Effect of roll hot press temperature on crystallite size of PVDF film
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hartono, Ambran, E-mail: ambranhartono@yahoo.com; Sanjaya, Edi; Djamal, Mitra
2014-03-24
Fabrication PVDF films have been made using Hot Roll Press. Preparation of samples carried out for nine different temperatures. This condition is carried out to see the effect of Roll Hot Press temperature on the size of the crystallite of PVDF films. To obtain the diffraction pattern of sample characterization is performed using X-Ray Diffraction. Furthermore, from the diffraction pattern is obtained, the calculation to determine the crystallite size of the sample by using the Scherrer equation. From the experimental results and the calculation of crystallite sizes obtained for the samples with temperature 130 °C up to 170 °C respectivelymore » increased from 7.2 nm up to 20.54 nm. These results show that increasing temperatures will also increase the size of the crystallite of the sample. This happens because with the increasing temperature causes the higher the degree of crystallization of PVDF film sample is formed, so that the crystallite size also increases. This condition indicates that the specific volume or size of the crystals depends on the magnitude of the temperature as it has been studied by Nakagawa.« less
Using sieving and pretreatment to separate plastics during end-of-life vehicle recycling.
Stagner, Jacqueline A; Sagan, Barsha; Tam, Edwin Kl
2013-09-01
Plastics continue to be a challenge for recovering materials at the end-of-life for vehicles. However, it may be possible to improve the recovery of plastics by exploiting material characteristics, such as shape, or by altering their behavior, such as through temperature changes, in relation to recovery processes and handling. Samples of a 2009 Dodge Challenger front fascia were shredded in a laboratory-scale hammer mill shredder. A 2 × 2 factorial design study was performed to determine the effect of sample shape (flat versus curved) and sample temperature (room temperature versus cryogenic temperature) on the size of the particles exiting from the shredder. It was determined that sample shape does not affect the particle size; however, sample temperature does affect the particle size. At cryogenic temperatures, the distribution of particle sizes is much narrower than at room temperature. Having a more uniform particle size could make recovery of plastic particles, such as these more efficient during the recycling of end-of-life vehicles. Samples of Chrysler minivan headlights were also shredded at room temperature and at cryogenic temperatures. The size of the particles of the two different plastics in the headlights is statistically different both at room temperature and at cryogenic temperature, and the particles are distributed narrowly. The research suggests that incremental changes in end-of-life vehicle processing could be effective in aiding materials recovery.
Cryogenic homogenization and sampling of heterogeneous multi-phase feedstock
Doyle, Glenn Michael; Ideker, Virgene Linda; Siegwarth, James David
2002-01-01
An apparatus and process for producing a homogeneous analytical sample from a heterogenous feedstock by: providing the mixed feedstock, reducing the temperature of the feedstock to a temperature below a critical temperature, reducing the size of the feedstock components, blending the reduced size feedstock to form a homogeneous mixture; and obtaining a representative sample of the homogeneous mixture. The size reduction and blending steps are performed at temperatures below the critical temperature in order to retain organic compounds in the form of solvents, oils, or liquids that may be adsorbed onto or absorbed into the solid components of the mixture, while also improving the efficiency of the size reduction. Preferably, the critical temperature is less than 77 K (-196.degree. C.). Further, with the process of this invention the representative sample may be maintained below the critical temperature until being analyzed.
Thermal conductivity of graphene mediated by strain and size
Kuang, Youdi; Shi, Sanqiang; Wang, Xinjiang; ...
2016-06-09
Based on first-principles calculations and full iterative solution of the linearized Boltzmann–Peierls transport equation for phonons, we systematically investigate effects of strain, size and temperature on the thermal conductivity k of suspended graphene. The calculated size-dependent and temperature-dependent k for finite samples agree well with experimental data. The results show that, contrast to the convergent room-temperature k = 5450 W/m-K of unstrained graphene at a sample size ~8 cm, k of strained graphene diverges with increasing the sample size even at high temperature. Out-of-plane acoustic phonons are responsible for the significant size effect in unstrained and strained graphene due tomore » their ultralong mean free path and acoustic phonons with wavelength smaller than 10 nm contribute 80% to the intrinsic room temperature k of unstrained graphene. Tensile strain hardens the flexural modes and increases their lifetimes, causing interesting dependence of k on sample size and strain due to the competition between boundary scattering and intrinsic phonon–phonon scattering. k of graphene can be tuned within a large range by strain for the size larger than 500 μm. These findings shed light on the nature of thermal transport in two-dimensional materials and may guide predicting and engineering k of graphene by varying strain and size.« less
Experimental and numerical modeling research of rubber material during microwave heating process
NASA Astrophysics Data System (ADS)
Chen, Hailong; Li, Tao; Li, Kunling; Li, Qingling
2018-05-01
This paper aims to investigate the heating behaviors of block rubber by experimental and simulated method. The COMSOL Multiphysics 5.0 software was utilized in numerical simulation work. The effects of microwave frequency, power and sample size on temperature distribution are examined. The effect of frequency on temperature distribution is obvious. The maximum and minimum temperatures of block rubber increase first and then decrease with frequency increasing. The microwave heating efficiency is maximum in the microwave frequency of 2450 MHz. However, more uniform temperature distribution is presented in other microwave frequencies. The influence of microwave power on temperature distribution is also remarkable. The smaller the power, the more uniform the temperature distribution on the block rubber. The effect of power on microwave heating efficiency is not obvious. The effect of sample size on temperature distribution is evidently found. The smaller the sample size, the more uniform the temperature distribution on the block rubber. However, the smaller the sample size, the lower the microwave heating efficiency. The results can serve as references for the research on heating rubber material by microwave technology.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Anandakumar, U.; Webb, J.E.; Singh, R.N.
The matrix cracking behavior of a zircon matrix - uniaxial SCS 6 fiber composite was studied as a function of initial flaw size and temperature. The composites were fabricated by a tape casting and hot pressing technique. Surface flaws of controlled size were introduced using a vicker`s indenter. The composite samples were tested in three point flexure at three different temperatures to study the non steady state and steady state matrix cracking behavior. The composite samples exhibited steady state and non steady matrix cracking behavior at all temperatures. The steady state matrix cracking stress and steady state crack size increasedmore » with increasing temperature. The results of the study correlated well with the results predicted by the matrix cracking models.« less
Damage Accumulation in Silica Glass Nanofibers.
Bonfanti, Silvia; Ferrero, Ezequiel E; Sellerio, Alessandro L; Guerra, Roberto; Zapperi, Stefano
2018-06-06
The origin of the brittle-to-ductile transition, experimentally observed in amorphous silica nanofibers as the sample size is reduced, is still debated. Here we investigate the issue by extensive molecular dynamics simulations at low and room temperatures for a broad range of sample sizes, with open and periodic boundary conditions. Our results show that small sample-size enhanced ductility is primarily due to diffuse damage accumulation, that for larger samples leads to brittle catastrophic failure. Surface effects such as boundary fluidization contribute to ductility at room temperature by promoting necking, but are not the main driver of the transition. Our results suggest that the experimentally observed size-induced ductility of silica nanofibers is a manifestation of finite-size criticality, as expected in general for quasi-brittle disordered networks.
NASA Astrophysics Data System (ADS)
Ratnawulan, Fauzi, Ahmad; AE, Sukma Hayati
2017-08-01
Copper oxide powder was prepared from Copper iron from South Solok, Indonesia. The samples was dried and calcined for an hour at temperatures of 145°C, 300°C,850°C, 1000°C. Phase transformation and crystallite size of the calcined powders have been investigated as a function of calcination temperature by room-temperature X-ray diffraction (XRD). It was seen that the tenorite, CuO was successfully obtained. With increasing calcining temperature, CuO transformed from malachite Cu2(CO3)(OH)2 to tenorite phase (CuO) and crystallite size of prepared samples increased from 36 nm to 76 nm.
Albasan, Hasan; Lulich, Jody P; Osborne, Carl A; Lekcharoensuk, Chalermpol; Ulrich, Lisa K; Carpenter, Kathleen A
2003-01-15
To determine effects of storage temperature and time on pH and specific gravity of and number and size of crystals in urine samples from dogs and cats. Randomized complete block design. 31 dogs and 8 cats. Aliquots of each urine sample were analyzed within 60 minutes of collection or after storage at room or refrigeration temperatures (20 vs 6 degrees C [68 vs 43 degrees F]) for 6 or 24 hours. Crystals formed in samples from 11 of 39 (28%) animals. Calcium oxalate (CaOx) crystals formed in vitro in samples from 1 cat and 8 dogs. Magnesium ammonium phosphate (MAP) crystals formed in vitro in samples from 2 dogs. Compared with aliquots stored at room temperature, refrigeration increased the number and size of crystals that formed in vitro; however, the increase in number and size of MAP crystals in stored urine samples was not significant. Increased storage time and decreased storage temperature were associated with a significant increase in number of CaOx crystals formed. Greater numbers of crystals formed in urine aliquots stored for 24 hours than in aliquots stored for 6 hours. Storage time and temperature did not have a significant effect on pH or specific gravity. Urine samples should be analyzed within 60 minutes of collection to minimize temperature- and time-dependent effects on in vitro crystal formation. Presence of crystals observed in stored samples should be validated by reevaluation of fresh urine.
Effect of annealing temperature on the size and magnetic properties of CoFe2O4 nanoparticle
NASA Astrophysics Data System (ADS)
Sunny, Annrose; Akshay, V. R.; Vasundhara, M.
2018-05-01
CoFe2O4 (CFO) nanoparticles (NPs) are synthesized using sol gel method and are annealed at 400, 600 and 800 °C for 4h. The crystal structure and morphology of the NPs are investigated through XRD and TEM analysis. The X- ray diffraction analysis shows that all the samples are well formed and attain a cubic structure with Fd-3m space group. The morphology of the material is found to be polygonal and the particle size of the NPs is increased with increase of annealing temperature as 400, 600 and 800 to be 20 nm, 30 nm and 70 nm respectively. The magnetic properties of the NPs are investigated using VSM and observed that the curie temperature for 400, 600 and 800 °C annealing temperature are 762 K, 780 K, 769 K respectively. The Ms of 600 sample is 80 emu/g. The 400 and 800 sample shows lower Ms value this is due to poor crystalanity and exaggerated grain growth at the respective temperatures. The coercivity of the sample shows linear dependence with particle size of the material the highest coercivity is obtained for 400 sample and low value for 800 sample.
NASA Astrophysics Data System (ADS)
Verma, Narendra Kumar; Patel, Sandeep Kumar Singh; Kumar, Dinesh; Singh, Chandra Bhal; Singh, Akhilesh Kumar
2018-05-01
We have investigated the effect of sintering temperature on the densification behaviour, grain size, structural and dielectric properties of BaTiO3 ceramics, prepared by high energy ball milling method. The Powder x-ray diffraction reveals the tetragonal structure with space group P4mm for all the samples. The samples were sintered at four different temperatures, (T = 900°C, 1000°C, 1100°C, 1200°C and 1300°C). Density increased with increasing sintering temperature, reaching up to 97% at 1300°C. A grain growth was observed with increasing sintering temperature. Impedance analyses of the sintered samples at various temperatures were performed. Increase in dielectric constant and Curie temperature is observed with increasing sintering temperature.
Influence of temperature and aging time on HA synthesized by the hydrothermal method.
Kothapalli, C R; Wei, M; Legeros, R Z; Shaw, M T
2005-05-01
The influence of temperature and aging time on the morphology and mechanical properties of nano-sized hydroxyapatite (HA) synthesized by a hydrothermal method is reported here. The pre-mixed reactants were poured into a stirred autoclave and reacted at temperatures between 25-250 degrees C for 2-10 h. HA powders thus obtained were examined using X-ray diffraction (XRD), high-resolution field emission scanning electron microscopy (FESEM) and a particle size analyzer. It was found that the aspect ratio of the particles increased with the reaction temperature. The length of the HA particles increased with the reaction temperature below 170 degrees C, but it decreased when the temperature was raised above 170 degrees C. The agglomerates of HA particles were formed during synthesis, and their sizes were strongly dependent on reaction temperatures. As the reaction temperature increased, the agglomerate size decreased (p = 0.008). The density of the discs pressed from these samples reached 85-90% of the theoretical density after sintering at 1200 degrees C for 1 h. No decomposition to other calcium phosphates was detected at this sintering temperature. A correlation existed (p = 0.05) between the agglomerate sizes of HA particles synthesized at various conditions and their sintered densities. With the increase of the agglomerate size, the sintered density of the HA compact decreased. It was found that both the sintered density and flexural strength increased with increasing aging time and reaction temperature. A maximum flexural strength of 78 MPa was observed for the samples synthesized at 170 degrees C for 5 h with the predicted average at these conditions being 65 MPa. These samples attained an average sintered density of 88%.
NASA Astrophysics Data System (ADS)
Gholizadeh, Ahmad
2018-04-01
In the present work, the influence of different sintering atmospheres and temperatures on physical properties of the Cu0.5Zn0.5Fe2O4 nanoparticles including the redistribution of Zn2+ and Fe3+ ions, the oxidation of Fe atoms in the lattice, crystallite sizes, IR bands, saturation magnetization and magnetic core sizes have been investigated. The fitting of XRD patterns by using Fullprof program and also FT-IR measurement show the formation of a cubic structure with no presence of impurity phase for all the samples. The unit cell parameter of the samples sintered at the air- and inert-ambient atmospheres trend to decrease with sintering temperature, but for the samples sintered under carbon monoxide-ambient atmosphere increase. The magnetization curves versus the applied magnetic field, indicate different behaviour for the samples sintered at 700 °C with the respect to the samples sintered at 300 °C. Also, the saturation magnetization increases with the sintering temperature and reach a maximum 61.68 emu/g in the sample sintered under reducing atmosphere at 600 °C. The magnetic particle size distributions of samples have been calculated by fitting the M-H curves with the size distributed Langevin function. The results obtained from the XRD and FTIR measurements suggest that the magnetic core size has the dominant effect in variation of the saturation magnetization of the samples.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jomekian, A.; Faculty of Chemical Engineering, Iran University of Science and Technology; Behbahani, R.M., E-mail: behbahani@put.ac.ir
Ultra porous ZIF-8 particles synthesized using PEO/PA6 based poly(ether-block-amide) (Pebax 1657) as structure directing agent. Structural properties of ZIF-8 samples prepared under different synthesis parameters were investigated by laser particle size analysis, XRD, N{sub 2} adsorption analysis, BJH and BET tests. The overall results showed that: (1) The mean pore size of all ZIF-8 samples increased remarkably (from 0.34 nm to 1.1–2.5 nm) compared to conventionally synthesized ZIF-8 samples. (2) Exceptional BET surface area of 1869 m{sup 2}/g was obtained for a ZIF-8 sample with mean pore size of 2.5 nm. (3) Applying high concentrations of Pebax 1657 to themore » synthesis solution lead to higher surface area, larger pore size and smaller particle size for ZIF-8 samples. (4) Both, Increase in temperature and decrease in molar ratio of MeIM/Zn{sup 2+} had increasing effect on ZIF-8 particle size, pore size, pore volume, crystallinity and BET surface area of all investigated samples. - Highlights: • The pore size of ZIF-8 samples synthesized with Pebax 1657 increased remarkably. • The BET surface area of 1869 m{sup 2}/gr obtained for a ZIF-8 synthesized sample with Pebax. • Increase in temperature had increasing effect on textural properties of ZIF-8 samples. • Decrease in MeIM/Zn{sup 2+} had increasing effect on textural properties of ZIF-8 samples.« less
NASA Astrophysics Data System (ADS)
Bose, Vipin C.; Biju, V.
2015-02-01
Nanostructured Mn3O4 sample with an average crystallite size of ˜15 nm is synthesized via the reduction of potassium permanganate using hydrazine. The average particle size obtained from the Transmission Electron Microscopy analysis is in good agreement with the average crystallite size estimated from X-ray diffraction analysis. The presence of Mn4+ ions at the octahedral sites is inferred from the results of Raman, UV-visible absorption and X-ray photoelectron spectroscopy analyzes. DC electrical conductivity of the sample in the temperature range 313-423 K, is about five orders of magnitude larger than that reported for single crystalline Mn3O4 sample. The dominant conduction mechanism is identified to be of the polaronic hopping of holes between cations in the octahedral sites. The zero field cooled and field cooled magnetization of the sample is studied in the range 20-300 K. The Curie temperature for the sample is about 45 K, below which the sample is ferrimagnetic. A blocking temperature of 35 K is observed in the field cooled curve. It is observed that the sample shows hysteresis at temperatures below the Curie temperature with no saturation, even at an applied field (20 kOe). The presence of an ordered core and disordered surface of spin arrangements is observed from the magnetization studies. Above the Curie temperature, the sample shows linear dependence of magnetization on applied field with no hysteresis characteristic of paramagnetic phase.
