in-situ analysis, e.g. reflectometry. Precise temperature dependent dielectric measurements are necessary for the growth of GaInP/GaInAs/Ge triple-junction solar cells and the hetero epitaxy of GaN on silicon and sapphire. We performed spectroscopic ellipsometry (SE) measurements of the dielectric function of silicon, germanium and GaN between 1.5 eV and 6.5 eV in the temperature range from 300 K to 1300 K. The Samples were deoxidized chemically or by heating. High resolution SE spectra were taken every 50 K while cooling down to room temperature. The temperature dependence of the critical energies is compared to literature. Measurements for germanium showed a shift of the E{sub 2} critical point of {proportional_to}0.1 eV toward lower energies. The reason for this behavior is a non-negligible oxide layer on the samples in the literature.

Surface monitoring for pitting evolution into uniform corrosion on Cu-Ni-Zn ternary alloy in alkaline chloride solution: ex-situ LCM and in-situ SECM

Science.gov (United States)

Kong, Decheng; Dong, Chaofang; Zheng, Zhaoran; Mao, Feixiong; Xu, Aoni; Ni, Xiaoqing; Man, Cheng; Yao, Jizheng; Xiao, Kui; Li, Xiaogang

2018-05-01

The evolution of the corrosion process on Cu-Ni-Zn alloy in alkaline chloride solution was investigated by in-situ scanning electrochemical microscopy, X-ray photoelectron spectroscopy, and ex-situ laser confocal microscopy, and the effects of ambient temperature and polarization time were also discussed. The results demonstrated a higher pitting nucleation rate and lower pit growth rate at low temperature. The ratio of pit depth to mouth diameter decreased with increasing pit volume and temperature, indicating that pits preferentially propagate in the horizontal direction rather than the vertical direction owing to the presence of corrosion products and deposited copper. The surface current was uniform and stabilized at approximately 2.2 nA during the passive stage, whereas the current increased after the pits were formed with the maximum approaching 3 nA. Increasing the temperature led to an increase in porous corrosion products (CuO, Zn(OH)2, and Ni(OH)2) and significantly increased the rate of transition from pitting to uniform corrosion. Dezincification corrosion was detected by energy dispersive spectrometry, and a mechanism for pitting transition into uniform corrosion induced by dezincification at the grain boundaries is proposed.

A 350 mK, 9 T scanning tunneling microscope for the study of superconducting thin films on insulating substrates and single crystals.

Science.gov (United States)

Kamlapure, Anand; Saraswat, Garima; Ganguli, Somesh Chandra; Bagwe, Vivas; Raychaudhuri, Pratap; Pai, Subash P

2013-12-01

We report the construction and performance of a low temperature, high field scanning tunneling microscope (STM) operating down to 350 mK and in magnetic fields up to 9 T, with thin film deposition and in situ single crystal cleaving capabilities. The main focus lies on the simple design of STM head and a sample holder design that allows us to get spectroscopic data on superconducting thin films grown in situ on insulating substrates. Other design details on sample transport, sample preparation chamber, and vibration isolation schemes are also described. We demonstrate the capability of our instrument through the atomic resolution imaging and spectroscopy on NbSe2 single crystal and spectroscopic maps obtained on homogeneously disordered NbN thin film.

In-situ temperature calibration below 1 K using the μ+ Knight shift in CMN

International Nuclear Information System (INIS)

Heffner, R.H.; Le, L.P.; Amato, A.; Baines, C.

1996-01-01

The authors present μ + paramagnetic shift measurements between 12 K and about 65 mK in cerium magnesium nitrate (CMN) to investigate its utility as an in-situ temperature calibration source for low temperature μSR experiments. CMN is a salt which exhibits Curie-law susceptibility to temperatures as low as 5 mK. The μ + Knight shift is measured to be (1.46 ± 0.03) x 10 -3 /T + (0.004 ± 0.02) x 10 -3 , corresponding to a transferred hyperfine field of -28.5 kOe/μ B

Processing of Graphene combining Optical Detection and Scanning Probe Lithography

Directory of Open Access Journals (Sweden)

Zimmermann Sören

2015-01-01

Full Text Available This paper presents an experimental setup tailored for robotic processing of graphene with in-situ vision based control. A robust graphene detection approach is presented applying multiple image processing operations of the visual feedback provided by a high-resolution light microscope. Detected graphene flakes can be modified using a scanning probe based lithographical process that is directly linked to the in-situ optical images. The results of this process are discussed with respect to further application scenarios.

Atomized scan strategy for high definition for VR application

Science.gov (United States)

Huang, Shuping; Ran, Feng; Ji, Yuan; Chen, Wendong

2017-10-01

Silicon-based OLED (Organic Light Emitting Display) microdisplay technology begins to attract people's attention in the emerging VR and AR devices. The high display frame refresh rate is an important solution to alleviate the dizziness in VR applications. Traditional display circuit drivers use the analog method or the digital PWM method that follow the serial scan order from the first pixel to the last pixel by using the shift registers. This paper proposes a novel atomized scan strategy based on the digital fractal scan strategy using the pseudo-random scan order. It can be used to realize the high frame refresh rate with the moderate pixel clock frequency in the high definition OLED microdisplay. The linearity of the gray level is also improved compared with the Z fractal scan strategy.

A 30 mK, 13.5 T scanning tunneling microscope with two independent tips

Energy Technology Data Exchange (ETDEWEB)

Roychowdhury, Anita [Laboratory for Physical Sciences, College Park, Maryland 20742 (United States); Center for Nanophysics and Advanced Materials, Department of Physics, University of Maryland, College Park, Maryland 20740 (United States); Gubrud, M. A.; Dana, R.; Dreyer, M. [Laboratory for Physical Sciences, College Park, Maryland 20742 (United States); Anderson, J. R.; Lobb, C. J.; Wellstood, F. C. [Center for Nanophysics and Advanced Materials, Department of Physics, University of Maryland, College Park, Maryland 20740 (United States)

2014-04-15

We describe the design, construction, and performance of an ultra-low temperature, high-field scanning tunneling microscope (STM) with two independent tips. The STM is mounted on a dilution refrigerator and operates at a base temperature of 30 mK with magnetic fields of up to 13.5 T. We focus on the design of the two-tip STM head, as well as the sample transfer mechanism, which allows in situ transfer from an ultra high vacuum preparation chamber while the STM is at 1.5 K. Other design details such as the vibration isolation and rf-filtered wiring are also described. Their effectiveness is demonstrated via spectral current noise characteristics and the root mean square roughness of atomic resolution images. The high-field capability is shown by the magnetic field dependence of the superconducting gap of Cu{sub x}Bi{sub 2}Se{sub 3}. Finally, we present images and spectroscopy taken with superconducting Nb tips with the refrigerator at 35 mK that indicate that the effective temperature of our tips/sample is approximately 184 mK, corresponding to an energy resolution of 16 μeV.

A 30 mK, 13.5 T scanning tunneling microscope with two independent tips.

Science.gov (United States)

Roychowdhury, Anita; Gubrud, M A; Dana, R; Anderson, J R; Lobb, C J; Wellstood, F C; Dreyer, M

2014-04-01

We describe the design, construction, and performance of an ultra-low temperature, high-field scanning tunneling microscope (STM) with two independent tips. The STM is mounted on a dilution refrigerator and operates at a base temperature of 30 mK with magnetic fields of up to 13.5 T. We focus on the design of the two-tip STM head, as well as the sample transfer mechanism, which allows in situ transfer from an ultra high vacuum preparation chamber while the STM is at 1.5 K. Other design details such as the vibration isolation and rf-filtered wiring are also described. Their effectiveness is demonstrated via spectral current noise characteristics and the root mean square roughness of atomic resolution images. The high-field capability is shown by the magnetic field dependence of the superconducting gap of CuxBi2Se3. Finally, we present images and spectroscopy taken with superconducting Nb tips with the refrigerator at 35 mK that indicate that the effective temperature of our tips/sample is approximately 184 mK, corresponding to an energy resolution of 16 μeV.