NASA Astrophysics Data System (ADS)
Taheriniya, Shabnam; Parhizgar, Sara Sadat; Sari, Amir Hossein
2018-06-01
To study the alumina template pore size distribution as a function of Al thin film grain size distribution, porous alumina templates were prepared by anodizing sputtered aluminum thin films. To control the grain size the aluminum samples were sputtered with the rate of 0.5, 1 and 2 Å/s and the substrate temperature was either 25, 75 or 125 °C. All samples were anodized for 120 s in 1 M sulfuric acid solution kept at 1 °C while a 15 V potential was being applied. The standard deviation value for samples deposited at room temperature but with different rates is roughly 2 nm in both thin film and porous template form but it rises to approximately 4 nm with substrate temperature. Samples with the average grain size of 13, 14, 18.5 and 21 nm respectively produce alumina templates with an average pore size of 8.5, 10, 15 and 16 nm in that order which shows the average grain size limits the average pore diameter in the resulting template. Lateral correlation length and grain boundary effect are other factors that affect the pore formation process and pore size distribution by limiting the initial current density.
NMR/MRI with hyperpolarized gas and high Tc SQUID
Schlenga, Klaus; de Souza, Ricardo E.; Wong-Foy, Annjoe; Clarke, John; Pines, Alexander
2000-01-01
A method and apparatus for the detection of nuclear magnetic resonance (NMR) signals and production of magnetic resonance imaging (MRI) from samples combines the use of hyperpolarized inert gases to enhance the NMR signals from target nuclei in a sample and a high critical temperature (Tc) superconducting quantum interference device (SQUID) to detect the NMR signals. The system operates in static magnetic fields of 3 mT or less (down to 0.1 mT), and at temperatures from liquid nitrogen (77K) to room temperature. Sample size is limited only by the size of the magnetic field coils and not by the detector. The detector is a high Tc SQUID magnetometer designed so that the SQUID detector can be very close to the sample, which can be at room temperature.
NASA Astrophysics Data System (ADS)
Ranjbar, M.; Ghazi, M. E.; Izadifard, M.
2018-06-01
In this paper we have investigated the annealing temperature effect on the structure, morphology, dielectric and magnetic properties of sol-gel synthesized multiferroic BiFeO3 nanoparticles. X-ray diffraction spectroscopy revealed that all the samples have rhombohedrally distorted perovskite structure and the most pure BFO phase is obtained on the sample annealed at 800 °C. Field emission scanning electron microscopy (FESEM) revealed that increasing annealing temperature would increase the particle size. Decrease in dielectric constant was also observed by increasing annealing temperature. Vibrating sample method (VSM) analysis confirmed that samples annealed at 500-700 °C with particle size below the BFO's spiral spin structure length, have well saturated M-H curve and show ferromagnetic behavior.
NASA Astrophysics Data System (ADS)
Wilbourn, E.; Thornton, D.; Brooks, S. D.; Graff, J.
2016-12-01
The role of marine aerosols as ice nucleating particles is currently poorly understood. Despite growing interest, there are remarkably few ice nucleation measurements on representative marine samples. Here we present results of heterogeneous ice nucleation from laboratory studies and in-situ air and sea water samples collected during NAAMES (North Atlantic Aerosol and Marine Ecosystems Study). Thalassiosira weissflogii (CCMP 1051) was grown under controlled conditions in batch cultures and the ice nucleating activity depended on the growth phase of the cultures. Immersion freezing temperatures of the lab-grown diatoms were determined daily using a custom ice nucleation apparatus cooled at a set rate. Our results show that the age of the culture had a significant impact on ice nucleation temperature, with samples in stationary phase causing nucleation at -19.9 °C, approximately nine degrees warmer than the freezing temperature during exponential growth phase. Field samples gathered during the NAAMES II cruise in May 2016 were also tested for ice nucleating ability. Two types of samples were gathered. Firstly, whole cells were fractionated by size from surface seawater using a BD Biosciences Influx Cell Sorter (BD BS ISD). Secondly, aerosols were generated using the SeaSweep and subsequently size-selected using a PIXE Cascade Impactor. Samples were tested for the presence of ice nucleating particles (INP) using the technique described above. There were significant differences in the freezing temperature of the different samples; of the three sample types the lab-grown cultures tested during stationary phase froze at the warmest temperatures, followed by the SeaSweep samples (-25.6 °C) and the size-fractionated cell samples (-31.3 °C). Differences in ice nucleation ability may be due to size differences between the INP, differences in chemical composition of the sample, or some combination of these two factors. Results will be presented and atmospheric implications discussed.
NASA Astrophysics Data System (ADS)
Thomas, Rini; Das, Gangadhar; Mondal, Rajib; Pradheesh, R.; Mahato, R. N.; Geetha Kumary, T.; Nirmala, R.; Morozkin, A. V.; Lamsal, J.; Yelon, W. B.; Nigam, A. K.; Malik, S. K.
2012-04-01
Nanocrystalline La0.15Ca0.85MnO3 samples of various grain sizes ranging from ˜17 to 42 nm have been prepared by sol-gel technique. Phase purity and composition were verified by room temperature x-ray diffraction and SEM-EDAX analysis. The bulk La0.15Ca0.85MnO3 is known to order antiferromagnetically around 170 K and to undergo a simultaneous crystal structural transition. DC magnetization measurements on 17 nm size La0.15Ca0.85MnO3 show a peak at ˜130 K (TN) in zero-field-cooled (ZFC) state. Field-cooled magnetization bifurcates from ZFC data around 200 K hinting a weak ferromagnetic component near room temperature due to surface moments of the nanoparticle sample. Low temperature powder neutron diffraction experiments reveal that the incomplete structural transition from room temperature orthorhombic to low temperature orthorhombic-monoclinic state also occurs in the nanoparticle sample as in the bulk. Magnetization in the ordered state decreases as particle size increases, thus indicating the reduction of the competing ferromagnetic surface moments.
NASA Astrophysics Data System (ADS)
Terada, T.; Sato, M.; Mochizuki, N.; Yamamoto, Y.; Tsunakawa, H.
2013-12-01
Magnetic properties of ferromagnetic minerals generally depend on their chemical composition, crystal structure, size, and shape. In the usual paleomagnetic study, we use a bulk sample which is the assemblage of magnetic minerals showing broad distributions of various magnetic properties. Microscopic and Curie-point observations of the bulk sample enable us to identify the constituent magnetic minerals, while other measurements, for example, stepwise thermal and/or alternating field demagnetizations (ThD, AFD) make it possible to estimate size, shape and domain state of the constituent magnetic grains. However, estimation based on stepwise demagnetizations has a limitation that magnetic grains with the same coercivity Hc (or blocking temperature Tb) can be identified as the single population even though they could have different size and shape. Dunlop and West (1969) carried out mapping of grain size and coercivity (Hc) using pTRM. However, it is considered that their mapping method is basically applicable to natural rocks containing only SD grains, since the grain sizes are estimated on the basis of the single domain theory (Neel, 1949). In addition, it is impossible to check thermal alteration due to laboratory heating in their experiment. In the present study we propose a new experimental method which makes it possible to estimate distribution of size and shape of magnetic minerals in a bulk sample. The present method is composed of simple procedures: (1) imparting ARM to a bulk sample, (2) ThD at a certain temperature, (3) stepwise AFD on the remaining ARM, (4) repeating the steps (1) ~ (3) with ThD at elevating temperatures up to the Curie temperature of the sample. After completion of the whole procedures, ARM spectra are calculated and mapped on the HC-Tb plane (hereafter called HC-Tb diagram). We analyze the Hc-Tb diagrams as follows: (1) For uniaxial SD populations, theoretical curve for a certain grain size (or shape anisotropy) is drawn on the Hc-Tb diagram. The curves are calculated using the single domain theory, since coercivity and blocking temperature of uniaxial SD grains can be expressed as a function of size and shape. (2) Boundary between SD and MD grains are calculated and drawn on the Hc-Tb diagram according to the theory by Butler and Banerjee (1975). (3) Theoretical predictions by (1) and (2) are compared with the obtained ARM spectra to estimate quantitive distribution of size, shape and domain state of magnetic grains in the sample. This mapping method has been applied to three samples: Hawaiian basaltic lava extruded in 1995, Ueno basaltic lava formed during Matsuyama chron, and Oshima basaltic lava extruded in 1986. We will discuss physical states of magnetic grains (size, shape, domain state, etc.) and their possible origins.
Temperature dependence of the size distribution function of InAs quantum dots on GaAs(001)
DOE Office of Scientific and Technical Information (OSTI.GOV)
Arciprete, F.; Fanfoni, M.; Patella, F.
2010-04-15
We present a detailed atomic-force-microscopy study of the effect of annealing on InAs/GaAs(001) quantum dots grown by molecular-beam epitaxy. Samples were grown at a low growth rate at 500 deg. C with an InAs coverage slightly greater than critical thickness and subsequently annealed at several temperatures. We find that immediately quenched samples exhibit a bimodal size distribution with a high density of small dots (<50 nm{sup 3}) while annealing at temperatures greater than 420 deg. C leads to a unimodal size distribution. This result indicates a coarsening process governing the evolution of the island size distribution function which is limitedmore » by the attachment-detachment of the adatoms at the island boundary. At higher temperatures one cannot ascribe a single rate-determining step for coarsening because of the increased role of adatom diffusion. However, for long annealing times at 500 deg. C the island size distribution is strongly affected by In desorption.« less
NASA Astrophysics Data System (ADS)
Dadras, Sedigheh; Davoudiniya, Masoumeh
2018-05-01
This paper sets out to investigate and compare the effects of Ag nanoparticles and carbon nanotubes (CNTs) doping on the mechanical properties of Y1Ba2Cu3O7-δ (YBCO) high temperature superconductor. For this purpose, the pure and doped YBCO samples were synthesized by sol-gel method. The microstructural analysis of the samples is performed using X-ray diffraction (XRD). The crystalline size, lattice strain and stress of the pure and doped YBCO samples were estimated by modified forms of Williamson-Hall analysis (W-H), namely, uniform deformation model (UDM), uniform deformation stress model (UDSM) and the size-strain plot method (SSP). These results show that the crystalline size, lattice strain and stress of the YBCO samples declined by Ag nanoparticles and CNTs doping.
Ferromagnetism appears in nitrogen implanted nanocrystalline diamond films
NASA Astrophysics Data System (ADS)
Remes, Zdenek; Sun, Shih-Jye; Varga, Marian; Chou, Hsiung; Hsu, Hua-Shu; Kromka, Alexander; Horak, Pavel
2015-11-01
The nanocrystalline diamond films turn to be ferromagnetic after implanting various nitrogen doses on them. Through this research, we confirm that the room-temperature ferromagnetism of the implanted samples is derived from the measurements of magnetic circular dichroism (MCD) and superconducting quantum interference device (SQUID). Samples with larger crystalline grains as well as higher implanted doses present more robust ferromagnetic signals at room temperature. Raman spectra indicate that the small grain-sized samples are much more disordered than the large grain-sized ones. We propose that a slightly large saturated ferromagnetism could be observed at low temperature, because the increased localization effects have a significant impact on more disordered structure.
Effects of crystallite size on the structure and magnetism of ferrihydrite
DOE Office of Scientific and Technical Information (OSTI.GOV)
Wang, Xiaoming; Zhu, Mengqiang; Koopal, Luuk K.
2015-12-15
The structure and magnetic properties of nano-sized (1.6 to 4.4 nm) ferrihydrite samples are systematically investigated through a combination of X-ray diffraction (XRD), X-ray pair distribution function (PDF), X-ray absorption spectroscopy (XAS) and magnetic analyses. The XRD, PDF and Fe K-edge XAS data of the ferrihydrite samples are all fitted well with the Michel ferrihydrite model, indicating similar local-, medium- and long-range ordered structures. PDF and XAS fitting results indicate that, with increasing crystallite size, the average coordination numbers of Fe–Fe and the unit cell parameter c increase, while Fe2 and Fe3 vacancies and the unit cell parameter a decrease.more » Mössbauer results indicate that the surface layer is relatively disordered, which might have been caused by the random distribution of Fe vacancies. These results support Hiemstra's surface-depletion model in terms of the location of disorder and the variations of Fe2 and Fe3 occupancies with size. Magnetic data indicate that the ferrihydrite samples show antiferromagnetism superimposed with a ferromagnetic-like moment at lower temperatures (100 K and 10 K), but ferrihydrite is paramagnetic at room temperature. In addition, both the magnetization and coercivity decrease with increasing ferrihydrite crystallite size due to strong surface effects in fine-grained ferrihydrites. Smaller ferrihydrite samples show less magnetic hyperfine splitting and a lower unblocking temperature (T B) than larger samples. The dependence of magnetic properties on grain size for nano-sized ferrihydrite provides a practical way to determine the crystallite size of ferrihydrite quantitatively in natural environments or artificial systems.« less
Grain size effect on the electrical and magneto-transport properties of nanosized Pr0.67Sr0.33MnO3
NASA Astrophysics Data System (ADS)
Ng, S. W.; Lim, K. P.; Halim, S. A.; Jumiah, H.
2018-06-01
In this study, nanosized of Pr0.67Sr0.33MnO3 prepared via sol-gel method followed by heat treatment at 600-1000 °C in intervals of 100 °C were synthesized. The structure, surface morphology, electrical, magneto-transport and magnetic properties of the samples were investigated. Rietveld refinements of X-ray diffraction patterns confirm that single phase orthorhombic crystal structure with the space group of Pnma (62) is formed at 600 °C. A strong dependence of surface morphology, electrical and magneto-transport properties on grain size have been observed in this manganites system. Both grain size and crystallite size are increases with the sintering temperature due to the congregation effect. Upon increasing grain size, the paramagnetic-ferromagnetic transition temperature increases from 278 K to 295 K. The resistivity drops and the metal-insulator transition temperature shifted from 184 K to 248 K with increases of grain size due to the grain growth and reduction of grain boundary. Below metal-insulator transition temperature, the samples fit well to the combination of resistivity due to grain or domain boundaries, electron-electron scattering process and electron-phonon interaction. The resistivity data above the metal-insulator transition temperature is well described using small polaron hopping and variable range hopping models. It is found that the negative magnetoresistance also increases with larger grain size where the highest %MR of - 26% can be observed for sample sintered at 1000 °C (245 nm).
NASA Astrophysics Data System (ADS)
Jiang, Chengpeng; Fan, Xi'an; Hu, Jie; Feng, Bo; Xiang, Qiusheng; Li, Guangqiang; Li, Yawei; He, Zhu
2018-04-01
During the past few decades, Bi2Te3-based alloys have been investigated extensively because of their promising application in the area of low temperature waste heat thermoelectric power generation. However, their thermal stability must be evaluated to explore the appropriate service temperature. In this work, the thermal stability of zone melting p-type (Bi, Sb)2Te3-based ingots was investigated under different annealing treatment conditions. The effect of service temperature on the thermoelectric properties and hardness of the samples was also discussed in detail. The results showed that the grain size, density, dimension size and mass remained nearly unchanged when the service temperature was below 523 K, which suggested that the geometry size of zone melting p-type (Bi, Sb)2Te3-based materials was stable below 523 K. The power factor and Vickers hardness of the ingots also changed little and maintained good thermal stability. Unfortunately, the thermal conductivity increased with increasing annealing temperature, which resulted in an obvious decrease of the zT value. In addition, the thermal stabilities of the zone melting p-type (Bi, Sb)2Te3-based materials and the corresponding powder metallurgy samples were also compared. All evidence implied that the thermal stabilities of the zone-melted (ZMed) p-type (Bi, Sb)2Te3 ingots in terms of crystal structure, geometry size, power factor (PF) and hardness were better than those of the corresponding powder metallurgy samples. However, their thermal stabilities in terms of zT values were similar under different annealing temperatures.
NASA Astrophysics Data System (ADS)
Palihawadana Arachchige, Maheshika; Nemala, Humeshkar; Naik, Vaman; Naik, Ratna
Magnetic hyperthermia (MHT) has a great potential as a non-invasive cancer therapy technique. Specific absorption rate (SAR) which measures the efficiency of heat generation, mainly depends on magnetic properties of nanoparticles such as saturation magnetization (Ms) and magnetic anisotropy (K) which depend on the size and shape. Therefore, MHT applications of magnetic nanoparticles often require a controllable synthesis to achieve desirable magnetic properties. We have synthesized Fe3O4 nanoparticles using two different methods, co-precipitation (CP) and hydrothermal (HT) techniques to produce similar XRD crystallite size of 12 nm, and subsequently coated with dextran to prepare ferrofluids for MHT. However, TEM measurements show average particle sizes of 13.8 +/-3.6 nm and 14.6 +/-3.6 nm for HT and CP samples, implying the existence of an amorphous surface layer for both. The MHT data show the two samples have very different SAR values of 110 W/g (CP) and 40W/g (HT) at room temperature, although they have similar Ms of 70 +/-4 emu/g regardless of their different TEM sizes. We fitted the temperature dependent SAR using linear response theory to explain the observed results. CP sample shows a larger magnetic core with a narrow size distribution and a higher K value compared to that of HT sample.
Boonna, Sureeporn; Tongta, Sunanta
2018-07-01
Structural transformation of crystallized debranched cassava starch prepared by temperature cycling (TC) treatment and then subjected to annealing (ANN), heat-moisture treatment (HMT) and dual hydrothermal treatments of ANN and HMT was investigated. The relative crystallinity, lateral crystal size, melting temperature and resistant starch (RS) content increased for all hydrothermally treated samples, but the slowly digestible starch (SDS) content decreased. The RS content followed the order: HMT → ANN > HMT > ANN → HMT > ANN > TC, respectively. The HMT → ANN sample showed a larger lateral crystal size with more homogeneity, whereas the ANN → HMT sample had a smaller lateral crystal size with a higher melting temperature. After cooking at 50% moisture, the increased RS content of samples was observed, particularly for the ANN → HMT sample. These results suggest that structural changes of crystallized debranched starch during hydrothermal treatments depend on initial crystalline characteristics and treatment sequences, influencing thermal stability, enzyme digestibility, and cooking stability. Copyright © 2018 Elsevier Ltd. All rights reserved.