In situ study at high pressure and temperature of the environment of water in hydrous Na and Ca aluminosilicate melts and coexisting aqueous fluids

Science.gov (United States)

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

2017-07-01

The bonding and speciation of water dissolved in Na silicate and Na and Ca aluminosilicate melts were inferred from in situ Raman spectroscopy of the samples, in hydrothermal diamond anvil cells, while at crustal temperature and pressure conditions. Raman data were also acquired on Na silicate and Na and Ca aluminosilicate glasses, quenched from hydrous melts equilibrated at high temperature and pressure in a piston cylinder apparatus. In the hydrous melts, temperature strongly influences O-H stretching ν(O-H) signals, reflecting its control on the bonding of protons between different molecular complexes. Pressure and melt composition effects are much smaller and difficult to discriminate with the present data. However, the chemical composition of the melt + fluid system influences the differences between the ν(O-H) signals from the melts and the fluids and, hence, between their hydrogen partition functions. Quenching modifies the O-H stretching signals: strong hydrogen bonds form in the glasses below the glass transition temperature Tg, and this phenomenon depends on glass composition. Therefore, glasses do not necessarily record the O-H stretching signal shape in melts near Tg. The melt hydrogen partition function thus cannot be assessed with certainty using O-H stretching vibration data from glasses. From the present results, the ratio of the hydrogen partition functions of hydrous silicate melts and aqueous fluids mostly depends on temperature and the bulk melt + fluid system chemical composition. This implies that the fractionation of hydrogen isotopes between magmas and aqueous fluids in water-saturated magmatic systems with differences in temperature and bulk chemical composition will be different.

In situ transmission electron microscopy study of ion-irradiated copper: comparison of the temperature dependence of cascade collapse in fcc- and bcc-metals

International Nuclear Information System (INIS)

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

2000-01-01

The kinetics which drive cascade formation and subsequent collapse into point-defect clusters are investigated by analyzing the microstructure produced in situ by low fluence 100 keV Kr ion irradiations of fcc-Cu over a wide temperature range (18-873 K). The yield of collapsed point-defect clusters is demonstrated unequivocally to be temperature dependent, remaining approximately constant up to lattice temperatures of 573 K and then abruptly decreasing with increasing temperature. This drop in yield is not caused by defect loss during or following ion irradiation. In addition, this temperature dependence can be explained by a thermal spike effect. These in situ yield measurements are compared to previous ex situ yield measurements in fcc-Ni and bcc-Mo

Thermal expansion behavior of empressite, AgTe: A structural study by means of in situ high-temperature single-crystal X-ray diffraction

Energy Technology Data Exchange (ETDEWEB)

Bindi, Luca [Museo di Storia Naturale, sez. di Mineralogia, Universita di Firenze, Via La Pira 4, I-50121 Firenze (Italy)], E-mail: luca.bindi@unifi.it

2009-04-03

The crystal structure of empressite, AgTe, a rare silver telluride, has been investigated by in situ X-ray single-crystal diffraction methods within the temperature range 298-463 K. AgTe remains orthorhombic, space group Pmnb (Pnma as standard), and shows only normal thermal expansion over the entire temperature range. The unit-cell parameters show a gradual increase with the increase of temperature. Slight adjustments in the geometry of Ag-tetrahedra and in the crystal-chemical environment of tellurium atoms occur in a continuous way without abrupt structural changes. The coefficients of thermal expansion along various axes are: {alpha}{sub a} = 1.5 x 10{sup -5} K{sup -1}, {alpha}{sub b} = 3.0 x 10{sup -5} K{sup -1}, {alpha}{sub c} = 2.2 x 10{sup -5} K{sup -1}, and the bulk thermal expansion coefficient {alpha}{sub V} is 5.4 x 10{sup -5} K{sup -1} for the temperature range 298-463 K.

Novel Quantification of Sediment Concentration in Turbidity Currents Through in-situ Measurements of Conductivity and Temperature

Science.gov (United States)

Xu, J.; Wang, Z.; Gwiazda, R.; Paull, C. K.; Talling, P.; Parsons, D. R.; Maier, K. L.; Simmons, S.; Cartigny, M.

2017-12-01

During a large turbidity current event observed by seven moorings placed along Monterey Canyon, offshore central California, in the axial channel between 300 and 1900 meters water depth, a conductivity/temperature sensor placed 11 meters above canyon floor on the mooring at 1500 meters water depth recorded a rapid decrease of conductivity and increase of temperature during the passage of a large turbidity current. The conductivity decline is unlikely caused by fresh water input owing to lack of precipitation in the region prior to the event. We investigated the mechanisms of turbidity currents' high sediment concentration reducing the measured conductivity. By conducting a series of laboratory experiments with a range of different concentrations, grain size, and water temperature combinations, we quantified a relationship between reduced conductivity and the elevated sediment concentration. This relationship can be used for estimating the very high sediment concentrations in a turbidity current with a condition of assuming constant salinity of the ambient seawater. The empirical relationship was then applied to the in-situ time-series of temperature and conductivity measured during this turbidity current. The highest sediment concentration, in the head of the flow, reached nearly 400 g/L (volume concentration 17%). Such a high value, which has yet been reported in literature for an oceanic turbidity current, will have significant implications for the dynamics and deposits of such flows.

Evaluating the Properties of High-Temperature and Low-Temperature Wear of TiN Coatings Deposited at Different Temperatures

Directory of Open Access Journals (Sweden)

B. Khorrami Mokhori

2017-02-01

Full Text Available In this research titanium nitride (TiN films were prepared by plasma assisted chemical vapor deposition using TiCl4, H2, N2 and Ar on the AISI H13 tool steel. Coatings were deposited during different substrate temperatures (460°C, 480 ° C  and 510 °C. Wear tests were performed in order to study the acting wear mechanisms in the high(400 °C and low (25 °C temperatures by ball on disc method. Coating structure and chemical composition were characterized using scanning electron microscopy, microhardness and X-ray diffraction. Wear test result was described in ambient temprature according to wear rate. It was evidenced that the TiN coating deposited at 460 °C has the least weight loss with the highest hardness value. The best wear resistance was related to the coating with the highest hardness (1800 Vickers. Wear mechanisms were observed to change by changing wear temperatures. The result of wear track indicated that low-temprature wear has surface fatigue but high-temperature wear showed adhesive mechanism.

i-anvils : in situ measurements of pressure, temperature and conductivity in diamond anvil cells

Science.gov (United States)

Munsch, P.; Bureau, H.; Kubsky, S.; Meijer, J.; Datchi, F.; Ninet, S.; Estève, I.

2011-12-01

The precise determination of the pressure and temperature conditions during diamond anvils cells (DAC) experiments is of primary importance. Such determinations are critical more especially for the fields corresponding to "low pressures" (micro-structures are implanted in the diamond anvil lattice a few micrometers below the surface, the sensors are located a few μm below the center of the diamond culet (sample chamber position). When conductive electrodes are implanted at the position of the sample chamber on the culet of the anvil, instead of P,T sensors, they allow in situ measurements of electrical properties of the loaded sample at high P,T conditions in a DAC. The principle consists of applying an electrical potential across the structures through external contacts placed on the slopes of the anvil. The resistivity of these structures is sensitive to pressure and temperature applied in the sample chamber. The electrical transport properties of the sample can be measured the same way when electrodes have been implanted on the culet. Here we will present our last progresses, more especially using the focus ion beam (FIB) technology to perform contacts and electrodes. Progresses about the i-anvils connexions with the electronic devices will also be shown. We will present the last P and T sensors calibrations. Furnaces are also introduced through Boron implantation into the anvils, allowing the possibility to reach intermediate temperatures between externally heated DAC (up to 1100°C) and laser heated DAC (from 1500°C to a few thousands). Preliminary tests and the interest of such devices will be discussed at the meeting. A new diamond anvil cell has been especially designed for this purpose. This DAC allows in situ spectroscopies and X-Ray characterisation of geological fluids in their equilibrium conditions in the crust and in the upper mantle. Preliminary results will be presented.