Electrical and magnetic properties of nano-sized magnesium ferrite
NASA Astrophysics Data System (ADS)
T, Smitha; X, Sheena; J, Binu P.; Mohammed, E. M.
2015-02-01
Nano-sized magnesium ferrite was synthesized using sol-gel techniques. Structural characterization was done using X-ray diffractometer and Fourier Transform Infrared Spectrometer. Vibration Sample Magnetometer was used to record the magnetic measurements. XRD analysis reveals the prepared sample is single phasic without any impurity. Particle size calculation shows the average crystallite size of the sample is 19nm. FTIR analysis confirmed spinel structure of the prepared samples. Magnetic measurement study shows that the sample is ferromagnetic with high degree of isotropy. Hysterisis loop was traced at temperatures 100K and 300K. DC electrical resistivity measurements show semiconducting nature of the sample.
Wang, Zhaojie; Alaniz, Joseph E; Jang, Wanyoung; Garay, Javier E; Dames, Chris
2011-06-08
The thermal conductivity reduction due to grain boundary scattering is widely interpreted using a scattering length assumed equal to the grain size and independent of the phonon frequency (gray). To assess these assumptions and decouple the contributions of porosity and grain size, five samples of undoped nanocrystalline silicon have been measured with average grain sizes ranging from 550 to 64 nm and porosities from 17% to less than 1%, at temperatures from 310 to 16 K. The samples were prepared using current activated, pressure assisted densification (CAPAD). At low temperature the thermal conductivities of all samples show a T(2) dependence which cannot be explained by any traditional gray model. The measurements are explained over the entire temperature range by a new frequency-dependent model in which the mean free path for grain boundary scattering is inversely proportional to the phonon frequency, which is shown to be consistent with asymptotic analysis of atomistic simulations from the literature. In all cases the recommended boundary scattering length is smaller than the average grain size. These results should prove useful for the integration of nanocrystalline materials in devices such as advanced thermoelectrics.
Erfani, Maryam; Saion, Elias; Soltani, Nayereh; Hashim, Mansor; Wan Abdullah, Wan Saffiey B.; Navasery, Manizheh
2012-01-01
Calcium borate nanoparticles have been synthesized by a thermal treatment method via facile co-precipitation. Differences of annealing temperature and annealing time and their effects on crystal structure, particle size, size distribution and thermal stability of nanoparticles were investigated. The formation of calcium borate compound was characterized by X-ray diffraction (XRD) and Fourier Transform Infrared spectroscopy (FTIR), Transmission electron microscopy (TEM), and Thermogravimetry (TGA). The XRD patterns revealed that the co-precipitated samples annealed at 700 °C for 3 h annealing time formed an amorphous structure and the transformation into a crystalline structure only occurred after 5 h annealing time. It was found that the samples annealed at 900 °C are mostly metaborate (CaB2O4) nanoparticles and tetraborate (CaB4O7) nanoparticles only observed at 970 °C, which was confirmed by FTIR. The TEM images indicated that with increasing the annealing time and temperature, the average particle size increases. TGA analysis confirmed the thermal stability of the annealed samples at higher temperatures. PMID:23203073
ZnFe2O4 nanoparticles dispersed in a highly porous silica aerogel matrix: a magnetic study.
Bullita, S; Casu, A; Casula, M F; Concas, G; Congiu, F; Corrias, A; Falqui, A; Loche, D; Marras, C
2014-03-14
We report the detailed structural characterization and magnetic investigation of nanocrystalline zinc ferrite nanoparticles supported on a silica aerogel porous matrix which differ in size (in the range 4-11 nm) and the inversion degree (from 0.4 to 0.2) as compared to bulk zinc ferrite which has a normal spinel structure. The samples were investigated by zero-field-cooling-field-cooling, thermo-remnant DC magnetization measurements, AC magnetization investigation and Mössbauer spectroscopy. The nanocomposites are superparamagnetic at room temperature; the temperature of the superparamagnetic transition in the samples decreases with the particle size and therefore it is mainly determined by the inversion degree rather than by the particle size, which would give an opposite effect on the blocking temperature. The contribution of particle interaction to the magnetic behavior of the nanocomposites decreases significantly in the sample with the largest particle size. The values of the anisotropy constant give evidence that the anisotropy constant decreases upon increasing the particle size of the samples. All these results clearly indicate that, even when dispersed with low concentration in a non-magnetic and highly porous and insulating matrix, the zinc ferrite nanoparticles show a magnetic behavior similar to that displayed when they are unsupported or dispersed in a similar but denser matrix, and with higher loading. The effective anisotropy measured for our samples appears to be systematically higher than that measured for supported zinc ferrite nanoparticles of similar size, indicating that this effect probably occurs as a consequence of the high inversion degree.
Anomalous permittivity in fine-grain barium titanate
NASA Astrophysics Data System (ADS)
Ostrander, Steven Paul
Fine-grain barium titanate capacitors exhibit anomalously large permittivity. It is often observed that these materials will double or quadruple the room temperature permittivity of a coarse-grain counterpart. However, aside from a general consensus on this permittivity enhancement, the properties of the fine-grain material are poorly understood. This thesis examines the effect of grain size on dielectric properties of a self-consistent set of high density undoped barium titanate capacitors. This set included samples with grain sizes ranging from submicron to ˜20 microns, and with densities generally above 95% of the theoretical. A single batch of well characterized powder was milled, dry-pressed then isostatically-pressed. Compacts were fast-fired, but sintering temperature alone was used to control the grain size. With this approach, the extrinsic influences are minimized within the set of samples, but more importantly, they are normalized between samples. That is, with a single batch of powder and with identical green processing, uniform impurity concentration is expected. The fine-grain capacitors exhibited a room temperature permittivity of ˜5500 and dielectric losses of ˜2%. The Curie-temperature decreased by {˜}5sp°C from that of the coarse-grain material, and the two ferroelectric-ferroelectric phase transition temperatures increased by {˜}10sp°C. The grain size induced permittivity enhancement was only active in the tetragonal and orthorhombic phases. Strong dielectric anomalies were observed in samples with grain size as small as {˜}0.4\\ mum. It is suggested that the strong first-order character observed in the present data is related to control of microstructure and stoichiometry. Grain size effects on conductivity losses, ferroelectric losses, ferroelectric dispersion, Maxwell-Wagner dispersion, and dielectric aging of permittivity and loss were observed. For the fine-grain material, these observations suggest the suppression of domain wall motion below the Curie transition, and the suppression of conductivity above the Curie transition.
A Model of Thermal Conductivity for Planetary Soils: 1. Theory for Unconsolidated Soils
NASA Technical Reports Server (NTRS)
Piqueux, S.; Christensen, P. R.
2009-01-01
We present a model of heat conduction for mono-sized spherical particulate media under stagnant gases based on the kinetic theory of gases, numerical modeling of Fourier s law of heat conduction, theoretical constraints on the gas thermal conductivity at various Knudsen regimes, and laboratory measurements. Incorporating the effect of the temperature allows for the derivation of the pore-filling gas conductivity and bulk thermal conductivity of samples using additional parameters (pressure, gas composition, grain size, and porosity). The radiative and solid-to-solid conductivities are also accounted for. Our thermal model reproduces the well-established bulk thermal conductivity dependency of a sample with the grain size and pressure and also confirms laboratory measurements finding that higher porosities generally lead to lower conductivities. It predicts the existence of the plateau conductivity at high pressure, where the bulk conductivity does not depend on the grain size. The good agreement between the model predictions and published laboratory measurements under a variety of pressures, temperatures, gas compositions, and grain sizes provides additional confidence in our results. On Venus, Earth, and Titan, the pressure and temperature combinations are too high to observe a soil thermal conductivity dependency on the grain size, but each planet has a unique thermal inertia due to their different surface temperatures. On Mars, the temperature and pressure combination is ideal to observe the soil thermal conductivity dependency on the average grain size. Thermal conductivity models that do not take the temperature and the pore-filling gas composition into account may yield significant errors.
NASA Astrophysics Data System (ADS)
Maaz, K.; Karim, S.; Mumtaz, A.; Hasanain, S. K.; Liu, J.; Duan, J. L.
2009-06-01
Magnetic nanoparticles of nickel ferrite (NiFe 2O 4) have been synthesized by co-precipitation route using stable ferric and nickel salts with sodium hydroxide as the precipitating agent and oleic acid as the surfactant. X-ray diffraction (XRD) and transmission electron microscope (TEM) analyses confirmed the formation of single-phase nickel ferrite nanoparticles in the range 8-28 nm depending upon the annealing temperature of the samples during the synthesis. The size of the particles ( d) was observed to be increasing linearly with annealing temperature of the sample while the coercivity with particle size goes through a maximum, peaking at ˜11 nm and then decreases for larger particles. Typical blocking effects were observed below ˜225 K for all the prepared samples. The superparamagnetic blocking temperature ( T B) was found to be increasing with increasing particle size that has been attributed to the increased effective anisotropy energy of the nanoparticles. The saturation moment of all the samples was found much below the bulk value of nickel ferrite that has been attributed to the disordered surface spins or dead/inert layer in these nanoparticles.
Stoichiometry of Cd(S,Se) nanocrystals by anomalous small-angle x-ray scattering
NASA Astrophysics Data System (ADS)
Ramos, Aline; Lyon, Olivier; Levelut, Claire
1995-12-01
In Cd(S,Se)-doped glasses the optical properties are strongly dependent on the size of the nanocrystals, but can be also largely modified by changes in the crystal stoichiometry; however, the information on both stoichiometry and size is difficult to obtain in crystals smaller than 10 nm. The intensity scattered at small angles is classically used to get information about nanoparticles sizes. Moreover the variation of amplitude of this intensity with the energy of the x ray—``the anomalous effect''—near the selenium edge is related to stoichiometry. Anomalous small-angle x-ray scattering has been used as a tentative method to get information about stoichiometry in nanocrystals with size lower than 10 nm. Experiments have been performed on samples treated for 2 days at temperatures in the range 540-650 °C. The samples treated at temperatures above 580 °C contain crystals with size larger than 4 nm. For all these samples the anomalous effect has nearly the same amplitude, and we found the stoichiometry x=0.4 for the CdSxSe1-x nanocrystals. This agrees with the previous results obtained by scanning electron microscopy and Raman spectroscopy. The results are also confirmed by measurements of the position of the optical absorption edge and by wide-angle x-ray scattering experiments. For the sample treated at 560 °C, the nanocrystal size is 3 nm and the stoichiometry x=0.6 is deduced from the anomalous effect. For samples treated at lower temperatures the anomalous effect is not observable, indicating an even lower selenium content in the nanocrystals (x≳0.7). We observed differences in the Se content of nanocrystals for different heat treatments of the same initial glass. These results may be very helpful to interpret the change in the optical properties when the temperature of the treatments decreases in the range 560-590 °C. In this temperature range, compositional effects seem to be of the same order of magnitude as the effects of the quantum confinement.
Detection of melting by X-ray imaging at high pressure
DOE Office of Scientific and Technical Information (OSTI.GOV)
Li, Li; Weidner, Donald J.
2014-06-15
The occurrence of partial melting at elevated pressure and temperature is documented in real time through measurement of volume strain induced by a fixed temperature change. Here we present the methodology for measuring volume strains to one part in 10{sup −4} for mm{sup 3} sized samples in situ as a function of time during a step in temperature. By calibrating the system for sample thermal expansion at temperatures lower than the solidus, the onset of melting can be detected when the melting volume increase is of comparable size to the thermal expansion induced volume change. We illustrate this technique withmore » a peridotite sample at 1.5 GPa during partial melting. The Re capsule is imaged with a CCD camera at 20 frames/s. Temperature steps of 100 K induce volume strains that triple with melting. The analysis relies on image comparison for strain determination and the thermal inertia of the sample is clearly seen in the time history of the volume strain. Coupled with a thermodynamic model of the melting, we infer that we identify melting with 2 vol.% melting.« less
Influence of specimen dimensions on ductile-to-brittle transition temperature in Charpy impact test
NASA Astrophysics Data System (ADS)
Rzepa, S.; Bucki, T.; Konopík, P.; Džugan, J.; Rund, M.; Procházka, R.
2017-02-01
This paper discusses the correlation between specimen dimensions and transition temperature. Notch toughness properties of Standard Charpy-V specimens are compared to samples with lower width (7.5 mm, 5 mm, 2.5 mm) and sub-size Charpy specimens with cross section 3×4. In this study transition curves are correlated with lateral ductile part of fracture related ones for 5 considered geometries. Based on the results obtained, correlation procedure for transition temperature determination of full size specimens defined by fracture appearance of sub-sized specimens is proposed.
Yu, Jiaguo; Qi, Lifang; Cheng, Bei; Zhao, Xiufeng
2008-12-30
Tungsten trioxide hollow microspheres were prepared by immersing SrWO4 microspheres in a concentrated HNO3 solution, and then calcined at different temperatures. The prepared tungsten oxide samples were characterized by X-ray diffraction, X-ray photoelectron spectroscopy, Fourier transform infrared spectra, differential thermal analysis-thermogravimetry, UV-visible spectrophotometry, scanning electron microscopy, N2 adsorption/desorption measurements. The photocatalytic activity of the samples was evaluated by photocatalytic decolorization of rhodamine B aqueous solution under visible-light irradiation. It was found that with increasing calcination temperatures, the average crystallite size and average pore size increased, on the contrary, Brunauer-Emmett-Teller-specific surface areas decreased. However, pore volume and porosity increased firstly, and then decreased. Increasing calcination temperatures resulted in the changes of surface morphology of hollow microspheres. The un-calcined and 300 degrees C-calcined samples showed higher photocatalytic activity than other samples. At 400 degrees C, the photocatalytic activity decreased greatly due to the decrease of specific surface areas. At 500 degrees C, the photocatalytic activity of the samples increased again due to the junction effect of two phases.
Magnetic properties of M0.3Fe2.7O4 (M = Fe, Zn and Mn) ferrites nanoparticles
NASA Astrophysics Data System (ADS)
Modaresi, Nahid; Afzalzadeh, Reza; Aslibeiki, Bagher; Kameli, Parviz
2018-06-01
In the present article a comparative study on the structural and magnetic properties of nano-sized M0.3Fe0.7Fe2O4 (M = Fe, Zn and Mn) ferrites have been reported. The X-ray diffraction (XRD) patterns show that the crystallite size depends on the cation distribution. The Rietveld refinement of XRD patterns using MAUD software determines the distribution of cations and unit cell dimensions. The magnetic measurements show that the maximum and minimum value of saturation magnetization is obtained for Zn and Mn doped samples, respectively. The peak temperature of AC magnetic susceptibility of Zn and Fe doped samples below 300 K shows the superparamagnetic behavior in these samples at room temperature. the AC susceptibility results confirm the presence of strong interactions between the nanoparticles which leads to a superspin glass state in the samples at low temperatures.
In Situ Balloon-Borne Ice Particle Imaging in High-Latitude Cirrus
NASA Astrophysics Data System (ADS)
Kuhn, Thomas; Heymsfield, Andrew J.
2016-09-01
Cirrus clouds reflect incoming solar radiation, creating a cooling effect. At the same time, these clouds absorb the infrared radiation from the Earth, creating a greenhouse effect. The net effect, crucial for radiative transfer, depends on the cirrus microphysical properties, such as particle size distributions and particle shapes. Knowledge of these cloud properties is also needed for calibrating and validating passive and active remote sensors. Ice particles of sizes below 100 µm are inherently difficult to measure with aircraft-mounted probes due to issues with resolution, sizing, and size-dependent sampling volume. Furthermore, artefacts are produced by shattering of particles on the leading surfaces of the aircraft probes when particles several hundred microns or larger are present. Here, we report on a series of balloon-borne in situ measurements that were carried out at a high-latitude location, Kiruna in northern Sweden (68N 21E). The method used here avoids these issues experienced with the aircraft probes. Furthermore, with a balloon-borne instrument, data are collected as vertical profiles, more useful for calibrating or evaluating remote sensing measurements than data collected along horizontal traverses. Particles are collected on an oil-coated film at a sampling speed given directly by the ascending rate of the balloon, 4 m s-1. The collecting film is advanced uniformly inside the instrument so that an always unused section of the film is exposed to ice particles, which are measured by imaging shortly after sampling. The high optical resolution of about 4 µm together with a pixel resolution of 1.65 µm allows particle detection at sizes of 10 µm and larger. For particles that are 20 µm (12 pixel) in size or larger, the shape can be recognized. The sampling volume, 130 cm3 s-1, is well defined and independent of particle size. With the encountered number concentrations of between 4 and 400 L-1, this required about 90- to 4-s sampling times to determine particle size distributions of cloud layers. Depending on how ice particles vary through the cloud, several layers per cloud with relatively uniform properties have been analysed. Preliminary results of the balloon campaign, targeting upper tropospheric, cold cirrus clouds, are presented here. Ice particles in these clouds were predominantly very small, with a median size of measured particles of around 50 µm and about 80 % of all particles below 100 µm in size. The properties of the particle size distributions at temperatures between -36 and -67 °C have been studied, as well as particle areas, extinction coefficients, and their shapes (area ratios). Gamma and log-normal distribution functions could be fitted to all measured particle size distributions achieving very good correlation with coefficients R of up to 0.95. Each distribution features one distinct mode. With decreasing temperature, the mode diameter decreases exponentially, whereas the total number concentration increases by two orders of magnitude with decreasing temperature in the same range. The high concentrations at cold temperatures also caused larger extinction coefficients, directly determined from cross-sectional areas of single ice particles, than at warmer temperatures. The mass of particles has been estimated from area and size. Ice water content (IWC) and effective diameters are then determined from the data. IWC did vary only between 1 × 10-3 and 5 × 10-3 g m-3 at temperatures below -40 °C and did not show a clear temperature trend. These measurements are part of an ongoing study.
Size effects in olivine control strength in low-temperature plasticity regime
NASA Astrophysics Data System (ADS)
Kumamoto, K. M.; Thom, C.; Wallis, D.; Hansen, L. N.; Armstrong, D. E. J.; Goldsby, D. L.; Warren, J. M.; Wilkinson, A. J.
2017-12-01
The strength of the lithospheric mantle during deformation by low-temperature plasticity controls a range of geological phenomena, including lithospheric-scale strain localization, the evolution of friction on deep seismogenic faults, and the flexure of tectonic plates. However, constraints on the strength of olivine in this deformation regime are difficult to obtain from conventional rock-deformation experiments, and previous results vary considerably. We demonstrate via nanoindentation that the strength of olivine in the low-temperature plasticity regime is dependent on the length-scale of the test, with experiments on smaller volumes of material exhibiting larger yield stresses. This "size effect" has previously been explained in engineering materials as a result of the role of strain gradients and associated geometrically necessary dislocations in modifying plastic behavior. The Hall-Petch effect, in which a material with a small grain size exhibits a higher strength than one with a large grain size, is thought to arise from the same mechanism. The presence of a size effect resolves discrepancies among previous experimental measurements of olivine, which were either conducted using indentation methods or were conducted on polycrystalline samples with small grain sizes. An analysis of different low-temperature plasticity flow laws extrapolated to room temperature reveals a power-law relationship between length-scale (grain size for polycrystalline deformation and contact radius for indentation tests) and yield strength. This suggests that data from samples with large inherent length scales best represent the plastic strength of the coarse-grained lithospheric mantle. Additionally, the plastic deformation of nanometer- to micrometer-sized asperities on fault surfaces may control the evolution of fault roughness due to their size-dependent strength.
NASA Astrophysics Data System (ADS)
Sakthiraj, K.; Hema, M.; Balachandra Kumar, K.
2018-06-01
In the present study, nanocrystalline tin oxide materials were prepared using sol-gel method with different reaction temperatures (25 °C, 50 °C, 75 °C & 90 °C) and the relation between the room temperature ferromagnetic property of the sample with processing temperature has been analysed. The X-ray diffraction pattern and infrared absorption spectra of the as-prepared samples confirm the purity of the samples. Transmission electron microscopy images visualize the particle size variation with respect to reaction temperature. The photoluminescence spectra of the samples demonstrate that luminescence process in materials is originated due to the electron transition mediated by defect centres. The room temperature ferromagnetic property is observed in all the samples with different amount, which was confirmed using vibrating sample magnetometer measurements. The saturation magnetization value of the as-prepared samples is increased with increasing the reaction temperature. From the photoluminescence & magnetic measurements we accomplished that, more amount of surface defects like oxygen vacancy and tin interstitial are created due to the increase in reaction temperature and it controls the ferromagnetic property of the samples.
NASA Astrophysics Data System (ADS)
Albab, Muh Fadhil; Yuwono, Akhmad Herman; Sofyan, Nofrijon; Ramahdita, Ghiska
2017-02-01
In the current study, hydroxyapatite (HA)/chitosan-based bone scaffold has been fabricated using Thermally Induced Phase Separation (TIPS) method under freezing temperature variation of -20, -30, -40 and -80 °C. The samples with weight percent ratio of 70% HA and 30% chitosan were homogeneously mixed and subsequently dissolved in 2% acetic acid. The synthesized samples were further characterized using Fourier transform infrared (FTIR), compressive test and scanning electron microscope (SEM). The investigation results showed that low freezing temperature reduced the pore size and increased the compressive strength of the scaffold. In the freezing temperature of -20 °C, the pore size was 133.93 µm with the compressive strength of 5.9 KPa, while for -80 °C, the pore size declined to 60.55 µm with the compressive strength 29.8 KPa. Considering the obtained characteristics, HA/chitosan obtained in this work has potential to be applied as a bone scaffold.
Dilution effects on ultrafine particle emissions from Euro 5 and Euro 6 diesel and gasoline vehicles
NASA Astrophysics Data System (ADS)
Louis, Cédric; Liu, Yao; Martinet, Simon; D'Anna, Barbara; Valiente, Alvaro Martinez; Boreave, Antoinette; R'Mili, Badr; Tassel, Patrick; Perret, Pascal; André, Michel
2017-11-01
Dilution and temperature used during sampling of vehicle exhaust can modify particle number concentration and size distribution. Two experiments were performed on a chassis dynamometer to assess exhaust dilution and temperature on particle number and particle size distribution for Euro 5 and Euro 6 vehicles. In the first experiment, the effects of dilution (ratio from 8 to 4 000) and temperature (ranging from 50 °C to 150 °C) on particle quantification were investigated directly from tailpipe for a diesel and a gasoline Euro 5 vehicles. In the second experiment, particle emissions from Euro 6 diesel and gasoline vehicles directly sampled from the tailpipe were compared to the constant volume sampling (CVS) measurements under similar sampling conditions. Low primary dilutions (3-5) induced an increase in particle number concentration by a factor of 2 compared to high primary dilutions (12-20). Low dilution temperatures (50 °C) induced 1.4-3 times higher particle number concentration than high dilution temperatures (150 °C). For the Euro 6 gasoline vehicle with direct injection, constant volume sampling (CVS) particle number concentrations were higher than after the tailpipe by a factor of 6, 80 and 22 for Artemis urban, road and motorway, respectively. For the same vehicle, particle size distribution measured after the tailpipe was centred on 10 nm, and particles were smaller than the ones measured after CVS that was centred between 50 nm and 70 nm. The high particle concentration (≈106 #/cm3) and the growth of diameter, measured in the CVS, highlighted aerosol transformations, such as nucleation, condensation and coagulation occurring in the sampling system and this might have biased the particle measurements.
Chakradhar, R P S; Basu, Bharathibai J; Lakshmi, R V
2011-02-01
Europium-doped rare-earth oxysulphides (red phosphors) are often used as reference luminophore in pyrene-based pressure sensor coatings for aerodynamic applications. Different red phosphor samples were characterized for their particle size, chemical composition, photoluminescent properties and temperature sensitivity. The red phosphor samples were characterized using energy-dispersive X-ray spectroscopy (EDX) for elemental analysis and scanning electron microscopy (SEM) for morphology and particle size measurement. The particle size was in the range of 1.5-5.7 μm with morphology of hexagonal or spherical shape. It was found that phosphor with higher europium content exhibited higher luminescent emission intensity. The phosphor coatings were prepared by spraying a dispersion of the material in silicone resin. Smooth coatings were obtained by using phosphor samples with smaller particle size. Upon 334 nm excitation, the coatings showed characteristic luminescence 5D0→7FJ (J=0, 1, 2, 3, 4) of the Eu3+ ions. The electronic transition located at 626 nm (5D0→7F2) of Eu3+ ions was stronger than the magnetic dipole transition located at 595 nm (5D0→7F1). Luminescence decay curves obeyed double exponential behaviour. The phosphor samples showed temperature sensitivity of -0.012 to -0.168%/°C in the temperature range of 25-50 °C. Copyright © 2010 Elsevier B.V. All rights reserved.
Liu, Zhi; Cheng, Buwen; Hu, Weixuan; Su, Shaojian; Li, Chuanbo; Wang, Qiming
2012-07-11
Four-bilayer Ge quantum dots (QDs) with Si spacers were grown on Si(001) substrates by ultrahigh vacuum chemical vapor deposition. In three samples, all Ge QDs were grown at 520 °C, while Si spacers were grown at various temperatures (520 °C, 550 °C, and 580 °C). Enhancement and redshift of room temperature photoluminescence (PL) were observed from the samples in which Si spacers were grown at a higher temperature. The enhancement of PL is explained by higher effective electrons capturing in the larger size Ge QDs. Quantum confinement of the Ge QDs is responsible for the redshift of PL spectra. The Ge QDs' size and content were investigated by atomic force microscopy and Raman scattering measurements.
Hoover, Kelli; Uzunovic, Adnan; Gething, Brad; Dale, Angela; Leung, Karen; Ostiguy, Nancy; Janowiak, John J.
2010-01-01
To reduce the risks associated with global transport of wood infested with pinewood nematode Bursaphelenchus xylophilus, microwave irradiation was tested at 14 temperatures in replicated wood samples to determine the temperature that would kill 99.9968% of nematodes in a sample of ≥ 100,000 organisms, meeting a level of efficacy of Probit 9. Treatment of these heavily infested wood samples (mean of > 1,000 nematodes/g of sapwood) produced 100% mortality at 56 °C and above, held for 1 min. Because this “brute force” approach to Probit 9 treats individual nematodes as the observational unit regardless of the number of wood samples it takes to treat this number of organisms, we also used a modeling approach. The best fit was to a Probit function, which estimated lethal temperature at 62.2 (95% confidence interval 59.0-70.0) °C. This discrepancy between the observed and predicted temperature to achieve Probit 9 efficacy may have been the result of an inherently limited sample size when predicting the true mean from the total population. The rate of temperature increase in the small wood samples (rise time) did not affect final nematode mortality at 56 °C. In addition, microwave treatment of industrial size, infested wood blocks killed 100% of > 200,000 nematodes at ≥ 56 °C held for 1 min in replicated wood samples. The 3rd-stage juvenile (J3) of the nematode, that is resistant to cold temperatures and desiccation, was abundant in our wood samples and did not show any resistance to microwave treatment. Regression analysis of internal wood temperatures as a function of surface temperature produced a regression equation that could be used with a relatively high degree of accuracy to predict internal wood temperatures, under the conditions of this study. These results provide strong evidence of the ability of microwave treatment to successfully eradicate B. xylophilus in infested wood at or above 56 °C held for 1 min. PMID:22736846
Grain size effect on the permittivity of La1.5Sr0.5NiO4 nanoparticles
NASA Astrophysics Data System (ADS)
Dang Thanh, Tran; Van Hong, Le
2009-09-01
Using the annealing at different temperatures the La1.5Sr0.5NiO4 ceramic samples with different mean grain size were manufactured. Mean grain size (
Large exchange bias effect in NiFe2O4/CoO nanocomposites
NASA Astrophysics Data System (ADS)
Mohan, Rajendra; Prasad Ghosh, Mritunjoy; Mukherjee, Samrat
2018-03-01
In this work, we report the exchange bias effect of NiFe2O4/CoO nanocomposites, synthesized via chemical co-precipitation method. Four samples of different particle size ranging from 4 nm to 31 nm were prepared with the annealing temperature varying from 200 °C to 800 °C. X-ray diffraction analysis of all the samples confirmed the presence of cubic spinel phase of Nickel ferrite along with CoO phase without trace of any impurity. Sizes of the particles were studied from transmission electron micrographs and were found to be in agreement with those estimated from x-ray diffraction. Field cooled (FC) hysteresis loops at 5 K revealed an exchange bias (HE) of 2.2 kOe for the sample heated at 200 °C which decreased with the increase of particle size. Exchange bias expectedly vanished at 300 K due to high thermal energy (kBT) and low effective surface anisotropy. M-T curves revealed a blocking temperature of 135 K for the sample with smaller particle size.
Temperature dependent surface and spectral modifications of nano V2O5 films
NASA Astrophysics Data System (ADS)
Manthrammel, M. Aslam; Fatehmulla, A.; Al-Dhafiri, A. M.; Alshammari, A. S.; Khan, Aslam
2017-03-01
Nanocrystalline V2O5 films have been deposited on glass substrates at 300°C substrate temperature using thermal evaporation technique and were subjected to thermal annealing at different temperatures 350, 400, and 550°C. X-ray diffraction (XRD) spectra exhibit sharper and broader characteristic peaks respectively indicating the rearrangement of nanocrystallite phases with annealing temperatures. Other phases of vanadium oxides started emerging with the rise in annealing temperature and the sample converted completely to VO2 (B) phase at 550°C annealing. FESEM images showed an increase in crystallite size with 350 and 400°C annealing temperatures followed by a decrease in crystallite size for the sample annealed at 550°C. Transmission spectra showed an initial redshift of the fundamental band edge with 350 and 400°C while a blue shift for the sample annealed at 550°C, which was in agreement with XRD and SEM results. The films exhibited smart window properties as well as nanorod growth at specific annealing temperatures. Apart from showing the PL and defect related peaks, PL studies also supported the observations made in the transmission spectra.
Magnetic study of Co-doped CdSe nanoparticles
NASA Astrophysics Data System (ADS)
Das, Sayantani; Banerjee, Sourish; Sinha, T. P.
2018-04-01
Cobalt (2 %, 5 % and 10 %) doped cadmium selenide (CdSe) nanoparticles have been synthesized by soft chemical route. The XRD pattern shows the cubic structure of the sample. Crystallization temperature of the samples is calculated using differential scanning calorimeter. The average particle size of all the samples is found to be ˜ 25 nm. Field dependent (M-H) and temperature dependent (M-T) magnetization explains the presence of ferromagnetic components in the samples at room temperature and low temperature. In order to estimate the antiferromagnetic coupling among the doped TM atoms, an M-T measurement at 500 Oe has been carried out under zero field cooled (ZFC) and field cooled (FC) conditions and Curie-Weiss temperature θ of the samples has been estimated from 1/χ vs T plots.
Structural properties and gas sensing behavior of sol-gel grown nanostructured zinc oxide
DOE Office of Scientific and Technical Information (OSTI.GOV)
Rajyaguru, Bhargav; Gadani, Keval; Kansara, S. B.
2016-05-06
In this communication, we report the results of the studies on structural properties and gas sensing behavior of nanostructured ZnO grown using acetone precursor based modified sol-gel technique. Final product of ZnO was sintered at different temperatures to vary the crystallite size while their structural properties have been studied using X-ray diffraction (XRD) measurement performed at room temperature. XRD results suggest the single phasic nature of all the samples and crystallite size increases from 11.53 to 20.96 nm with increase in sintering temperature. Gas sensing behavior has been studied for acetone gas which indicates that lower sintered samples are moremore » capable to sense the acetone gas and related mechanism has been discussed in the light of crystallite size, crystal boundary density, defect mechanism and possible chemical reaction between gas traces and various oxygen species.« less
NASA Astrophysics Data System (ADS)
El-Sayed, Karimat; Mohamed, Mohamed Bakr; Hamdy, Sh.; Ata-Allah, S. S.
2017-02-01
Nano-crystalline NiFe2O4 was synthesized by citrate and sol-gel methods at different annealing temperatures and the results were compared with a bulk sample prepared by ceramic method. The effect of methods of preparation and different annealing temperatures on the crystallize size, strain, bond lengths, bond angles, cations distribution and degree of inversions were investigated by X-ray powder diffraction, high resolution transmission electron microscope, Mössbauer effect spectrometer and vibrating sample magnetometer. The cations distributions were determined at both octahedral and tetrahedral sites using both Mössbauer effect spectroscopy and a modified Bertaut method using Rietveld method. The Mössbauer effect spectra showed a regular decrease in the hyperfine field with decreasing particle size. Saturation magnetization and coercivity are found to be affected by the particle size and the cations distribution.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pransisco, Prengki, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Shafie, Afza, E-mail: prengkipransisco@gmail.com, E-mail: afza@petronas.com.my; Guan, Beh Hoe, E-mail: beh.hoeguan@petronas.com.my
2014-10-24
This paper examines the effect of calcination process on the structural and magnetic properties material nanostructure composite of Ni{sub 0Ð}œ‡{sub 5}Zn{sub 0Ð}œ‡{sub 25}Cu{sub 0.25} Fe{sub 2}O{sub 4} ferrites. The samples were successfully prepared by sol-gel method at different calcination temperature, which are 600°C, 700°C, 800°C and 900°C. Morphological investigation, average crystallite size and microstructure of the material were examined by using X-ray diffraction (XRD) and confirmed by high resolution transmission electron microscope (HRTEM) and field emission scanning electron microscope (FESEM). The effects of calcination temperature on the magnetic properties were calculated by using vibrating sample magnetometer (VSM). The XRD resultmore » shows single-phase cubic spinel structure with interval average size 5.9-38 nm, and grain size microstructure of the material was increasing with temperature increases. The highest magnetization saturation was reached at a temperature 800°C with value 53.89 emu/g, and the value coercive force (Hc) was inversely with the grain size.« less
Size effect on atomic structure in low-dimensional Cu-Zr amorphous systems.