Practical ultrasonic transducers for high-temperature applications using bismuth titanate and Ceramabind 830

Science.gov (United States)

Xu, Janet L.; Batista, Caio F. G.; Tittmann, Bernhard R.

2018-04-01

Structural health monitoring of large valve bodies in high-temperature environments such as power plants faces several limitations: commercial transducers are not rated for such high temperatures, gel couplants will evaporate, and measurements cannot be made in-situ. To solve this, we have furthered the work of Ledford in applying a practical transducer in liquid form which hardens and air dries directly onto the substrate. The transducer material is a piezoceramic film composed of bismuth titanate and a high-temperature binding agent, Ceramabind 830. The effects of several fabrication conditions were studied to optimize transducer performance and ensure repeatability. These fabrication conditions include humidity, binder ratio, water ratio, substrate roughness, and film thickness. The final product is stable for both reactive and non-reactive substrates, has a quick fabrication time, and has an operating temperature up to the Curie temperature of BIT, 650°C, well beyond the safe operating temperature of PZT (150°C).

Development of a PIGE-Detection System for in-situ Inspection and Quality Assurance in the Evolution of Fast Rotating Parts in High Temperature Environment Manufactured from TiAl

Directory of Open Access Journals (Sweden)

S. Neve

2013-04-01

Full Text Available Intermetallic -titanium aluminides are a promising material in high temperature technologies. Their high specific strength at temperatures above 700°C offers the possibility for their use as components of aerospace and automotive industries. With a specific weight of 50% of that of the widely used Ni-based superalloys TiAl is very suitable as material for fast rotating parts like turbine blades in aircraft engines and land based power stations or turbocharger rotors. Thus lower mechanical stresses and a reduced fuel consumption and CO2-emission are expected. To overcome the insufficient oxidation protection the halogen effect offers an innovative way. After surface doping using F-implantation or liquid phase-treatment with an F-containing solution and subsequent oxidation at high temperatures the formation of a protective alumina scale can be achieved. By using non-destructive ion beam analyses (PIGE, RBS F was found at the metal/oxide interface. For analysis of large scale components a new vacuum chamber at the IKF was installed and became operative. With this prototype of in-situ quality assurance system for the F-doping of manufactured parts from TiAl some performance test measurements were done and presented in this paper

Development of a PIGE-Detection System for in-situ Inspection and Quality Assurance in the Evolution of Fast Rotating Parts in High Temperature Environment Manufactured from TiAl

International Nuclear Information System (INIS)

Neve, S.; Zschau, H. E.; Masset, P.J.; Schütze, M.

2013-01-01

Intermetallic γ-titanium aluminides are a promising material in high temperature technologies. Their high specific strength at temperatures above 700 O C offers the possibility for their use as components of aerospace and automotive industries. With a specific weight of 50% of that of the widely used Ni-based superalloys TiAl is very suitable as material for fast rotating parts like turbine blades in aircraft engines and land based power stations or turbocharger rotors. Thus lower mechanical stresses and a reduced fuel consumption and CO 2 -emission are expected. To overcome the insufficient oxidation protection the halogen effect offers an innovative way. After surface doping using F-implantation or liquid phase-treatment with an F-containing solution and subsequent oxidation at high temperatures the formation of a protective alumina scale can be achieved. By using non-destructive ion beam analyses (PIGE, RBS) F was found at the metal/oxide interface. For analysis of large scale components a new vacuum chamber at the IKF was installed and became operative. With this prototype of in-situ quality assurance system for the F-doping of manufactured parts from TiAl some performance test measurements were done and presented in this paper. (author)

In situ high-pressure measurement of crystal solubility by using neutron diffraction

Science.gov (United States)

Chen, Ji; Hu, Qiwei; Fang, Leiming; He, Duanwei; Chen, Xiping; Xie, Lei; Chen, Bo; Li, Xin; Ni, Xiaolin; Fan, Cong; Liang, Akun

2018-05-01

Crystal solubility is one of the most important thermo-physical properties and plays a key role in industrial applications, fundamental science, and geoscientific research. However, high-pressure in situ measurements of crystal solubility remain very challenging. Here, we present a method involving high-pressure neutron diffraction for making high-precision in situ measurements of crystal solubility as a function of pressure over a wide range of pressures. For these experiments, we designed a piston-cylinder cell with a large chamber volume for high-pressure neutron diffraction. The solution pressures are continuously monitored in situ based on the equation of state of the sample crystal. The solubility at a high pressure can be obtained by applying a Rietveld quantitative multiphase analysis. To evaluate the proposed method, we measured the high-pressure solubility of NaCl in water up to 610 MPa. At a low pressure, the results are consistent with the previous results measured ex situ. At a higher pressure, more reliable data could be provided by using an in situ high-pressure neutron diffraction method.

In situ NiTi/Nb(Ti) composite

International Nuclear Information System (INIS)

Jiang, Daqiang; Cui, Lishan; Jiang, Jiang; Zheng, Yanjun

2013-01-01

Graphical abstract: - Highlights: • In situ NiTi/Nb(Ti) composites were fabricated. • The transformation temperature was affected by the mixing Ti:Ni atomic ratios. • The NiTi component became micron-scale lamella after forging and rolling. • The composite exhibited high strength and high damping capacity. - Abstract: This paper reports on the creation of a series of in situ NiTi/Nb(Ti) composites with controllable transformation temperatures based on the pseudo-binary hypereutectic transformation of NiTi–Nb system. The composite constituent morphology was controlled by forging and rolling. It is found that the thickness of the NiTi lamella in the composite reached micron level after the hot-forging and cold-rolling. The NiTi/Nb(Ti) composite exhibited high damping capacity as well as high yield strength

In-situ investigation of crack propagation in {gamma}-TiAl alloys using atomic force, focus ion beam and scanning electron microscopy

Energy Technology Data Exchange (ETDEWEB)

Iqbal, Farasat; Goeken, Mathias [Lehrstuhl Allgemeine Werkstoffeigenschaften, Friedrich-Alexander-Universitaet Erlangen-Nuernberg (Germany); Pyczak, Florian [GKSS Research Centre Geesthacht, Geesthacht (Germany)

2009-07-01

The present study is focused on crack propagation mechanism in Ti-45Al-1Cr and Ti-45Al-5Nb alloys with lamellar microstructure. Atomic force microscopy (AFM) is a versatile technique to study the crack propagation in-situ. AFM was employed to investigate the local deformations near the crack tip. Scanning electron microscopy (SEM) supplements the in-situ observations and was used to get a basic understanding of the crack propagation path over larger distances.A focused ion beam (FIB) was used to investigate the structures and deformation traces underneath the surface. It is concluded that the {gamma}/{alpha}2 interfaces act as favorable sites for new interfacial crack nucleation and also for interlamellar crack propagation. Nucleation of new cracks was often preceded by the interaction of deformation twins with interfaces and also by strong shear band activity in the {gamma}-TiAl lamellae visible as significant surface topography in AFM.Mostly the underneath crack path follows the {gamma}/{alpha}2 interface similar to the situation observed at the surface. The local misorientation measured with electron backscattered diffraction (EBSD) shows {gamma}-lamellae as the region of high deformation as compare to neighboring {alpha}2 -lamellae around the crack tip and its surroundings.

High temperature in operando and in situ spectroscopy on electrified surfaces and interfaces

DEFF Research Database (Denmark)

Chatzichristodoulou, Christodoulos; Hansen, Karin Vels; Holtappels, Peter

electrodes without contaminants have demanded a better insight into the electrode surface reactions and chemistries. Spectroscopic techniques can be applied to these cells but are still experimentally challenging due to the high temperature operation conditions. DTU Energy has in the recent years invested...