Zhang, W B; Liu, J; Lu, S H; Zhang, H; Wang, H; Wang, X D; Cao, Q P; Zhang, D X; Jiang, J Z
2017-08-04
The size effect on atomic structure of a Cu 64 Zr 36 amorphous system, including zero-dimensional small-size amorphous particles (SSAPs) and two-dimensional small-size amorphous films (SSAFs) together with bulk sample was investigated by molecular dynamics simulations. We revealed that sample size strongly affects local atomic structure in both Cu 64 Zr 36 SSAPs and SSAFs, which are composed of core and shell (surface) components. Compared with core component, the shell component of SSAPs has lower average coordination number and average bond length, higher degree of ordering, and lower packing density due to the segregation of Cu atoms on the shell of Cu 64 Zr 36 SSAPs. These atomic structure differences in SSAPs with various sizes result in different glass transition temperatures, in which the glass transition temperature for the shell component is found to be 577 K, which is much lower than 910 K for the core component. We further extended the size effect on the structure and glasses transition temperature to Cu 64 Zr 36 SSAFs, and revealed that the T g decreases when SSAFs becomes thinner due to the following factors: different dynamic motion (mean square displacement), different density of core and surface and Cu segregation on the surface of SSAFs. The obtained results here are different from the results for the size effect on atomic structure of nanometer-sized crystalline metallic alloys.
Reduction Behavior of Assmang and Comilog ore in the SiMn Process
NASA Astrophysics Data System (ADS)
Kim, Pyunghwa Peace; Holtan, Joakim; Tangstad, Merete
The reduction behavior of raw materials from Assmang and Comilog based charges were experimentally investigated with CO gas up to 1600 °C. Quartz, HC FeMn slag or limestone were added to Assmang or Comilog according to the SiMn production charge, and mass loss results were obtained by using a TGA furnace. The results showed that particle size, type of manganese ore and mixture have close relationship to the reduction behavior of raw materials during MnO and SiO2 reduction. The influence of particle size to mass loss was apparent when Assmang or Comilog was mixed with only coke (FeMn) while it became insignificant when quartz and HC FeMn slag (SiMn) were added. This implied that quartz and HC FeMn slag had favored the incipient slag formation regardless of particle size. This explained the similar mass loss tendencies of SiMn charge samples between 1200-1500 °C, contrary to FeMn charge samples where different particle sizes showed significant difference in mass loss. Also, while FeMn charge samples showed progressive mass loss, SiMn charge samples showed diminutive mass loss until 1500 °C. However, rapid mass losses were observed with SiMn charge samples in this study above 1500 °C, and they have occurred at different temperatures. This implied rapid reduction of MnO and SiO2 and the type of ore and addition of HC FeMn slag have significant influence determining these temperatures. The temperatures observed for the rapid mass loss were approximately 1503 °C (Quartz and HC FeMn slag addition in Assmang), 1543 °C (Quartz addition in Assmang) and 1580-1587 °C (Quartz and limestone addition in Comilog), respectively. These temperatures also showed indications of possible SiMn production at process temperatures lower than 1550 °C.
NASA Astrophysics Data System (ADS)
Kaiser, Michael; Grunwald, Dennis; Marhan, Sven; Poll, Christian; Bamminger, Chris; Ludwig, Bernard
2016-04-01
Potential increases in soil temperature due to climate change might result in intensified soil organic matter (SOM) decomposition and thus higher CO2 emissions. Management options to increase and stabilize SOM include the application of biochar. However, the effects of biochar amendments under elevated soil temperatures on SOM dynamics are largely unknown. The objective of this study was to analyze the effect of biochar application and elevated soil temperature on the amount and composition of OM associated with fractions of different turnover kinetics. Samples were taken from four treatments of the Hohenheim Climate Change Experiment with the factors temperature (ambient or elevated by 2.5 °C in 4 cm depth, six years before sampling) and biochar (control and 30 t / ha Miscanthus pyrolysis biochar, one year before sampling) in two depths (0 - 5 and 5 - 15 cm). Basal respiration and microbial biomass C were analyzed within an incubation experiment. Aggregate size-fractions were separated by wet-sieving and the free light, occluded light (oLF), and heavy fractions were isolated by density fractionation. All fractions were analyzed for organic C and δ13C as well as by infrared spectroscopy. Preliminary data suggest that biochar significantly increased basal respiration and that the microbial biomass C was significantly affected by elevated temperature. No biochar-C was found in the microbial biomass. Biochar and elevated temperature had only minor effects on the organic C associated with aggregate-size classes, although biochar was incorporated into all fractions already after one year of application. Biochar application significantly increased the organic C associated with oLF. In most samples affected by biochar, the proportion of C=O groups was significantly increased. The results suggest that already after one year, biochar-mineral interactions were formed leading to an aggregate occlusion of applied biochar. At least in the short-term, the effect of biochar on the amount and composition of OM associated with different aggregate-size and density fractions seem to be independent from soil temperature.
Microstructural Evaluation of Forging Parameters for Superalloy Disks
NASA Technical Reports Server (NTRS)
Falsey, John R.
2004-01-01
Forgings of nickel base superalloy were formed under several different strain rates and forging temperatures. Samples were taken from each forging condition to find the ASTM grain size, and the as large as grain (ALA). The specimens were mounted in bakelite, polished, etched and then optical microscopy was used to determine grain size. The specimens ASTM grain sizes from each forging condition were plotted against strain rate, forging temperature, and presoak time. Grain sizes increased with increasing forging temperature. Grain sizes also increased with decreasing strain rates and increasing forging presoak time. The ALA had been determined from each forging condition using the ASTM standard method. Each ALA was compared with the ASTM grain size of each forging condition to determine if the grain sizes were uniform or not. The forging condition of a strain rate of .03/sec and supersolvus heat treatment produced non uniform grains indicated by critical grain growth. Other anomalies are noted as well.
NASA Astrophysics Data System (ADS)
Pena, C. F.; Soffner, M. E.; Mansanares, A. M.; Sampaio, J. A.; Gandra, F. C. G.; da Silva, E. C.; Vargas, H.
2017-10-01
Nanoparticles of La0.67Ca0.33MnO3 were synthesized via the sol-gel method, thermally treated and characterized using X-ray diffraction, magnetization, electron spin resonance and magnetoacoustic experiments. The formation of the desired perovskite structure was verified and the average size of the nanoparticles was also determined. An increase of the particle size by rising the treatment temperature was observed. The Curie temperature and the isothermal entropy variation of the samples were obtained from the magnetization data. The isothermal entropy change, produced under the application of an external magnetic field, which expresses the magnetocaloric effect, became significantly larger for the samples treated at higher temperatures. These results are in good agreement with those obtained by magnetoacoustics, based on the direct and contactless measurement of the temperature change, validating the ability of the technique to study the magnetocaloric effect in reduced mass and nanoparticles samples.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Muhammed Shafi, P.; Chandra Bose, A., E-mail: acbose@nitt.edu
2015-05-15
Nanocrystalline tin oxide (SnO{sub 2}) powders with different grain size were prepared by chemical precipitation method. The reaction was carried out by varying the period of hydrolysis and the as-prepared samples were annealed at different temperatures. The samples were characterized using X-ray powder diffractometer and transmission electron microscopy. The microstrain and crystallite size were calculated for all the samples by using Williamson-Hall (W-H) models namely, isotropic strain model (ISM), anisotropic strain model (ASM) and uniform deformation energy density model (UDEDM). The morphology and particle size were determined using TEM micrographs. The directional dependant young’s modulus was modified as an equationmore » relating elastic compliances (s{sub ij}) and Miller indices of the lattice plane (hkl) for tetragonal crystal system and also the equation for elastic compliance in terms of stiffness constants was derived. The changes in crystallite size and microstrain due to lattice defects were observed while varying the hydrolysis time and the annealing temperature. The dependence of crystallite size on lattice strain was studied. The results were correlated with the available studies on electrical properties using impedance spectroscopy.« less
Temperature-dependent plastic hysteresis in highly confined polycrystalline Nb films
NASA Astrophysics Data System (ADS)
Waheed, S.; Hao, R.; Zheng, Z.; Wheeler, J. M.; Michler, J.; Balint, D. S.; Giuliani, F.
2018-02-01
In this study, the effect of temperature on the cyclic deformation behaviour of a confined polycrystalline Nb film is investigated. Micropillars encapsulating a thin niobium interlayer are deformed under cyclic axial compression at different test temperatures. A distinct plastic hysteresis is observed for samples tested at elevated temperatures, whereas negligible plastic hysteresis is observed for samples tested at room temperature. These results are interpreted using planar discrete dislocation plasticity incorporating slip transmission across grain boundaries. The effect of temperature-dependent grain boundary energy and dislocation mobility on dislocation penetration and, consequently, the size of plastic hysteresis is simulated to correlate with the experimental results. It is found that the decrease in grain boundary energy barrier caused by the increase in temperature does not lead to any appreciable change in the cyclic response. However, dislocation mobility significantly affects the size of plastic hysteresis, with high mobilities leading to a larger hysteresis. Therefore, it is postulated that the experimental observations are predominantly caused by an increase in dislocation mobility as the temperature is increased above the critical temperature of body-centred cubic niobium.
NASA Astrophysics Data System (ADS)
Zan, Jinbo; Fang, Xiaomin; Yan, Maodu; Shen, Miaomiao
2018-05-01
Hysteresis, thermomagnetic and low-temperature magnetic experiments on particle-size fractioned samples from the Chinese Loess Plateau (CLP) can be used to better characterize the magnetic mineralogy and magnetic granulometry of Chinese loess/paleosols. However, a systematic study of the grain-size-dependent magnetic mineralogy of the Central Asian loess deposits has not been undertaken. In this paper, four size fractions of seventeen loess and paleosol samples from Central Asia and the CLP were subjected to aforementioned rock magnetic measurements. Our findings are as follows: (1) In Central Asia, the fractionated samples from loess and paleosol couplets exhibit no obvious differences in their magnetic mineralogy due to weak pedogenesis. (2) Thermomagnetic analyses suggest that the content of maghemite in the clay fraction of paleosols from the CLP is one or two orders of magnitude larger than that of the loess samples from the CLP and Central Asia. This result does not support the view that maghemite in the loess/palaeosol sequences of the CLP originated mainly from eolian sources. (3) Both hysteresis and low-temperature magnetic experiments demonstrate that detrital ferrimagnetic grains are mostly enriched in the 20-75 μm fraction of loess/paleosols from Central Asia and the CLP. The relative paucity of coarser magnetic grains in the > 75 μm fractions indicate that a positive correlation does not always exist between the magnetic concentration parameters and the sedimentological particle size in Chinese loess deposits. (4) The regional variations in the magnetic properties of the 20-75 μm fraction suggest that the supply of clastic sediments is the main control on the magnetic properties of loess deposits in Central Asia.
Linking phytoplankton community metabolism to the individual size distribution.
Padfield, Daniel; Buckling, Angus; Warfield, Ruth; Lowe, Chris; Yvon-Durocher, Gabriel
2018-05-25
Quantifying variation in ecosystem metabolism is critical to predicting the impacts of environmental change on the carbon cycle. We used a metabolic scaling framework to investigate how body size and temperature influence phytoplankton community metabolism. We tested this framework using phytoplankton sampled from an outdoor mesocosm experiment, where communities had been either experimentally warmed (+ 4 °C) for 10 years or left at ambient temperature. Warmed and ambient phytoplankton communities differed substantially in their taxonomic composition and size structure. Despite this, the response of primary production and community respiration to long- and short-term warming could be estimated using a model that accounted for the size- and temperature dependence of individual metabolism, and the community abundance-body size distribution. This work demonstrates that the key metabolic fluxes that determine the carbon balance of planktonic ecosystems can be approximated using metabolic scaling theory, with knowledge of the individual size distribution and environmental temperature. © 2018 The Authors. Ecology Letters published by CNRS and John Wiley & Sons Ltd.
NASA Astrophysics Data System (ADS)
Dhama, Pallavi; Kumar, Aparabal; Banerji, P.
2018-04-01
In this paper, we explored the effect of sintering temperature on the microstructure, thermal and electrical properties of iodine doped indium selenide in the temperature range 300 - 700 K. Samples were prepared by a collaborative process of vacuum melting, ball milling and spark plasma sintering at 570 K, 630 K and 690 K. Single phase samples were obtained at higher sintering temperature as InSe is stable only at lower temperature. With increasing sintering temperature, densities of the samples were found to improve with larger grain size formation. Negative values of Seebeck coefficient were observed which indicates n-type carrier transport. Seebeck coefficient increases with sintering temperature and found to be the highest for the sample sintered at 690 K. Thermal conductivity found to be lower in the samples sintered at lower temperatures. The maximum thermoelectric figure of merit found to be ˜ 1 at 700 K due to the enhanced power factor as a result of improved microstructure.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Shanmugavel, T., E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Raj, S. Gokul, E-mail: gokulrajs@hotmail.com, E-mail: shanmugavelnano@gmail.com; Rajarajan, G.
2015-06-24
Combustion synthesis of single phase Nickel ferrite was successfully achieved at low temperature regime. The obtained powders were calcinated to increase the crystallinity and their characterization change due to calcinations is investigated in detail. Citric acid used as a chelating agent for the synthesis of nickel ferrite. Pure single phase nickel ferrites were found at this low temperature. The average crystalline sizes were measured by using powder XRD measurements. Surface morphology was investigated through Transmission Electron Microscope (TEM). Particle size calculated in XRD is compared with TEM results. Magnetic behaviour of the samples is analyzed by using Vibrating Sample Magnetometermore » (VSM). Saturation magnetization, coercivity and retentivity are measured and their results are discussed in detail.« less
Raman and dielectric studies of GdMnO3 bulk ceramics synthesized from nano powders
NASA Astrophysics Data System (ADS)
Samantaray, S.; Mishra, D. K.; Roul, B. K.
2017-05-01
Nanocrystalline GdMnO3 (GMO) powders has been synthesized by a simple chemical route i. e. pyrophoric reaction technique and then sintered in the form of bulk pellet at 850°C for 24 hours by adopting slow step sintering schedule. It is observed that by reducing the particles size, chemical route enhances the mixing process as well as decreasing the sintering temperature to get single phase material system in compared to the polycrystalline sample prepared directly from the micron sized commercial powder. Raman spectroscopic studies confirm that the sample is in single phase without any detectable impurity. Frequency dependent dielectric properties i.e., dielectric constant (K) and dielectric loss (tanδ) of GMO ceramics sintered at 850°C for 24 hours were studied at room temperature. The sample showed high K value (˜2736) in the frequency of 100 Hz at room temperature.
Measurements of Regolith Simulant Thermal Conductivity Under Asteroid and Mars Surface Conditions
NASA Astrophysics Data System (ADS)
Ryan, A. J.; Christensen, P. R.
2017-12-01
Laboratory measurements have been necessary to interpret thermal data of planetary surfaces for decades. We present a novel radiometric laboratory method to determine temperature-dependent thermal conductivity of complex regolith simulants under rough to high vacuum and across a wide range of temperatures. This method relies on radiometric temperature measurements instead of contact measurements, eliminating the need to disturb the sample with thermal probes. We intend to determine the conductivity of grains that are up to 2 cm in diameter and to parameterize the effects of angularity, sorting, layering, composition, and eventually cementation. We present the experimental data and model results for a suite of samples that were selected to isolate and address regolith physical parameters that affect bulk conductivity. Spherical glass beads of various sizes were used to measure the effect of size frequency distribution. Spherical beads of polypropylene and well-rounded quartz sand have respectively lower and higher solid phase thermal conductivities than the glass beads and thus provide the opportunity to test the sensitivity of bulk conductivity to differences in solid phase conductivity. Gas pressure in our asteroid experimental chambers is held at 10^-6 torr, which is sufficient to negate gas thermal conduction in even our coarsest of samples. On Mars, the atmospheric pressure is such that the mean free path of the gas molecules is comparable to the pore size for many regolith particulates. Thus, subtle variations in pore size and/or atmospheric pressure can produce large changes in bulk regolith conductivity. For each sample measured in our martian environmental chamber, we repeat thermal measurement runs at multiple pressures to observe this behavior. Finally, we present conductivity measurements of angular basaltic simulant that is physically analogous to sand and gravel that may be present on Bennu. This simulant was used for OSIRIS-REx TAGSAM Sample Return Arm engineering tests. We measure the original size frequency distribution as well as several sorted size fractions. These results will support the efforts of the OSIRIS-REx team in selecting a site on asteroid Bennu that is safe for the spacecraft and meets grain size requirements for sampling.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Bhagwat, Mahesh; Ramaswamy, Veda
Nanocrystalline zirconia powder with a fairly narrow particle size distribution has been synthesized by the amorphous citrate route. The sample obtained has a high BET surface area of 89 m{sup 2} g{sup -1}. Rietveld refinement of the powder X-ray diffraction (XRD) profile of the zirconia sample confirms stabilization of zirconia in the tetragonal phase with around 8% monoclinic impurity. The data show the presence of both anionic as well as cationic vacancies in the lattice. Crystallite size determined from XRD is 8 nm and is in close agreement with the particle size determined by TEM. The in situ high temperature-X-raymore » diffraction (HTXRD) study revealed high thermal stability of the mixture till around 1023 K after which the transformation of tetragonal phase into the monoclinic phase has been seen as a function of temperature till 1473 K. This transformation is accompanied by an increase in the crystallite size of the sample from 8 to 55 nm. The thermal expansion coefficients are 9.14 x 10{sup -6} K{sup -1} along 'a'- and 15.8 x 10{sup -6} K{sup -1} along 'c'-axis. The lattice thermal expansion coefficient in the temperature range 298-1623 K is 34.6 x 10{sup -6} K{sup -1}.« less
Size dependence of magnetorheological properties of cobalt ferrite ferrofluid
DOE Office of Scientific and Technical Information (OSTI.GOV)
Radhika, B.; Sahoo, Rasmita; Srinath, S., E-mail: srinath@uohyd.ac.in
2015-06-24
Cobalt Ferrite nanoparticles were synthesized using co-precipitation method at reaction temperatures of 40°C and 80°C. X-Ray diffraction studies confirm cubic phase formation. The average crystallite sizes were found to be ∼30nm and ∼48nm for 40°C sample and 80°C sample respectively. Magnetic properties measured using vibrating sample magnetometer show higher coercivety and magnetization for sample prepared at 80°C. Magnetorheological properties of CoFe2O4 ferrofluids were measured and studied.
Scaling ice microstructures from the laboratory to nature: cryo-EBSD on large samples.
NASA Astrophysics Data System (ADS)
Prior, David; Craw, Lisa; Kim, Daeyeong; Peyroux, Damian; Qi, Chao; Seidemann, Meike; Tooley, Lauren; Vaughan, Matthew; Wongpan, Pat
2017-04-01
Electron backscatter diffraction (EBSD) has extended significantly our ability to conduct detailed quantitative microstructural investigations of rocks, metals and ceramics. EBSD on ice was first developed in 2004. Techniques have improved significantly in the last decade and EBSD is now becoming more common in the microstructural analysis of ice. This is particularly true for laboratory-deformed ice where, in some cases, the fine grain sizes exclude the possibility of using a thin section of the ice. Having the orientations of all axes (rather than just the c-axis as in an optical method) yields important new information about ice microstructure. It is important to examine natural ice samples in the same way so that we can scale laboratory observations to nature. In the case of ice deformation, higher strain rates are used in the laboratory than those seen in nature. These are achieved by increasing stress and/or temperature and it is important to assess that the microstructures produced in the laboratory are comparable with those observed in nature. Natural ice samples are coarse grained. Glacier and ice sheet ice has a grain size from a few mm up to several cm. Sea and lake ice has grain sizes of a few cm to many metres. Thus extending EBSD analysis to larger sample sizes to include representative microstructures is needed. The chief impediments to working on large ice samples are sample exchange, limitations on stage motion and temperature control. Large ice samples cannot be transferred through a typical commercial cryo-transfer system that limits sample sizes. We transfer through a nitrogen glove box that encloses the main scanning electron microscope (SEM) door. The nitrogen atmosphere prevents the cold stage and the sample from becoming covered in frost. Having a long optimal working distance for EBSD (around 30mm for the Otago cryo-EBSD facility) , by moving the camera away from the pole piece, enables the stage to move without crashing into either the EBSD camera or the SEM pole piece (final lens). In theory a sample up to 100mm perpendicular to the tilt axis by 150mm parallel to the tilt axis can be analysed. In practice, the motion of our stage is restricted to maximum dimensions of 100 by 50mm by a conductive copper braid on our cold stage. Temperature control becomes harder as the samples become larger. If the samples become too warm then they will start to sublime and the quality of EBSD data will reduce. Large samples need to be relatively thin ( 5mm or less) so that conduction of heat to the cold stage is more effective at keeping the surface temperature low. In the Otago facility samples of up to 40mm by 40mm present little problem and can be analysed for several hours without significant sublimation. Larger samples need more care, e.g. fast sample transfer to keep the sample very cold. The largest samples we work on routinely are 40 by 60mm in size. We will show examples of EBSD data from glacial ice and sea ice from Antarctica and from large laboratory ice samples.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Correa, E. L., E-mail: eduardo.correa@usp.br; Bosch-Santos, B.; Cavalcante, F. H. M.
2016-05-15
The magnetic behavior of Gd{sub 2}O{sub 3} nanoparticles, produced by thermal decomposition method and subsequently annealed at different temperatures, was investigated by magnetization measurements and, at an atomic level, by perturbed γ − γ angular correlation (PAC) spectroscopy measuring hyperfine interactions at {sup 111}In({sup 111}Cd) probe nuclei. Nanoparticle structure, size and shape were characterized by X-ray diffraction (XRD) and Transmission Electron Microscopy (TEM). Magnetization measurements were carried out to characterize the paramagnetic behavior of the samples. XRD results show that all samples crystallize in the cubic-C form of the bixbyite structure with space group Ia3. TEM images showed that particlesmore » annealed at 873 K present particles with highly homogeneous sizes in the range from 5 nm to 10 nm and those annealed at 1273 K show particles with quite different sizes from 5 nm to 100 nm, with a wide size distribution. PAC and magnetization results show that samples annealed at 873 and 1273 K are paramagnetic. Magnetization measurements show no indication of blocking temperatures for all samples down to 2 K and the presence of antiferromagnetic correlations.« less
NASA Astrophysics Data System (ADS)
Rida, A.; Makke, A.; Rouhaud, E.; Micoulaut, M.
2017-10-01
We use molecular dynamics simulations to study the mechanical properties of a columnar nanocrystalline copper with a mean grain size between 8.91 nm and 24 nm. The used samples were generated by using a melting cooling method. These samples were submitted to uniaxial tensile test. The results reveal the presence of a critical mean grain size between 16 and 20 nm, where there is an inversion in the conventional Hall-Petch tendency. This inversion is illustrated by the increase of flow stress with the increase of the mean grain size. This transition is caused by shifting of the deformation mechanism from dislocations to a combination of grain boundaries sliding and dislocations. Moreover, the effect of temperature on the mechanical properties of nanocrystalline copper has been investigated. The results show a decrease of the flow stress and Young's modulus when the temperature increases.
Synthetic Conditions for High-Accuracy Size Control of PbS Quantum Dots.
Zhang, Jianbing; Crisp, Ryan W; Gao, Jianbo; Kroupa, Daniel M; Beard, Matthew C; Luther, Joseph M
2015-05-21
Decreasing the variability in quantum dot (QD) syntheses is desirable for better uniformity of samples for use in QD-based studies and applications. Here we report a highly reproducible linear relationship between the concentration of ligand (in this case oleic acid, OA) and the lowest energy exciton peak position (nm) of the resulting PbS QDs for various hot-injection temperatures. Thus, for a given injection temperature, the size of the PbS QD product is purely controlled by the amount of OA. We used this relationship to study PbS QD solar cells that are fabricated from the same size of PbS QDs but synthesized using four different injection temperatures: 95, 120, 150, and 185 °C. We find that the power conversion efficiency does not depend on injection temperature but that the V(oc) is higher for QDs synthesized at lower temperatures while the J(sc) is improved in higher temperature QDs.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Kaur, Manpreet, E-mail: manpreet.kaur@thapar.edu; Singh, Gaganjot; Bimbraw, Keshav
Nanostructured titania have been successfully synthesized by hydrolysis of alkoxide at calcination temperatures 500 °C, 600 °C and 700 °C. As the calcination temperature increases, alcohol washed samples show lesser rutile content as compared to water washed samples. Morphology and Particle sizes was determined by field emission scanning electron microscopy (FESEM), while thermogravimetric-differential scanning calorimetry (TG-DSC) was used to determine thermal stability. Alcohol washed samples undergo 30% weight loss whereas 16% in water washed samples was observed. The mean particle sizes were found to be increase from 37 nm to 100.9 nm and 35.3 nm to 55.2 nm for water and alcohol washed samplesmore » respectively. Hydrolysis of alkoxide was shown to be an effective means to prepare thermally stable titania by using alcohol washed samples as a precursor.« less
Bastistella, Luciane; Rousset, Patrick; Aviz, Antonio; Caldeira-Pires, Armando; Humbert, Gilles; Nogueira, Manoel
2018-02-09
New experimental techniques, as well as modern variants on known methods, have recently been employed to investigate the fundamental reactions underlying the oxidation of biochar. The purpose of this paper was to experimentally and statistically study how the relative humidity of air, mass, and particle size of four biochars influenced the adsorption of water and the increase in temperature. A random factorial design was employed using the intuitive statistical software Xlstat. A simple linear regression model and an analysis of variance with a pairwise comparison were performed. The experimental study was carried out on the wood of Quercus pubescens , Cyclobalanopsis glauca , Trigonostemon huangmosun , and Bambusa vulgaris , and involved five relative humidity conditions (22, 43, 75, 84, and 90%), two mass samples (0.1 and 1 g), and two particle sizes (powder and piece). Two response variables including water adsorption and temperature increase were analyzed and discussed. The temperature did not increase linearly with the adsorption of water. Temperature was modeled by nine explanatory variables, while water adsorption was modeled by eight. Five variables, including factors and their interactions, were found to be common to the two models. Sample mass and relative humidity influenced the two qualitative variables, while particle size and biochar type only influenced the temperature.
Kiełbasa, Anna; Walczyńska, Aleksandra; Fiałkowska, Edyta; Pajdak-Stós, Agnieszka; Kozłowski, Jan
2014-12-01
Temperature-Size Rule (TSR) is a phenotypic body size response of ectotherms to changing temperature. It is known from the laboratory studies, but seasonal patterns in the field were not studied so far. We examined the body size changes in time of rotifers inhabiting activated sludge. We hypothesize that temperature is the most influencing parameter in sludge environment, leading sludge rotifers to seasonally change their body size according to TSR, and that oxygen content also induces the size response. The presence of TSR in Lecane inermis rotifer was tested in a laboratory study with two temperature and two food-type treatments. The effect of interaction between temperature and food was significant; L. inermis followed TSR in one food type only. The seasonal variability in the body sizes of the rotifers L. inermis and Cephalodella gracilis was estimated by monthly sampling and analyzed by multiple regression, in relation to the sludge parameters selected as the most influential by multivariate analysis, and predicted to alter rotifer body size (temperature and oxygen). L. inermis varied significantly in size throughout the year, and this variability is explained by temperature as predicted by the TSR, but not by oxygen availability. C. gracilis also varied in size, though this variability was explained by both temperature and oxygen. We suggest that sludge age acts as a mortality factor in activated sludge. It may have a seasonal effect on the body size of L. inermis and modify a possible effect of oxygen. Activated sludge habitat is driven by both biological processes and human regulation, yet its resident organisms follow general evolutionary rule as they do in other biological systems. The interspecific response patterns differ, revealing the importance of taking species-specific properties into account. Our findings are applicable to sludge properties enhancement through optimizing the conditions for its biological component.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Jinlong, Lv, E-mail: ljlbuaa@126.com; State Key Lab of New Ceramic and Fine Processing, Tsinghua University, Beijing 100084; Tongxiang, Liang, E-mail: ljltsinghua@126.com
The nanocrystalline pure nickels with different grain orientations were fabricated by direct current electrodeposition process. The grain size slightly decreased with the increasing of electrodeposition solution temperature. However, grain orientation was affected significantly. Comparing with samples obtained at 50 °C and 80 °C, sample obtained at 20 °C had the strongest (111) orientation plane which increased electrochemical corrosion resistance of this sample. At the same time, the lowest (111) orientation plane deteriorated electrochemical corrosion resistance of sample obtained at 50 °C. - Graphical abstract: The increased electrodeposition temperature promoted slightly grain refinement. The grain orientation was affected significantly by electrodepositionmore » solution temperature. The (111) orientation plane of sample increased significantly corrosion resistance. Display Omitted.« less
Stress Dependence of Microstructures in Experimentally Deformed Calcite
NASA Astrophysics Data System (ADS)
Platt, J. P.; De Bresser, J. H. P.
2017-12-01
Measurements of dynamically recrystallized grain size (Dr), subgrain size (Sg), minimum bulge size (Blg), and the maximum scale length for surface-energy driven grain-boundary migration (γGBM) in experimentally deformed Cararra marble help define the dependence of these microstructural features on stress and temperature. Measurements were made optically on ultra-thin sections in order to allow these features to be defined during measurement on the basis of microstructural setting and geometry. Taken together with previously published data Dr defines a paleopiezometer with a stress exponent of -1.09. There is no discernible temperature dependence over the 500°C temperature range of the experiments. Recrystallization occured mainly by bulging and subgrain rotation, and the two processes operated together, so that it is not possible to separate grains nucleated by the two mechanisms. Sg and Dr measured in the same samples are closely similar in size, suggesting that new grains do not grow significantly after nucleation, and that subgrain size is likely to be the primary control on recrystallized grain size. Blg and γGBM measured on each sample define a relationship to stress with an exponent of approximately -1.6, which helps define the boundary in stress - grain-size space between a region of dominant strain-energy-driven grain-boundary migration at high stress, from a region of dominant surface-energy-driven grain-boundary migration at low stress.
NASA Astrophysics Data System (ADS)
Morozov, O.; Mats, O.; Mats, V.; Zhurba, V.; Khaimovich, P.
2018-01-01
The present article introduces the data of analysis of ranges of ion-implanted deuterium desorption from Zr-1% Nb alloy. The samples studied underwent plastic deformation, low temperature extrusion and electron irradiation. Plastic rolling of the samples at temperature ∼300 K resulted in plastic deformation with the degree of ε = 3.9 and the formation of nanostructural state with the average grain size of d = 61 nm. The high degree of defectiveness is shown in thermodesorption spectrum as an additional area of the deuterium desorption in the temperature ranges 650-850 K. The further processing of the sample (that had undergone plastic deformation by plastic rolling) with electron irradiation resulted in the reduction of the average grain size (58 nm) and an increase in borders concentration. As a result the amount of deuterium desorpted increased in the temperature ranges 650-900 K. In case of Zr-1% Nb samples deformed by extrusion the extension of desorption area is observed towards the temperature reduction down to 420 K. The formation of the phase state of deuterium solid solution in zirconium was not observed. The structural state behavior is a control factor in the process of deuterium thermodesorption spectrum structure formation with a fixed implanted deuterium dose (hydrogen diagnostics). It appears as additional temperature ranges of deuterium desorption depending on the type, character and defect content.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ghazanfari, Mohammad Reza, E-mail: Ghazanfari.mr@gmail.com; Amini, Rasool; Shams, Seyyedeh Fatemeh
Highlights: • MA samples show higher dielectric permittivity and Curie temperature. • In MA samples, dielectric loss is almost 27% less than conventional ones. • In MA samples, sintering time and temperature are lower than conventional ones. • In MA samples, particle morphology is more homogeneous conventional ones. • In MA samples, crystallite size is smaller conventional ones. - Abstract: In present work, in order to study the effects of synthesis techniques on dielectric properties, the BNBT lead-free piezoceramics with (Bi{sub 0.5}Na{sub 0.5}){sub 0.94}Ba{sub 0.06}TiO{sub 3} stoichiometry (called as BNBT6) were synthesized by mechanical alloying (MA) and conventional mixed oxidesmore » methods. The structural, microstructural, and dielectric properties were carried out by X-ray diffractometer (XRD), scanning electron microscope (SEM), and impedance analyzer LCR meter, respectively. Based on results, the density of MA samples is considerably higher than conventional samples owning to smaller particles size and more uniformity of particle shape of MA samples. Moreover, the dielectric properties of MA samples are comparatively improved in which the dielectric loss of these samples is almost 27% less than conventional ones. Furthermore, MA samples exhibit obviously higher dielectric permittivity and Curie temperature compared to the conventional samples.« less
NASA Astrophysics Data System (ADS)
Patel, N.; Mariazzi, S.; Toniutti, L.; Checchetto, R.; Miotello, A.; Dirè, S.; Brusa, R. S.
2007-09-01
Three series of silica thin films with thicknesses in the 300 nm range were deposited by spin coating on Si substrates using different compositions of the sol precursors. Film samples were thermally treated in static air at temperatures ranging from 300 to 900 °C. The effect of sol precursors and thermal treatment temperature on the film porosity was analysed by Fourier transform infrared (FTIR) spectroscopy, depth profiling with positron annihilation spectroscopy (DP-PAS) and the analysis of the capacitance-voltage (C-V) characteristic. The maximum of the total porosity was found to occur at a temperature of 600 °C when removal of porogen and OH groups was completed. Film densification due to the collapsing of the pores was observed after drying at 900 °C. DP-PAS provides evidence that the increase in the total porosity is related to a progressive increase in the pore size. The increase in the pore size never gives rise to the onset of connected porosity. In the silica film samples prepared using a low acidity sol precursor, the pore size is always lower than 1 nm. By increasing the acid catalyst ratio in the sol, larger pores are formed. Pores with size larger than 2.3 nm can be obtained by adding porogen to the sol. In each series of silica film samples the shift of the antisymmetric Si-O-Si transversal optical (TO3) mode upon thermal treatment correlates with a change of the pore size as evidenced by DP-PAS analysis. The pore microstructure of the three series of silica films is different at all the examined treatment temperatures and depends on the composition of the precursor sol.