An overview of rotating machine systems with high-temperature bulk superconductors

Science.gov (United States)

Zhou, Difan; Izumi, Mitsuru; Miki, Motohiro; Felder, Brice; Ida, Tetsuya; Kitano, Masahiro

2012-10-01

The paper contains a review of recent advancements in rotating machines with bulk high-temperature superconductors (HTS). The high critical current density of bulk HTS enables us to design rotating machines with a compact configuration in a practical scheme. The development of an axial-gap-type trapped flux synchronous rotating machine together with the systematic research works at the Tokyo University of Marine Science and Technology since 2001 are briefly introduced. Developments in bulk HTS rotating machines in other research groups are also summarized. The key issues of bulk HTS machines, including material progress of bulk HTS, in situ magnetization, and cooling together with AC loss at low-temperature operation are discussed.

Charge collection in Si detectors irradiated in situ at superfluid helium temperature

Energy Technology Data Exchange (ETDEWEB)

Verbitskaya, Elena, E-mail: elena.verbitskaya@cern.ch [Ioffe Institute, 26 Politekhnicheskaya str., St. Petersburg 194021 (Russian Federation); Eremin, Vladimir; Zabrodskii, Andrei [Ioffe Institute, 26 Politekhnicheskaya str., St. Petersburg 194021 (Russian Federation); Dehning, Bernd; Kurfürst, Christoph; Sapinski, Mariusz; Bartosik, Marcin R. [CERN, CH-1211, Geneva 23 (Switzerland); Egorov, Nicolai [Research Institute of Material Science and Technology, 4 Passage 4806, Moscow, Zelenograd 124460 (Russian Federation); Härkönen, Jaakko [Helsinki Institute of Physics, P.O.Box 64 (Gustaf Hallströmin katu 2) FI-00014 University of Helsinki (Finland)

2015-10-01

Silicon and diamond detectors operated in a superfluid helium bath are currently being considered for the upgrade of the LHC beam loss monitoring system. The detectors would be installed in immediate proximity of the superconducting coils of the triplet magnets. We present here the results of the in situ irradiation test for silicon detectors using 23 GeV protons while keeping the detectors at a temperature of 1.9 K. Red laser (630 nm) Transient Current Technique and DC current measurements were used to study the pulse response and collected charge for silicon detectors irradiated to a maximum radiation fluence of 1×10{sup 16} p/cm{sup 2}. The dependence between collected charge and irradiation fluence was parameterized using the Hecht equation and assumption of a uniform electric field distribution. The collected charge was found to degrade with particle fluence for both bias polarities. We observed that the main factor responsible for this degradation was related to trapping of holes on the donor-type radiation-induced defects. In contrast to expectations, along with formation of donors, acceptor-type defects (electron traps) are introduced into the silicon bulk. This suggests that the current models describing charge collection in irradiated silicon detectors require an extension for taking into account trapping at low temperatures with a contribution of shallow levels. New in situ irradiation tests are needed and planned now to extend statistics of the results and gain a deeper insight into the physics of low temperature detector operation in harsh radiation environment. - Highlights: • Si detectors irradiated in situ at 1.9 K by 23 GeV protons are further studied. • Trapping parameters are derived from the fits of collected charge vs. fluence data. • Acceptor-type defects are likely to be induced along with donor-type ones. • Trapping of holes has a dominating effect on the collected charge degradation. • New tests are planned to gain deeper insight

Morphological study of electrodeposited copper under the influence of ultrasound and low temperature

International Nuclear Information System (INIS)

Mallik, A.; Ray, B.C.

2009-01-01

The effects of temperature and cavitation on the electrochemistry principle were experimented here by adding the impact of sonication to synthesize ultrafine grained deposits at low temperatures. The X-ray diffraction analysis and microscopic studies confirmed the nanorange deposit. Scanning electron microscopy images have also confirmed the powdery and highly scattered deposits in silent conditions. Ultrasound was found to have a significant effect on the deposit morphology. The deposit obtained was compact, uniform and adherent. Energy dispersive spectroscopy result of the deposits revealed an oxidized silent deposit along with some adsorbed sulfur onto the electrode surface. In contrary the in situ cleaning associated with sonication has resulted in cleaner deposits.

In-situ solvothermal processing of polycaprolactone/hydroxyapatite nanocomposites with enhanced mechanical and biological performance for bone tissue engineering

Directory of Open Access Journals (Sweden)

Saeed Moeini

2017-09-01

Full Text Available The interest in biodegradable polymer-matrix nanocomposites with bone regeneration potential has been increasing in recent years. In the present work, a solvothermal process is introduced to prepare hydroxyapatite (HA nanorod-reinforced polycaprolactone in-situ. A non-aqueous polymer solution containing calcium and phosphorous precursors is prepared and processed in a closed autoclave at different temperatures in the range of 60–150 °C. Hydroxyapatite nanorods with varying aspect ratios are formed depending on the processing temperature. X-ray diffraction analysis and field-emission scanning electron microscopy indicate that the HA nanorods are semi-crystalline. Energy-dispersive X-ray spectroscopy and Fourier transform infrared spectrometry determine that the ratio of calcium to phosphorous increases as the processing temperature increases. To evaluate the effect of in-situ processing on the mechanical properties of the nanocomposites, highly porous scaffolds (>90% containing HA nanorods are prepared by employing freeze drying and salt leaching techniques. It is shown that the elastic modulus and strength of the nanocomposites prepared by the in-situ method is superior (∼15% to those of the ex-situ samples (blended HA nanorods with the polymer solution. The enhanced bone regeneration potential of the nanocomposites is shown via an in vitro bioactivity assay in a saturated simulated body fluid. An improved cell viability and proliferation is also shown by employing (3-(4,5- dimethylthiazol-2-yl-2, 5-diphenyl tetrazolium bromide (MTT assay in human osteosarcoma cell lines. The prepared scaffolds with in vitro regeneration capacity could be potentially useful for orthopaedic applications and maxillofacial surgery.

A low-temperature scanning tunneling microscope capable of microscopy and spectroscopy in a Bitter magnet at up to 34 T.

Science.gov (United States)

Tao, W; Singh, S; Rossi, L; Gerritsen, J W; Hendriksen, B L M; Khajetoorians, A A; Christianen, P C M; Maan, J C; Zeitler, U; Bryant, B

2017-09-01

We present the design and performance of a cryogenic scanning tunneling microscope (STM) which operates inside a water-cooled Bitter magnet, which can attain a magnetic field of up to 38 T. Due to the high vibration environment generated by the magnet cooling water, a uniquely designed STM and a vibration damping system are required. The STM scan head is designed to be as compact and rigid as possible, to minimize the effect of vibrational noise as well as fit the size constraints of the Bitter magnet. The STM uses a differential screw mechanism for coarse tip-sample approach, and operates in helium exchange gas at cryogenic temperatures. The reliability and performance of the STM are demonstrated through topographic imaging and scanning tunneling spectroscopy on highly oriented pyrolytic graphite at T = 4.2 K and in magnetic fields up to 34 T.

Analysis of the structural stability of the smectite submitted to high pressures and temperatures; Analise da estabilidade estrutural da esmectita sob altas pressoes e altas temperaturas

Energy Technology Data Exchange (ETDEWEB)

Alabarse, Frederico Gil

2009-10-15

The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

Defects of diamond single crystal grown under high temperature and high pressure

Energy Technology Data Exchange (ETDEWEB)

Su, Qingcai, E-mail: suqc@sdu.edu.cn [Key Laboratory of Liquid Structure and Heredity of Materials (Ministry of Education), Shandong University, Jinan, P. R. China, 250061 (China); School of Materials Science and Engineering, Shandong University, Jinan, P. R. China, 250061 (China); Shandong Engineering Research Center for Superhard Materials, Zoucheng, P. R. China 273500 (China); Zhang, Jianhua [School of Mechanical Engineering, Shandong University, Jinan, P. R. China, 250061 (China); Li, Musen [Key Laboratory of Liquid Structure and Heredity of Materials (Ministry of Education), Shandong University, Jinan, P. R. China, 250061 (China); School of Materials Science and Engineering, Shandong University, Jinan, P. R. China, 250061 (China); Shandong Engineering Research Center for Superhard Materials, Zoucheng, P. R. China 273500 (China)

2013-11-01

The diamond single crystal, synthesized with Fe–Ni–C–B system of catalyst under high temperature and high pressure, had been observed by field emission scanning electron microscope and transmission electron microscope. The presence of a cellular structure suggested that the diamond grew from melted catalyst solution and there existed a zone of component supercooling zone in front of the solid–liquid interface. The main impurities in the diamond crystal was (FeNi){sub 23}C{sub 6}. The triangle screw pit revealed on the (111) plane was generated by the screw dislocation meeting the diamond (111) plane at the points of emergence of dislocations. A narrow twin plane was formed between the two (111) plane. - Highlights: • High pressure, high temperature synthesis of diamond single crystal. • Fe–Ni–C–B used as catalyst, graphite as carbon source. • The main impurity in the diamond crystal was (FeNi){sub 23}C{sub 6}. • Surface defects arose from screw dislocations and stacking faults.