2016-01-01
Physical stability of synthetic skin samples during their exposure to microwave heating was investigated to demonstrate the use of the metal-assisted and microwave-accelerated decrystallization (MAMAD) technique for potential biomedical applications. In this regard, optical microscopy and temperature measurements were employed for the qualitative and quantitative assessment of damage to synthetic skin samples during 20 s intermittent microwave heating using a monomode microwave source (at 8 GHz, 2–20 W) up to 120 s. The extent of damage to synthetic skin samples, assessed by the change in the surface area of skin samples, was negligible for microwave power of ≤7 W and more extensive damage (>50%) to skin samples occurred when exposed to >7 W at initial temperature range of 20–39 °C. The initial temperature of synthetic skin samples significantly affected the extent of change in temperature of synthetic skin samples during their exposure to microwave heating. The proof of principle use of the MAMAD technique was demonstrated for the decrystallization of a model biological crystal (l-alanine) placed under synthetic skin samples in the presence of gold nanoparticles. Our results showed that the size (initial size ∼850 μm) of l-alanine crystals can be reduced up to 60% in 120 s without damage to synthetic skin samples using the MAMAD technique. Finite-difference time-domain-based simulations of the electric field distribution of an 8 GHz monomode microwave radiation showed that synthetic skin samples are predicted to absorb ∼92.2% of the microwave radiation. PMID:27917407
NASA Astrophysics Data System (ADS)
Semiatin, S. L.; Shank, J. M.; Shiveley, A. R.; Saurber, W. M.; Gaussa, E. F.; Pilchak, A. L.
2014-12-01
The effect of subsolvus forging temperature and strain rate on the grain size developed during final supersolvus heat treatment (SSHT) of two powder-metallurgy, gamma-gamma prime superalloys, IN-100 and LSHR, was established. For this purpose, isothermal, hot compression tests were performed at temperatures ranging from 1144 K (871 °C) and 22 K (22 °C) below the respective gamma-prime solvus temperatures ( T γ') and strain rates between 0.0003 and 10 s-1. Deformed samples were then heat treated 20 K (20 °C) above the solvus for 1 h with selected additional samples exposed for shorter and longer times. For both alloys, the grain size developed during SSHT was in the range of 15 to 30 μm, except for those processing conditions consisting of pre-deformation at the highest temperature, i.e., T γ'—22 K ( T γ'—22 °C), and strain rates in the range of ~0.001 to 0.1 s-1. In these latter instances, the heat-treated grain size was approx. four times as large. The observations were interpreted in terms of the mechanisms of deformation during hot working and their effect on the driving forces for grain-boundary migration which controls the evolution of the gamma-grain size.
Mössbauer and magnetic studies of surfactant mediated Ca-Mg doped ferrihydrite nanoparticles.
Layek, Samar; Mohapatra, M; Anand, S; Verma, H C
2013-03-01
Ultrafine (2-5 nm) particles of amorphous Ca-Mg co-doped ferrihydrite have been synthesized by surfactant mediated co-precipitation method. The evolution of the amorphous ferrihydrite by Ca-Mg co-doping is quite different from our earlier investigations on individual doping of Ca and Mg. Amorphous phase of ferrihydrite for the present study has been confirmed by X-ray diffraction (XRD) and Mössbauer spectroscopy at room temperature and low temperatures (40 K and 20 K). Hematite nanoparticles with crystallite size about 8, 38 and 70 nm were obtained after annealing the as-prepared samples at 400, 600 and 800 degrees C respectively in air atmosphere. Superparamagnetism has been found in 8 nm sized hematite nanoparticles which has been confirmed from the magnetic hysteresis loop with zero remanent magnetization and coercive field and also from the superparamagnetic doublet of its room temperature Mössbauer spectrum. The magnetic properties of the 38 and 70 nm sized particles have been studied by room temperature magnetic hysteresis loop measurements and Mössbauer spectroscopy. The coercive field in these hematite nanoparticles increases with increasing particle size. Small amount of spinel MgFe2O4 phase has been detected in the 800 degrees C annealed sample.
NASA Astrophysics Data System (ADS)
Mathis, Urs; Mohr, Martin; Forss, Anna-Maria
Particle measurements were performed in the exhaust of five light-duty vehicles (Euro-3) at +23, -7, and -20 °C ambient temperatures. The characterization included measurements of particle number, active surface area, number size distribution, and mass size distribution. We investigated two port-injection spark-ignition (PISI) vehicles, a direct-injection spark-ignition (DISI) vehicle, a compressed ignition (CI) vehicle with diesel particle filter (DPF), and a CI vehicle without DPF. To minimize sampling effects, particles were directly sampled from the tailpipe with a novel porous tube diluter at controlled sampling parameters. The diluted exhaust was split into two branches to measure either all or only non-volatile particles. Effect of ambient temperature was investigated on particle emission for cold and warmed-up engine. For the gasoline vehicles and the CI vehicle with DPF, the main portion of particle emission was found in the first minutes of the driving cycle at cold engine start. The particle emission of the CI vehicle without DPF was hardly affected by cold engine start. For the PISI vehicles, particle number emissions were superproportionally increased in the diameter size range from 0.1 to 0.3 μm during cold start at low ambient temperature. Based on the particle mass size distribution, the DPF removed smaller particles ( dp<0.5μm) more efficiently than larger particles ( dp>0.5μm). No significant effect of ambient temperature was observed when the engine was warmed up. Peak emission of volatile nanoparticles only took place at specific conditions and was poorly repeatable. Nucleation of particles was predominately observed during or after strong acceleration at high speed and during regeneration of the DPF.
NASA Astrophysics Data System (ADS)
Singh, Dharmendra; Rao, P. Nageswara; Jayaganthan, R.
2013-08-01
The influence of rolling at liquid nitrogen temperature and annealing on the microstructure and mechanical properties of Al 5083 alloy was studied in this paper. Cryorolled samples of Al 5083 show significant improvements in strength and hardness. The ultimate tensile strength increases up to 340 MPa and 390 MPa for the 30% and 50% cryorolled samples, respectively. The cryorolled samples, with 30% and 50% reduction, were subjected to Charpy impact testing at various temperatures from -190°C to 100°C. It is observed that increasing the percentage of reduction of samples during cryorolling has significant effect on decreasing impact toughness at all temperatures by increasing yield strength and decreasing ductility. Annealing of samples after cryorolling shows remarkable increment in impact toughness through recovery and recrystallization. The average grain size of the 50% cryorolled sample (14 μm) after annealing at 350°C for 1 h is found to be finer than that of the 30% cryorolled sample (25 μm). The scanning electron microscopy (SEM) analysis of fractured surfaces shows a large-size dimpled morphology, resembling the ductile fracture mechanism in the starting material and fibrous structure with very fine dimples in cryorolled samples corresponding to the brittle fracture mechanism.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Salili, S.M.; School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, Tehran; Ataie, A., E-mail: aataie@ut.ac.ir
This research aimed to synthesize nanostructured strontium-doped lanthanum manganite, La{sub 0.8}Sr{sub 0.2}MnO{sub 3} (LSMO), with its Curie temperature (T{sub c}) adjusted to the therapeutic range, through a mechanothermal route. In order to investigate the effect of heat treatment temperature and duration on the resulting crystallite size, morphology, magnetic behavior and Curie temperature, the starting powder mixture was milled in a planetary ball mill before being subsequently heat treated at distinct temperatures for different time lengths. The composition, morphology, and magnetic behavior were characterized using X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopymore » (HRTEM), selected area electron diffraction (SAED) and vibrating sample magnetometer (VSM). In addition, magnetic properties were further investigated using an alternating current (AC) susceptometer and thermo-magnetic analyzer. 20 h of milling produced a crystallite size reduction leading to a decrease in the heat treatment temperature of LSMO synthesis to 800 °C. Moreover, SEM analysis has shown the morphology of a strong agglomeration of fine nanoparticles. HRTEM showed clear lattice fringes of high crystallinity. The mean crystallite and particle size of 20-hour milled sample heat treated at 1100 °C for 10 h are relatively 69 and 100 nm, respectively. The VSM data at room temperature, indicated a paramagnetic behavior for samples heat treated at 800 °C. However, by increasing heat treatment temperature to 1100 °C, LSMO indicates a ferromagnetic behavior with well-adjusted Curie temperature of 320 K, suitable for hyperthermia applications. Also, reentrant spin glass (RSG) behavior has been found in heat treated samples. The particles are coated with (3-aminopropyl) triethoxysilane (APTES) for biocompatibility purposes; Fourier transform infrared spectroscopy (FTIR) and thermo-gravimetric analysis (TGA) are used for further confirmation of APTES coating. - Highlights: • La{sub 0.8}Sr{sub 0.2}MnO{sub 3} nanoparticles were synthesized via a mechanothermal route. • We report a significant reduction in the heat treatment temperature. • The Curie temperature was tuned within the therapeutic range. • The particles were coated with (3-aminopropyl) triethoxysilane for biocompatibility purposes.« less
Aslan, O; Hamill, R M; Sweeney, T; Reardon, W; Mullen, A M
2009-01-01
It is essential to isolate high-quality DNA from muscle tissue for PCR-based applications in traceability of animal origin. We wished to examine the impact of cooking meat to a range of core temperatures on the quality and quantity of subsequently isolated genomic (specifically, nuclear) DNA. Triplicate steak samples were cooked in a water bath (100 degrees C) until their final internal temperature was 75, 80, 85, 90, 95, or 100 degrees C, and DNA was extracted. Deoxyribonucleic acid quantity was significantly reduced in cooked meat samples compared with raw (6.5 vs. 56.6 ng/microL; P < 0.001), but there was no relationship with cooking temperature. Quality (A(260)/A(280), i.e., absorbance at 260 and 280 nm) was also affected by cooking (P < 0.001). For all 3 genes, large PCR amplicons (product size >800 bp) were observed only when using DNA from raw meat and steak cooked to lower core temperatures. Small amplicons (<200 bp) were present for all core temperatures. Cooking meat to high temperatures thus resulted in a reduced overall yield and probable fragmentation of DNA to sizes less than 800 bp. Although nuclear DNA is preferable to mitochondrial DNA for food authentication, it is less abundant, and results suggest that analyses should be designed to use small amplicon sizes for meat cooked to high core temperatures.
NASA Astrophysics Data System (ADS)
Baaziz, H.; Tozri, A.; Dhahri, E.; Hlil, E. K.
2018-03-01
We have undertaken a systematic study of critical behavior in La0.67Sr0.33MnO3 nanoparticles, sintered at different temperatures (L6, L8, L10 and L12 sintered at 600 °C, 800 °C, 1000 °C, 1200 °C respectively), by magnetization measurements. The critical exponents are estimated by various techniques such as the Modified Arrott plot, Kouvel-Fisher plot and critical isotherm technique. Compared to standard models, the critical exponents are close to those expected by the Mean-field model (with β = 0.5 γ = 1, and δ = 3) for (L6, L8, and L10) samples and by the (3D) Heisenberg model (β = 0.365, γ = 1.336 and δ = 4.80) for L12 sample. We conclude that the reduction of grain size strongly influences the universality class.
Liu, Yuefeng; Luo, Jingjie; Shin, Yooleemi; Moldovan, Simona; Ersen, Ovidiu; Hébraud, Anne; Schlatter, Guy; Pham-Huu, Cuong; Meny, Christian
2016-01-01
Assemblies of nanoparticles are studied in many research fields from physics to medicine. However, as it is often difficult to produce mono-dispersed particles, investigating the key parameters enhancing their efficiency is blurred by wide size distributions. Indeed, near-field methods analyse a part of the sample that might not be representative of the full size distribution and macroscopic methods give average information including all particle sizes. Here, we introduce temperature differential ferromagnetic nuclear resonance spectra that allow sampling the crystallographic structure, the chemical composition and the chemical order of non-interacting ferromagnetic nanoparticles for specific size ranges within their size distribution. The method is applied to cobalt nanoparticles for catalysis and allows extracting the size effect from the crystallographic structure effect on their catalytic activity. It also allows sampling of the chemical composition and chemical order within the size distribution of alloyed nanoparticles and can thus be useful in many research fields. PMID:27156575
Effect of Co doping on the magnetic and DC electrical properties of Mn-Zn nanoferrites
NASA Astrophysics Data System (ADS)
Khandan Fadafan, H.; Lotfi Orimi, R.; Nezhadeini, S.
2018-06-01
In this study, Cobalt-Manganese-Zinc nanoferrites with the formula CoxMn0.5-xZn0.5Fe2O4 with x = 0.0, 0.1, 0.3, and 0.5 prepared by chemical Co-precipitation method. Then the structure and morphology of the synthesized nanoparticles were characterized by X-ray diffraction (XRD) and transmitting electron microscopy (TEM), respectively. The XRD patterns indicated the formation of single-phased cubic structure of spinel ferrite in nanometer size with no minor phase. The TEM image showed the formation of nanoparticles with average size of about 40 nm and normal size distribution. The magnetic measurements of the nanoparticles were done at room temperature using a vibrating sample magnetometer (VSM). Results exhibited a super-paramagnetic like behavior for some of the samples. DC electrical resistivity measurements were carried out by two-probe technique from 25 to 250 °C and showed decreasing of the resistivity with temperature meanwhile passing a transition to form of a peak. The peaks values observed near the Curie temperatures of samples suggest that anomaly behavior can attributed to spin canting associated with the phase transition from para to ferromagnetic state at TC.
Egarievwe, Stephen U.; Yang, Ge; Egarievwe, Alexander; ...
2015-02-11
Bridgman-grown cadmium zinc telluride (CdZnTe or CZT) and cadmium manganese telluride (CdMnTe or CMT) crystals often have Te inclusions that limit their performances as X-ray- and gamma-ray-detectors. We present here the results of post-growth thermal annealing aimed at reducing and eliminating Te inclusions in them. In a 2D analysis, we observed that the sizes of the Te inclusions declined to 92% during a 60-h annealing of CZT at 510 °C under Cd vapor. Further, tellurium inclusions were eliminated completely in CMT samples annealed at 570 °C in Cd vapor for 26 h, whilst their electrical resistivity fell by an ordermore » of 10 2. During the temperature-gradient annealing of CMT at 730 °C and an 18 °C/cm temperature gradient for 18 h in a vacuum of 10 -5 mbar, we observed the diffusion of Te from the sample, causing a reduction in size of the Te inclusions. For CZT samples annealed at 700 °C in a 10 °C/cm temperature gradient, we observed the migration of Te inclusions from a low-temperature region to a high one at 0.022 μm/s. During the temperature-gradient annealing of CZT in a vacuum of 10 -5 mbar at 570 °C and 30 °C/cm for 18 h, some Te inclusions moved toward the high-temperature side of the wafer, while other inclusions of the same size, i.e., 10 µm in diameter, remained in the same position. These results show that the migration, diffusion, and reaction of Te with Cd in the matrix of CZT- and CMT-wafers are complex phenomena that depend on certain conditions.« less
Nanophase Carbonates on Mars: Implications for Carbonate Formation and Habitability
NASA Technical Reports Server (NTRS)
Archer, P. Douglas, Jr.; Lauer, H. Vern; Ming, Douglas W.; Niles, Paul B.; Morris, Richard V.; Rampe, Elizabeth B.; Sutter, Brad
2014-01-01
Despite having an atmosphere composed primarily of CO2 and evidence for abundant water in the past, carbonate minerals have only been discovered in small amounts in martian dust [1], in outcrops of very limited extent [2, 3], in soils in the Northern Plains (the landing site of the 2007 Phoenix Mars Scout Mission) [4] and may have recently been detected in aeolian material and drilled and powdered sedimentary rock in Gale Crater (the Mars Science Laboratory [MSL] landing site) [5]. Thermal analysis of martian soils by instruments on Phoenix and MSL has demonstrated a release of CO2 at temperatures as low as 250-300 degC, much lower than the traditional decomposition temperatures of calcium or magnesium carbonates. Thermal decomposition temperature can depend on a number of factors such as instrument pressure and ramp rate, and sample particle size [6]. However, if the CO2 released at low temperatures is from carbonates, small particle size is the only effect that could have such a large impact on decomposition temperature, implying the presence of extremely fine-grained (i.e., "nanophase" or clay-sized) carbonates. We hypothesize that this lower temperature release is the signature of small particle-sized (clay-sized) carbonates formed by the weathering of primary minerals in dust or soils through interactions with atmospheric water and carbon dioxide and that this process may persist under current martian conditions. Preliminary work has shown that clay-sized carbonate grains can decompose at much lower temperatures than previously thought. The first work took carbonate, decomposed it to CaO, then flowed CO2 over these samples held at temperatures >100 degC to reform carbonates. Thermal analysis confirmed that carbonates were indeed formed and transmission electron microsopy was used to determine crystal sized were on the order of 10 nm. The next step used minerals such as diopside and wollastonite that were sealed in a glass tube with a CO2 and H2O source. After reacting these materials for a number of hours, thermal analysis demonstrated the formations of carbonates that decomposed at temperatures as low as 500 degC [7]. Further work is underway to carry out the weathering process under more Mars-like conditions (low pressure and low temperature) to determine if the carbonate decomposition temperature can be shifted to even lower temperatures, consistent with what has been detected by thermal analysis instruments on Mars.
A New Probe to Change Curie Temperature of PbTiO3 Sensors
NASA Technical Reports Server (NTRS)
Katiyar, R. S.; Jinfang, Meng
1997-01-01
High temperature Raman spectra of nanocrystalline Pb(0.8)Ba(0.2)TiO3, Pb(0.8)Sr(0.2) TiO3, Pb(0.8)La(0.2)TiO3 and Pb(0.8)Ba(0.2)TiO3, have been measured, as a function of particle size. There appears respectively a distinct temperature-induced soft mode phase transition in every sample whose Curie temperature can be determined from the mean-field theory. The detailed Curie temperature shift in modified PbTi03 ceramics by Ba, Sr, La, and Zr, has also been investigated as a function of particle size. This study will favor preparations of high efficiency PbTi03 sensors with an adjustable Curie temperature.