In situ characterization of the nitridation of dysprosium during mechanochemical processing

Energy Technology Data Exchange (ETDEWEB)

Jaques, Brian J.; Osterberg, Daniel D.; Alanko, Gordon A.; Tamrakar, Sumit; Smith, Cole R.; Hurley, Michael F.; Butt, Darryl P., E-mail: DarrylButt@BoiseState.edu

2015-01-15

Highlights: • A nitridation reaction in a high energy planetary ball mill was monitored in situ. • Dysprosium mononitride was synthesized from Dy at low temperatures in short times. • Ideal gas law and in situ temperature and pressure used to assess reaction extent. • It is proposed that reaction rate is proportional to the creation of new surface. - Abstract: Processing of advanced nitride ceramics traditionally requires long durations at high temperatures and, in some cases, in hazardous atmospheres. In this study, dysprosium mononitride (DyN) was rapidly formed from elemental dysprosium in a closed system at ambient temperatures. An experimental procedure was developed to quantify the progress of the nitridation reaction during mechanochemical processing in a high energy planetary ball mill (HEBM) as a function of milling time and intensity using in situ temperature and pressure measurements, SEM, XRD, and particle size analysis. No intermediate phases were formed. It was found that the creation of fresh dysprosium surfaces dictates the rate of the nitridation reaction, which is a function of milling intensity and the number of milling media. These results show clearly that high purity nitrides can be synthesized with short processing times at low temperatures in a closed system requiring a relatively small processing footprint.

Simultaneous measurement of static and kinetic friction of ZnO nanowires in situ with a scanning electron microscope.

Science.gov (United States)

Polyakov, Boris; Dorogin, Leonid M; Vlassov, Sergei; Kink, Ilmar; Romanov, Alexey E; Lohmus, Rynno

2012-11-01

A novel method for in situ measurement of the static and kinetic friction is developed and demonstrated for zinc oxide nanowires (NWs) on oxidised silicon wafers. The experiments are performed inside a scanning electron microscope (SEM) equipped with a nanomanipulator with an atomic force microscope tip as a probe. NWs are pushed by the tip from one end until complete displacement is achieved, while NW bending is monitored by the SEM. The elastic bending profile of a NW during the manipulation process is used to calculate the static and kinetic friction forces. Copyright © 2012 Elsevier Ltd. All rights reserved.

In-situ neutron diffraction characterization of temperature dependence deformation in α-uranium

Science.gov (United States)

Calhoun, C. A.; Garlea, E.; Sisneros, T. A.; Agnew, S. R.

2018-04-01

In-situ strain neutron diffraction measurements were conducted at temperature on specimens coming from a clock-rolled α-uranium plate, and Elasto-Plastic Self-Consistent (EPSC) modeling was employed to interpret the findings. The modeling revealed that the active slip systems exhibit a thermally activated response, while deformation twinning remains athermal over the temperature ranges explored (25-150 °C). The modeling also allowed assessment of the effects of thermal residual stresses on the mechanical response during compression. These results are consistent with those from a prior study of room-temperature deformation, indicating that the thermal residual stresses strongly influence the internal strain evolution of grain families, as monitored with neutron diffraction, even though accounting for these residual stresses has little effect on the macroscopic flow curve, except in the elasto-plastic transition.

Final Report on Developing Microstructure-Property Correlation in Reactor Materials using in situ High-Energy X-rays

Energy Technology Data Exchange (ETDEWEB)

Li, Meimei [Argonne National Lab. (ANL), Argonne, IL (United States); Almer, Jonathan D. [Argonne National Lab. (ANL), Argonne, IL (United States); Yang, Yong [Univ. of Florida, Gainesville, FL (United States); Tan, Lizhen [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

2016-01-01

This report provides a summary of research activities on understanding microstructure – property correlation in reactor materials using in situ high-energy X-rays. The report is a Level 2 deliverable in FY16 (M2CA-13-IL-AN_-0403-0111), under the Work Package CA-13-IL-AN_- 0403-01, “Microstructure-Property Correlation in Reactor Materials using in situ High Energy Xrays”, as part of the DOE-NE NEET Program. The objective of this project is to demonstrate the application of in situ high energy X-ray measurements of nuclear reactor materials under thermal-mechanical loading, to understand their microstructure-property relationships. The gained knowledge is expected to enable accurate predictions of mechanical performance of these materials subjected to extreme environments, and to further facilitate development of advanced reactor materials. The report provides detailed description of the in situ X-ray Radiated Materials (iRadMat) apparatus designed to interface with a servo-hydraulic load frame at beamline 1-ID at the Advanced Photon Source. This new capability allows in situ studies of radioactive specimens subject to thermal-mechanical loading using a suite of high-energy X-ray scattering and imaging techniques. We conducted several case studies using the iRadMat to obtain a better understanding of deformation and fracture mechanisms of irradiated materials. In situ X-ray measurements on neutron-irradiated pure metal and model alloy and several representative reactor materials, e.g. pure Fe, Fe-9Cr model alloy, 316 SS, HT-UPS, and duplex cast austenitic stainless steels (CASS) CF-8 were performed under tensile loading at temperatures of 20-400°C in vacuum. A combination of wide-angle X-ray scattering (WAXS), small-angle X-ray scattering (SAXS), and imaging techniques were utilized to interrogate microstructure at different length scales in real time while the specimen was subject to thermal-mechanical loading. In addition, in situ X-ray studies were

Reliable and repeatable bonding technology for high temperature automotive power modules for electrified vehicles

International Nuclear Information System (INIS)

Yoon, Sang Won; Shiozaki, Koji; Glover, Michael D; Mantooth, H Alan

2013-01-01

This paper presents the feasibility of highly reliable and repeatable copper–tin transient liquid phase (Cu–Sn TLP) bonding as applied to die attachment in high temperature operational power modules. Electrified vehicles are attracting particular interest as eco-friendly vehicles, but their power modules are challenged because of increasing power densities which lead to high temperatures. Such high temperature operation addresses the importance of advanced bonding technology that is highly reliable (for high temperature operation) and repeatable (for fabrication of advanced structures). Cu–Sn TLP bonding is employed herein because of its high remelting temperature and desirable thermal and electrical conductivities. The bonding starts with a stack of Cu–Sn–Cu metal layers that eventually transforms to Cu–Sn alloys. As the alloys have melting temperatures (Cu 3 Sn: > 600 °C, Cu 6 Sn 5 : > 400 °C) significantly higher than the process temperature, the process can be repeated without damaging previously bonded layers. A Cu–Sn TLP bonding process was developed using thin Sn metal sheets inserted between copper layers on silicon die and direct bonded copper substrates, emulating the process used to construct automotive power modules. Bond quality is characterized using (1) proof-of-concept fabrication, (2) material identification using scanning electron microscopy and energy-dispersive x-ray spectroscopy analysis, and (3) optical analysis using optical microscopy and scanning acoustic microscope. The feasibility of multiple-sided Cu–Sn TLP bonding is demonstrated by the absence of bondline damage in multiple test samples fabricated with double- or four-sided bonding using the TLP bonding process. (paper)

In situ observation techniques of protective oxide layer

International Nuclear Information System (INIS)

Doi, Takashi; Adachi, Takeharu; Usuki, Noriaki

2015-01-01

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

Bimodular high temperature planar oxygen gas sensor

Directory of Open Access Journals (Sweden)

Xiangcheng eSun

2014-08-01

Full Text Available A bimodular planar O2 sensor was fabricated using NiO nanoparticles (NPs thin film coated yttria-stabilized zirconia (YSZ substrate. The thin film was prepared by radio frequency (r.f. magnetron sputtering of NiO on YSZ substrate, followed by high temperature sintering. The surface morphology of NiO nanoparticles film was characterized by atomic force microscopy (AFM and scanning electron microscopy (SEM. X-ray diffraction (XRD patterns of NiO NPs thin film before and after high temperature O2 sensing demonstrated that the sensing material possesses a good chemical and structure stability. The oxygen detection experiments were performed at 500 °C, 600 °C and 800 °C using the as-prepared bimodular O2 sensor under both potentiometric and resistance modules. For the potentiometric module, a linear relationship between electromotive force (EMF output of the sensor and the logarithm of O2 concentration was observed at each operating temperature, following the Nernst law. For the resistance module, the logarithm of electrical conductivity was proportional to the logarithm of oxygen concentration at each operating temperature, in good agreement with literature report. In addition, this bimodular sensor shows sensitive, reproducible and reversible response to oxygen under both sensing modules. Integration of two sensing modules into one sensor could greatly enrich the information output and would open a new venue in the development of high temperature gas sensors.

Microstructure and mechanical properties of diffusion bonded Al/Mg2Si metal matrix in situ composite

International Nuclear Information System (INIS)

Nami, H.; Halvaee, A.; Adgi, H.; Hadian, A.

2010-01-01

In this research, Al/Mg 2 Si composite produced by gravity casting, was joined by diffusion welding technique at 6 MPa pressure with various welding temperatures and durations. This metal matrix composite (MMC) containing 15% Mg 2 Si particles was produced by in situ technique. Specific diffusion bonding process was introduced as a low vacuum technique. Microstructure and shear strength of the joined areas were determined. Scanning electron microscopy examination was carried out on the welded interfaces and shear tests were conducted to the samples interface to find out the effect of welding temperatures and durations on the weldability. It was found that high welding temperatures resulted in increase of shear strength. However, increase in welding duration did not make any detectable changes. The bonded interface could be developed as a wavy state depending on the amount of parent material deformation that was associated with bonding temperature. Results indicated that MMC can be joined by diffusion welding technique successfully with satisfactory shear strength.

Reliability studies of high operating temperature MCT photoconductor detectors

Science.gov (United States)

Wang, Wei; Xu, Jintong; Zhang, Yan; Li, Xiangyang

2010-10-01

This paper concerns HgCdTe (MCT) infrared photoconductor detectors with high operating temperature. The near room temperature operation of detectors have advantages of light weight, less cost and convenient usage. Their performances are modest and they suffer from reliable problems. These detectors face with stability of the package, chip bonding area and passivation layers. It's important to evaluate and improve the reliability of such detectors. Defective detectors were studied with SEM(Scanning electron microscope) and microscopy. Statistically significant differences were observed between the influence of operating temperature and the influence of humidity. It was also found that humility has statistically significant influence upon the stability of the chip bonding and passivation layers, and the amount of humility isn't strongly correlated to the damage on the surface. Considering about the commonly found failures modes in detectors, special test structures were designed to improve the reliability of detectors. An accelerated life test was also implemented to estimate the lifetime of the high operating temperature MCT photoconductor detectors.

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

Energy Technology Data Exchange (ETDEWEB)

Liu, Xingbo [West Virginia Univ., Morgantown, WV (United States)

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.

Temperature-dependent surface porosity of Nb{sub 2}O{sub 5} under high-flux, low-energy He{sup +} ion irradiation

Energy Technology Data Exchange (ETDEWEB)

Novakowski, T.J., E-mail: tnovakow@purdue.edu; Tripathi, J.K.; Hosinski, G.M.; Joseph, G.; Hassanein, A.

2016-01-30

Graphical abstract: - Highlights: • Nb{sub 2}O{sub 5} surfaces are nanostructured with a novel He{sup +} ion irradiation process. • High-flux, low energy He{sup +} ion irradiation generates highly porous surfaces. • Top-down approach guarantees good contact between different crystallites. • Sample annealing demonstrates temperature effect on surface morphology. • Surface pore diameter increases with increasing temperature. - Abstract: The present study reports on high-flux, low-energy He{sup +} ion irradiation as a novel method of enhancing the surface porosity and surface area of naturally oxidized niobium (Nb). Our study shows that ion-irradiation-induced Nb surface micro- and nano-structures are highly tunable by varying the target temperature during ion bombardment. Mirror-polished Nb samples were irradiated with 100 eV He{sup +} ions at a flux of 1.2 × 10{sup 21} ions m{sup −2} s{sup −1} to a total fluence of 4.3 × 10{sup 24} ions m{sup −2} with simultaneous sample annealing in the temperature range of 773–1223 K to demonstrate the influence of sample temperature on the resulting Nb surface morphology. This surface morphology was primarily characterized using field-emission scanning electron microscopy (FE-SEM) and atomic force microscopy (AFM). Below 923 K, Nb surfaces form nano-scale tendrils and exhibit significant increases in surface porosity. Above 923 K, homogeneously populated nano-pores with an average diameter of ∼60 nm are observed in addition to a smaller population of sub-micron sized pores (up to ∼230 nm in diameter). Our analysis shows a significant reduction in surface pore number density and surface porosity with increasing sample temperature. High-resolution ex situ X-ray photoelectron spectroscopy (XPS) shows Nb{sub 2}O{sub 5} phase in all of the ion-irradiated samples. To further demonstrate the length scales in which radiation-induced surface roughening occurs, optical reflectivity was performed over a spectrum of

In-situ identification of marine organisms using high frequency, wideband ultrasound

DEFF Research Database (Denmark)

Pham, An Hoai

methods. Conventional acoustical methods use frequencies in the range of 10 to 500 kHz and give reasonable estimations of size distribution, if the species is known, but can only significantly support the determination of the actual species, if there are only a few known species available. It is expected...... that higher frequencies and broader bandwidths than used until now will give more information useful for fish species identification. The objective of this Ph.D. study has been to develop a method to investigate the possibility of in-situ identification of fish with high-frequency, wideband ultrasound...... and the fish bodies. The frequencies are 2, 3.5, and 6 MHz. The angles are -30°, -15°, 0°, 15°, and 30°. The results show that even though there are variations, a scan of the ultrasound backscatter along a fish of a specific species contains patterns that are characteristic for that species. This is true...

Safety, efficacy, and predictability of laser in situ keratomileusis to correct myopia or myopic astigmatism with a 750 Hz scanning-spot laser system.

Science.gov (United States)

Tomita, Minoru; Watabe, Miyuki; Yukawa, Satoshi; Nakamura, Nobuo; Nakamura, Tadayuki; Magnago, Thomas

2014-02-01

To evaluate the clinical outcomes of laser in situ keratomileusis (LASIK) to correct myopia or myopic astigmatism using the Amaris 750S 750 Hz excimer laser. Private LASIK center, Tokyo, Japan. Case series. Patients with myopia or myopic astigmatism (spherical equivalent -0.50 to -11.63 diopters [D]), a corrected distance visual acuity (CDVA) of 20/20 or better, and an estimated residual bed thickness of 300 μm or more had LASIK using the aspheric aberration-free ablation profile of the 750 Hz scanning-spot laser and the Femto LDV Crystal Line femtosecond laser for flap creation. Study parameters included uncorrected distance visual acuity (UDVA), CDVA, manifest refraction, astigmatism, and higher-order aberrations (HOAs). The study included 1280 eyes (685 patients). At 3 months, 96.6% of eyes had a UDVA of 20/20 or better and 99.1% had 20/32 or better; 94.1% of eyes were within ± 0.50 D of the intended correction and 98.9% were within ± 1.00 D; 89.7% of eyes had no residual cylinder and 96.0% had a postoperative astigmatism of less than 0.50 D. All eyes had a postoperative CDVA of 20/20 or better. The HOAs increased postoperatively (PLaser in situ keratomileusis with the 750 Hz scanning-spot laser was safe, effective, and predictable. No specific clinical side effects that might be associated with a high repetition rate occurred. Mr. Magnago is an employee of Schwind eye-tech-solutions GmbH. No other author has a financial or proprietary interest in any material or method mentioned. Copyright © 2013 ASCRS and ESCRS. Published by Elsevier Inc. All rights reserved.

An experimental platform for triaxial high-pressure/high-temperature testing of rocks using computed tomography

Science.gov (United States)

Glatz, Guenther; Lapene, Alexandre; Castanier, Louis M.; Kovscek, Anthony R.

2018-04-01

A conventional high-pressure/high-temperature experimental apparatus for combined geomechanical and flow-through testing of rocks is not X-ray compatible. Additionally, current X-ray transparent systems for computed tomography (CT) of cm-sized samples are limited to design temperatures below 180 °C. We describe a novel, high-temperature (>400 °C), high-pressure (>2000 psi/>13.8 MPa confining, >10 000 psi/>68.9 MPa vertical load) triaxial core holder suitable for X-ray CT scanning. The new triaxial system permits time-lapse imaging to capture the role of effective stress on fluid distribution and porous medium mechanics. System capabilities are demonstrated using ultimate compressive strength (UCS) tests of Castlegate sandstone. In this case, flooding the porous medium with a radio-opaque gas such as krypton before and after the UCS test improves the discrimination of rock features such as fractures. The results of high-temperature tests are also presented. A Uintah Basin sample of immature oil shale is heated from room temperature to 459 °C under uniaxial compression. The sample contains kerogen that pyrolyzes as temperature rises, releasing hydrocarbons. Imaging reveals the formation of stress bands as well as the evolution and connectivity of the fracture network within the sample as a function of time.

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

Science.gov (United States)

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

2017-04-07

The ferritic Fe-Cr-Ni-Al-Ti alloys strengthened by hierarchical-Ni 2 TiAl/NiAl or single-Ni 2 TiAl precipitates have been developed and received great attentions due to their superior creep resistance, as compared to conventional ferritic steels. Although the significant improvement of the creep resistance is achieved in the hierarchical-precipitate-strengthened ferritic alloy, the in-depth understanding of its high-temperature deformation mechanisms is essential to further optimize the microstructure and mechanical properties, and advance the development of the creep resistant materials. In the present study, in-situ neutron diffraction has been used to investigate the evolution of elastic strain of constitutive phases and their interactions, such as load-transfer/load-relaxation behavior between the precipitate and matrix, during tensile deformation and stress relaxation at 973 K, which provide the key features in understanding the governing deformation mechanisms. Crystal-plasticity finite-element simulations were employed to qualitatively compare the experimental evolution of the elastic strain during tensile deformation at 973 K. It was found that the coherent elastic strain field in the matrix, created by the lattice misfit between the matrix and precipitate phases for the hierarchical-precipitate-strengthened ferritic alloy, is effective in reducing the diffusional relaxation along the interface between the precipitate and matrix phases, which leads to the strong load-transfer capability from the matrix to precipitate.

High Temperature Annealing Studies on the Piezoelectric Properties of Thin Aluminum Nitride Films

Energy Technology Data Exchange (ETDEWEB)

Farrell, R.; Pagan, V.R.; Kabulski, A.; Kuchibhatla, S.; Harman, J.; Kasarla, K.R.; Rodak, L.E.; Hensel, J.P.; Famouri, P.; Korakakis, D.

2008-01-01

A Rapid Thermal Annealing (RTA) system was used to anneal sputtered and MOVPE-grown Aluminum Nitride (AlN) thin films at temperatures up to 1000°C in ambient and controlled environments. According to Energy Dispersive X-Ray Analysis (EDAX), the films annealed in an ambient environment rapidly oxidize after five minutes at 1000°C. Below 1000°C the films oxidized linearly as a function of annealing temperature which is consistent with what has been reported in literature [1]. Laser Doppler Vibrometry (LDV) was used to measure the piezoelectric coefficient, d33, of these films. Films annealed in an ambient environment had a weak piezoelectric response indicating that oxidation on the surface of the film reduces the value of d33. A high temperature furnace has been built that is capable of taking in-situ measurements of the piezoelectric response of AlN films. In-situ d33 measurements are recorded up to 300°C for both sputtered and MOVPE-grown AlN thin films. The measured piezoelectric response appears to increase with temperature up to 300°C possibly due to stress in the film.

High Temperature Annealing Studies on the Piezoelectric Properties of Thin Aluminum Nitride Films

Energy Technology Data Exchange (ETDEWEB)

R. Farrell; V. R. Pagan; A. Kabulski; Sridhar Kuchibhatl; J. Harman; K. R. Kasarla; L. E. Rodak; P. Famouri; J. Peter Hensel; D. Korakakis

2008-05-01

A Rapid Thermal Annealing (RTA) system was used to anneal sputtered and MOVPE grown Aluminum Nitride (AlN) thin films at temperatures up to 1000°C in ambient and controlled environments. According to Energy Dispersive X-Ray Analysis (EDAX), the films annealed in an ambient environment rapidly oxidize after five minutes at 1000°C. Below 1000°C the films oxidized linearly as a function of annealing temperature which is consistent with what has been reported in literature [1]. Laser Doppler Vibrometry (LDV) was used to measure the piezoelectric coefficient, d33, of these films. Films annealed in an ambient environment had a weak piezoelectric response indicating that oxidation on the surface of the film reduces the value of d33. A high temperature furnace has been built that is capable of taking in-situ measurements of the piezoelectric response of AlN films. In-situ d33 measurements are recorded up to 300°C for both sputtered and MOVPE-grown AlN thin films. The measured piezoelectric response appears to increase with temperature up to 300°C possibly due to stress in the film.

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

International Nuclear Information System (INIS)

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

2006-01-01

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

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

Science.gov (United States)

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

2006-05-01

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

Epitaxial deposition of silver ultrafine nano-clusters on defect-free surfaces of HOPG-derived few-layer graphene in a UHV multi-chamber by in-situ STM, ex-situ XPS and ab initio calculations

CSIR Research Space (South Africa)

Ndlovu, GF

2012-03-01

Full Text Available The growth of three-dimensional ultra-fine spherical nano-particles of silver on few layers of graphene derived from highly oriented pyrolytic graphite in ultra-high vacuum were characterized using in situ scanning tunneling microscopy (STM...

Room temperature synthesis and high temperature frictional study of silver vanadate nanorods

Energy Technology Data Exchange (ETDEWEB)

Singh, D P; Aouadi, S M [Department of Physics, Southern Illinois University, Carbondale-62901 (United States); Polychronopoulou, K [Department of Chemistry, University of Cyprus, Nicosia, 1678 (Cyprus); Rebholz, C, E-mail: dineshpsingh@gmail.com, E-mail: saouadi@physics.siu.edu [Department of Mechanical and Manufacturing Engineering, University of Cyprus, Nicosia, 1678 (Cyprus)

2010-08-13

We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly {beta}-AgV O{sub 3}) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 {mu}m and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 deg. C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O{sub 3} completely transformed into silver vanadium oxide (Ag{sub 2}V{sub 4}O{sub 11}) and silver with an increase in temperature from RT to 700 deg. C.

Room temperature synthesis and high temperature frictional study of silver vanadate nanorods.

Science.gov (United States)

Singh, D P; Polychronopoulou, K; Rebholz, C; Aouadi, S M

2010-08-13

We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly beta-AgV O(3)) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 microm and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 degrees C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O(3) completely transformed into silver vanadium oxide (Ag(2)V(4)O(11)) and silver with an increase in temperature from RT to 700 degrees C.

The structure of phosphate and borosilicate glasses and their structural evolution at high temperatures as studied with solid state NMR spectroscopy: Phase separation, crystallisation and dynamic species exchange

International Nuclear Information System (INIS)

Wegner, S.; Van Wullen, L.; Tricot, G.; Tricot, G.

2010-01-01

In this contribution we present an in-depth study of the network structure of different phosphate based and borosilicate glasses and its evolution at high temperatures. Employing a range of advanced solid state NMR methodologies, complemented by the results of XPS, the structural motifs on short and intermediate length scales are identified. For the phosphate based glasses, at temperatures above the glass transition temperature Tg, structural relaxation processes and the devitrification of the glasses were monitored in situ employing MAS NMR spectroscopy and X-ray diffraction. Dynamic species exchange involving rapid P-O-P and P-O-Al bond breaking and reforming was observed employing in situ 27 Al and 31 P MAS NMR spectroscopy and could be linked to viscous flow. For the borosilicate glasses, an atomic scale investigation of the phase separation processes was possible in a combined effort of ex situ NMR studies on glass samples with different thermal histories and in situ NMR studies using high temperature MAS NMR spectroscopy including 11 B MAS, 29 Si MAS and in situ 29 Si{ 11 B} REAPDOR NMR spectroscopy. (authors)

In-situ tensile test of high strength nanocrystalline bainitic steel

Energy Technology Data Exchange (ETDEWEB)

Haddad, Mike, E-mail: mike.haddad@uni-ulm.de [Institute of Micro and Nanomaterials, University of Ulm, Ulm (Germany); Ivanisenko, Yulia; Courtois-Manara, Eglantine [Institute of Nanotechnology, Karlsruhe Institute of Technology, Karlsruhe (Germany); Fecht, Hans-Jörg [Institute of Micro and Nanomaterials, University of Ulm, Ulm (Germany)

2015-01-03

Because of its great importance in modern engineering and technology applications, steel continues to be highly relevant in the modern research field of nanocrystalline materials. Innovative processing methods and procedures are required for the production of such materials, which possess superior properties compared to their conventional counter parts. In this research, the original microstructure of a commercial C45 steel (Fe, 0.42–0.5 wt% C, 0.5–0.8 wt% Mn) was modified from ferritic–pearlitic to bainitic. Warm high pressure torsion for 5 rotations at 6 GPa and 350 °C was used to process the bainitic sample leading to an ultrafine/nano-scale grain size. A unique nano-crystalline microstructure consisting of equiaxed and elongated ferrite grains with a mean size smaller than 150 nm appeared in images taken by Transmission Electron Microscopy. Results of in-situ tensile testing in a scanning electron microscope showed very high tensile strength, on the order of 2100 MPa with a total elongation of 4.5% in comparison with 800 MPa and around 16% in the original state. Fracture occurred abruptly, without any sign of necking, and was typically caused by the stress concentration at a surface flaw. Also, stress concentrations near all surface defects were observed on the sample, visualized by the formation of shear bands. The fracture surface was covered with dimples, indicating ductile fracture. These properties are fully comparable with high strength, high alloyed steels.

Charge collection in Si detectors irradiated in situ at superfluid helium temperature

Science.gov (United States)

Verbitskaya, Elena; Eremin, Vladimir; Zabrodskii, Andrei; Dehning, Bernd; Kurfürst, Christoph; Sapinski, Mariusz; Bartosik, Marcin R.; Egorov, Nicolai; Härkönen, Jaakko

2015-10-01

Silicon and diamond detectors operated in a superfluid helium bath are currently being considered for the upgrade of the LHC beam loss monitoring system. The detectors would be installed in immediate proximity of the superconducting coils of the triplet magnets. We present here the results of the in situ irradiation test for silicon detectors using 23 GeV protons while keeping the detectors at a temperature of 1.9 K. Red laser (630 nm) Transient Current Technique and DC current measurements were used to study the pulse response and collected charge for silicon detectors irradiated to a maximum radiation fluence of 1×1016 p/cm2. The dependence between collected charge and irradiation fluence was parameterized using the Hecht equation and assumption of a uniform electric field distribution. The collected charge was found to degrade with particle fluence for both bias polarities. We observed that the main factor responsible for this degradation was related to trapping of holes on the donor-type radiation-induced defects. In contrast to expectations, along with formation of donors, acceptor-type defects (electron traps) are introduced into the silicon bulk. This suggests that the current models describing charge collection in irradiated silicon detectors require an extension for taking into account trapping at low temperatures with a contribution of shallow levels. New in situ irradiation tests are needed and planned now to extend statistics of the results and gain a deeper insight into the physics of low temperature detector operation in harsh radiation environment.

Investigation of Kinetic Hydrate Inhibition Using a High Pressure Micro Differential Scanning Calorimeter

DEFF Research Database (Denmark)

Daraboina, Nagu; Malmos, Christine; von Solms, Nicolas

2013-01-01

of hydrate growth. Additionally, hydrate formed in the presence of inhibitor decomposed at higher temperatures compared to pure water, indicating that while hydrate formation is initially inhibited; once hydrates form, they are more stable in the presence of inhibitor. Overall, this method proved a viable......Methane hydrate formation and decomposition were investigated in the presence of the kinetic inhibitor (Luvicap EG) and synergist (polyethylene oxide; PEO) using a high pressure micro-differential scanning calorimeter (HP-μDSC) with both temperature ramping and isothermal temperature programs....... These investigations were performed using small samples in four different capillary tubes in the calorimeter cell. When the isothermal method was employed, it was found that Luvicap EG significantly delays the hydrate nucleation time as compared to water. The results obtained from the ramping method demonstrated...

Assessing the High Temperature, High Pressure Subsurface for Anaerobic Methane Oxidation

Science.gov (United States)

Harris, R. L.; Bartlett, D.; Byrnes, A. W.; Walsh, K. M.; Lau, C. Y. M.; Onstott, T. C.

2017-12-01

The anaerobic oxidation of methane (AOM) is an important sink in the global methane (CH4) budget. ANMEs are known to oxidize CH4 either independently or in consortia with bacteria, coupling the reduction of electron acceptors such as, SO42-, NO2-, NO3-, Mn4+, or Fe3+. To further constrain the contribution of AOM to the global CH4 budget, it is important to assess unexplored environments where AOM is thermodynamically possible such as the high pressure, high temperature deep biosphere. Provided plausible electron acceptor availability, increased temperature and pCH4 yield favorable Gibbs free energies for AOM reactions and the production of ATP (Fig. 1). To date, only sulfate-dependent AOM metabolism has been documented under high temperature conditions (50-72˚C), and AOM has not been assessed above 10.1 MPa. Given that ANMEs share close phylogenetic and metabolic heritage with methanogens and that the most heat-tolerant microorganism known is a barophilic methanogen, there possibly exist thermophilic ANMEs. Here we describe preliminary results from high pressure, high temperature stable isotope tracer incubation experiments on deep biosphere samples. Deep sub-seafloor sediments collected by IODP 370 from the Nankai Trough (257 - 865 m below seafloor) and deep fracture fluid from South Africa (1339 m below land surface) were incubated anaerobically in hydrostatic pressure vessels at 40 MPa in simulated in situ temperatures (40˚ - 80˚C). Sediments and fracture fluid were incubated in sulfate-free artificial seawater, a 2:98 13CH4:N2 headspace, and treated with one of the potential electron acceptors listed above in addition to kill and endogenous activity (i.e. no added electron acceptor) controls. Stable isotope analysis of dissolved inorganic carbon (DIC) suggests that AOM occurred within 60 days of incubation for all investigated electron acceptors and temperatures except 50˚C. Sulfate-dependent AOM rates are consistent with those previously reported in the