Molten salt synthesis of nanocrystalline phase of high dielectric constant material CaCu3Ti4O12.
Prakash, B Shri; Varma, K B R
2008-11-01
Nanocrystalline powders of giant dielectric constant material, CaCu3Ti4O12 (CCTO), have been prepared successfully by the molten salt synthesis (MSS) using KCl at 750 degrees C/10 h, which is significantly lower than the calcination temperature (approximately 1000 degrees C) that is employed to obtain phase pure CCTO in the conventional solid-state reaction route. The water washed molten salt synthesized powder, characterized by X-ray powder diffraction (XRD), Scanning electron microscopy (SEM), and Transmission electron microscopy (TEM) confirmed to be a phase pure CCTO associated with approximately 150 nm sized crystallites of nearly spherical shape. The decrease in the formation temperature/duration of CCTO in MSS method was attributed to an increase in the diffusion rate or a decrease in the diffusion length of reacting ions in the molten salt medium. As a consequence of liquid phase sintering, pellets of as-synthesized KCl containing CCTO powder exhibited higher sinterability and grain size than that of KCl free CCTO samples prepared by both MSS method and conventional solid-state reaction route. The grain size and the dielectric constant of KCl containing CCTO ceramics increased with increasing sintering temperature (900 degrees C-1050 degrees C). Indeed the dielectric constants of these ceramics were higher than that of KCl free CCTO samples prepared by both MSS method and those obtained via the solid-state reaction route and sintered at the same temperature. Internal barrier layer capacitance (IBLC) model was invoked to correlate the observed dielectric constant with the grain size in these samples.
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.
A cryogenic tensile testing apparatus for micro-samples cooled by miniature pulse tube cryocooler
NASA Astrophysics Data System (ADS)
Chen, L. B.; Liu, S. X.; Gu, K. X.; Zhou, Y.; Wang, J. J.
2015-12-01
This paper introduces a cryogenic tensile testing apparatus for micro-samples cooled by a miniature pulse tube cryocooler. At present, tensile tests are widely applied to measure the mechanical properties of materials; most of the cryogenic tensile testing apparatus are designed for samples with standard sizes, while for non-standard size samples, especially for microsamples, the tensile testing cannot be conducted. The general approach to cool down the specimens for tensile testing is by using of liquid nitrogen or liquid helium, which is not convenient: it is difficult to keep the temperature of the specimens at an arbitrary set point precisely, besides, in some occasions, liquid nitrogen, especially liquid helium, is not easily available. To overcome these limitations, a cryogenic tensile testing apparatus cooled by a high frequency pulse tube cryocooler has been designed, built and tested. The operating temperatures of the developed tensile testing apparatus cover from 20 K to room temperature with a controlling precision of ±10 mK. The apparatus configurations, the methods of operation and some cooling performance will be described in this paper.
Oillic, Samuel; Lemoine, Eric; Gros, Jean-Bernard; Kondjoyan, Alain
2011-07-01
Cooking loss kinetics were measured on cubes and parallelepipeds of beef Semimembranosus muscle ranging from 1 cm × 1 cm × 1 cm to 7 cm × 7 cm × 28 cm in size. The samples were water bath-heated at three different temperatures, i.e. 50°C, 70°C and 90°C, and for five different times. Temperatures were simulated to help interpret the results. Pre-freezing the sample, difference in ageing time, and in muscle fiber orientation had little influence on cooking losses. At longer treatment times, the effects of sample size disappeared and cooking losses depended only on the temperature. A selection of the tests was repeated on four other beef muscles and on veal, horse and lamb Semimembranosus muscle. Kinetics followed similar curves in all cases but resulted in different final water contents. The shape of the kinetics curves suggests first-order kinetics. Copyright © 2011 The American Meat Science Association. Published by Elsevier Ltd. All rights reserved.
Grindability and combustion behavior of coal and torrefied biomass blends.
Gil, M V; García, R; Pevida, C; Rubiera, F
2015-09-01
Biomass samples (pine, black poplar and chestnut woodchips) were torrefied to improve their grindability before being combusted in blends with coal. Torrefaction temperatures between 240 and 300 °C and residence times between 11 and 43 min were studied. The grindability of the torrefied biomass, evaluated from the particle size distribution of the ground sample, significantly improved compared to raw biomass. Higher temperatures increased the proportion of smaller-sized particles after grinding. Torrefied chestnut woodchips (280 °C, 22 min) showed the best grinding properties. This sample was blended with coal (5-55 wt.% biomass). The addition of torrefied biomass to coal up to 15 wt.% did not significantly increase the proportion of large-sized particles after grinding. No relevant differences in the burnout value were detected between the coal and coal/torrefied biomass blends due to the high reactivity of the coal. NO and SO2 emissions decreased as the percentage of torrefied biomass in the blend with coal increased. Copyright © 2015 Elsevier Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Lahiri, B. B.; Ranoo, Surojit; Muthukumaran, T.; Philip, John
2018-04-01
The effects of initial susceptibility and size polydispersity on magnetic hyperthermia efficiency in two water based ferrofluids containing phosphate and TMAOH coated superparamagnetic Fe3O4 nanoparticles were studied. Experiments were performed at a fixed frequency of 126 kHz on four different concentrations of both samples and under different external field amplitudes. It was observed that for field amplitudes beyond 45.0 kAm-1, the maximum temperature rise was in the vicinity of 42°C (hyperthermia limit) which indicated the suitability of the water based ferrofluids for hyperthermia applications. The maximum temperature rise and specific absorption rate were found to vary linearly with square of the applied field amplitudes, in accordance with theoretical predictions. It was further observed that for a fixed sample concentration, specific absorption rate was higher for the phosphate coated samples which was attributed to the higher initial static susceptibility and lower size polydispersity of phosphate coated Fe3O4.
Hoffmann, William D.; Kertesz, Vilmos; Srijanto, Bernadeta R.; ...
2017-02-20
The use of atomic force microscopy controlled nano-thermal analysis probes for reproducible spatially resolved thermally-assisted sampling of micrometer-sized areas (ca. 11 m 17 m wide 2.4 m deep) from relatively low number average molecular weight (M n < 3000) polydisperse thin films of poly(2-vinylpyridine) (P2VP) is presented. Following sampling, the nano-thermal analysis probes were moved up from the surface and the probe temperature ramped to liberate the sampled materials into the gas phase for atmospheric pressure chemical ionization and mass spectrometric analysis. Furthermore, the procedure and mechanism for material pickup, the sampling reproducibility and sampling size are discussed and themore » oligomer distribution information available from slow temperature ramps versus ballistic temperature jumps is presented. For the M n = 970 P2VP, the Mn and polydispersity index determined from the mass spectrometric data were in line with both the label values from the sample supplier and the value calculated from the simple infusion of a solution of polymer into the commercial atmospheric pressure chemical ionization source on this mass spectrometer. With a P2VP sample of higher Mn (M n = 2070 and 2970), intact oligomers were still observed (as high as m/z 2793 corresponding to the 26-mer), but a significant abundance of thermolysis products were also observed. In addition, the capability for confident identification of the individual oligomers by slowly ramping the probe temperature and collecting data dependent tandem mass spectra was also demonstrated. We also discuss the material type limits to the current sampling and analysis approach as well as possible improvements in nano-thermal analysis probe design to enable smaller area sampling and to enable controlled temperature ramps beyond the present upper limit of about 415°C.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Hoffmann, William D.; Kertesz, Vilmos; Srijanto, Bernadeta R.
The use of atomic force microscopy controlled nano-thermal analysis probes for reproducible spatially resolved thermally-assisted sampling of micrometer-sized areas (ca. 11 m 17 m wide 2.4 m deep) from relatively low number average molecular weight (M n < 3000) polydisperse thin films of poly(2-vinylpyridine) (P2VP) is presented. Following sampling, the nano-thermal analysis probes were moved up from the surface and the probe temperature ramped to liberate the sampled materials into the gas phase for atmospheric pressure chemical ionization and mass spectrometric analysis. Furthermore, the procedure and mechanism for material pickup, the sampling reproducibility and sampling size are discussed and themore » oligomer distribution information available from slow temperature ramps versus ballistic temperature jumps is presented. For the M n = 970 P2VP, the Mn and polydispersity index determined from the mass spectrometric data were in line with both the label values from the sample supplier and the value calculated from the simple infusion of a solution of polymer into the commercial atmospheric pressure chemical ionization source on this mass spectrometer. With a P2VP sample of higher Mn (M n = 2070 and 2970), intact oligomers were still observed (as high as m/z 2793 corresponding to the 26-mer), but a significant abundance of thermolysis products were also observed. In addition, the capability for confident identification of the individual oligomers by slowly ramping the probe temperature and collecting data dependent tandem mass spectra was also demonstrated. We also discuss the material type limits to the current sampling and analysis approach as well as possible improvements in nano-thermal analysis probe design to enable smaller area sampling and to enable controlled temperature ramps beyond the present upper limit of about 415°C.« less
Walczyńska, Aleksandra; Sobczyk, Łukasz
2017-09-01
The observation that ectotherm size decreases with increasing temperature (temperature-size rule; TSR) has been widely supported. This phenomenon intrigues researchers because neither its adaptive role nor the conditions under which it is realized are well defined. In light of recent theoretical and empirical studies, oxygen availability is an important candidate for understanding the adaptive role behind TSR. However, this hypothesis is still undervalued in TSR studies at the geographical level. We reanalyzed previously published data about the TSR pattern in diatoms sampled from Icelandic geothermal streams, which concluded that diatoms were an exception to the TSR. Our goal was to incorporate oxygen as a factor in the analysis and to examine whether this approach would change the results. Specifically, we expected that the strength of size response to cold temperatures would be different than the strength of response to hot temperatures, where the oxygen limitation is strongest. By conducting a regression analysis for size response at the community level, we found that diatoms from cold, well-oxygenated streams showed no size-to-temperature response, those from intermediate temperature and oxygen conditions showed reverse TSR, and diatoms from warm, poorly oxygenated streams showed significant TSR. We also distinguished the roles of oxygen and nutrition in TSR. Oxygen is a driving factor, while nutrition is an important factor that should be controlled for. Our results show that if the geographical or global patterns of TSR are to be understood, oxygen should be included in the studies. This argument is important especially for predicting the size response of ectotherms facing climate warming.
NASA Astrophysics Data System (ADS)
Abdallah, Hafiz M. I.; Moyo, Thomas; Ngema, Nokwanda
2015-11-01
Nanocrystalline Co0.5Ni05Fe2O4 ferrite with average crystallite size of 7.6 nm and lattice constant of 0.8372 nm was synthesized via a glycol-thermal process. The structure parameters and morphology of the as-synthesized sample and annealed samples were characterized by XRD, EDX, FTIR, HRSEM and HRTEM. The hyperfine interactions, iron distribution on the tetrahedral and octahedral sites for the as-synthesized sample and samples annealed at 500 °C were deduced by Mössbauer spectroscopy measurements at 300 K. The magnetization measurements for the as-synthesized and annealed samples (300-900 °C) were obtained by a vibrating sample magnetometer on a cryogen free measurement system at different isothermal temperatures (4-300 K) in external applied magnetic fields of ±5 T. The temperature dependence of the magnetic properties such as coercive field, saturation magnetization, remanent magnetization and squareness of hysteresis loops were investigated. The sample transformed from single-domain to multi-domain configuration at particle size of about 31 nm. At 300 K, the sample annealed at 700 °C exhibits a maximum coercivity. The as-prepared sample shows a substantial increase in coercivity from 0.182 kOe at 300 K to 6.018 kOe at 4 K.
NASA Astrophysics Data System (ADS)
Taer, E.; Kurniasih, B.; Sari, F. P.; Zulkifli, Taslim, R.; Sugianto, Purnama, A.; Apriwandi, Susanti, Y.
2018-02-01
The particle size analysis for supercapacitor carbon electrodes from rubber wood sawdust (SGKK) has been done successfully. The electrode particle size was reviewed against the properties such as density, degree of crystallinity, surface morphology and specific capacitance. The variations in particle size were made by different treatment on the grinding and sieving process. The sample particle size was distinguished as 53-100 µm for 20 h (SA), 38-53 µm for 20 h (SB) and < 38 µm with variations of grinding time for 40 h (SC) and 80 h (SD) respectively. All of the samples were activated by 0.4 M KOH solution. Carbon electrodes were carbonized at temperature of 600oC in N2 gas environment and then followed by CO2 gas activation at a temperature of 900oC for 2 h. The densities for each variation in the particle size were 1.034 g cm-3, 0.849 g cm-3, 0.892 g cm-3 and 0.982 g cm-3 respectively. The morphological study identified the distance between the particles more closely at 38-53 µm (SB) particle size. The electrochemical properties of supercapacitor cells have been investigated using electrochemical methods such as impedance spectroscopy and charge-discharge at constant current using Solatron 1280 tools. Electrochemical properties testing results have shown SB samples with a particle size of 38-53 µm produce supercapacitor cells with optimum capacitive performance.
A New On-the-Fly Sampling Method for Incoherent Inelastic Thermal Neutron Scattering Data in MCNP6
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pavlou, Andrew Theodore; Brown, Forrest B.; Ji, Wei
2014-09-02
At thermal energies, the scattering of neutrons in a system is complicated by the comparable velocities of the neutron and target, resulting in competing upscattering and downscattering events. The neutron wavelength is also similar in size to the target's interatomic spacing making the scattering process a quantum mechanical problem. Because of the complicated nature of scattering at low energies, the thermal data files in ACE format used in continuous-energy Monte Carlo codes are quite large { on the order of megabytes for a single temperature and material. In this paper, a new storage and sampling method is introduced that ismore » orders of magnitude less in size and is used to sample scattering parameters at any temperature on-the-fly. In addition to the reduction in storage, the need to pre-generate thermal scattering data tables at fine temperatures has been eliminated. This is advantageous for multiphysics simulations which may involve temperatures not known in advance. A new module was written for MCNP6 that bypasses the current S(α,β) table lookup in favor of the new format. The new on-the-fly sampling method was tested for graphite for two benchmark problems at ten temperatures: 1) an eigenvalue test with a fuel compact of uranium oxycarbide fuel homogenized into a graphite matrix, 2) a surface current test with a \\broomstick" problem with a monoenergetic point source. The largest eigenvalue difference was 152pcm for T= 1200K. For the temperatures and incident energies chosen for the broomstick problem, the secondary neutron spectrum showed good agreement with the traditional S(α,β) sampling method. These preliminary results show that sampling thermal scattering data on-the-fly is a viable option to eliminate both the storage burden of keeping thermal data at discrete temperatures and the need to know temperatures before simulation runtime.« less
Compact ultrahigh vacuum sample environments for x-ray nanobeam diffraction and imaging.
Evans, P G; Chahine, G; Grifone, R; Jacques, V L R; Spalenka, J W; Schülli, T U
2013-11-01
X-ray nanobeams present the opportunity to obtain structural insight in materials with small volumes or nanoscale heterogeneity. The effective spatial resolution of the information derived from nanobeam techniques depends on the stability and precision with which the relative position of the x-ray optics and sample can be controlled. Nanobeam techniques include diffraction, imaging, and coherent scattering, with applications throughout materials science and condensed matter physics. Sample positioning is a significant mechanical challenge for x-ray instrumentation providing vacuum or controlled gas environments at elevated temperatures. Such environments often have masses that are too large for nanopositioners capable of the required positional accuracy of the order of a small fraction of the x-ray spot size. Similarly, the need to place x-ray optics as close as 1 cm to the sample places a constraint on the overall size of the sample environment. We illustrate a solution to the mechanical challenge in which compact ion-pumped ultrahigh vacuum chambers with masses of 1-2 kg are integrated with nanopositioners. The overall size of the environment is sufficiently small to allow their use with zone-plate focusing optics. We describe the design of sample environments for elevated-temperature nanobeam diffraction experiments demonstrate in situ diffraction, reflectivity, and scanning nanobeam imaging of the ripening of Au crystallites on Si substrates.
Compact ultrahigh vacuum sample environments for x-ray nanobeam diffraction and imaging
NASA Astrophysics Data System (ADS)
Evans, P. G.; Chahine, G.; Grifone, R.; Jacques, V. L. R.; Spalenka, J. W.; Schülli, T. U.
2013-11-01
X-ray nanobeams present the opportunity to obtain structural insight in materials with small volumes or nanoscale heterogeneity. The effective spatial resolution of the information derived from nanobeam techniques depends on the stability and precision with which the relative position of the x-ray optics and sample can be controlled. Nanobeam techniques include diffraction, imaging, and coherent scattering, with applications throughout materials science and condensed matter physics. Sample positioning is a significant mechanical challenge for x-ray instrumentation providing vacuum or controlled gas environments at elevated temperatures. Such environments often have masses that are too large for nanopositioners capable of the required positional accuracy of the order of a small fraction of the x-ray spot size. Similarly, the need to place x-ray optics as close as 1 cm to the sample places a constraint on the overall size of the sample environment. We illustrate a solution to the mechanical challenge in which compact ion-pumped ultrahigh vacuum chambers with masses of 1-2 kg are integrated with nanopositioners. The overall size of the environment is sufficiently small to allow their use with zone-plate focusing optics. We describe the design of sample environments for elevated-temperature nanobeam diffraction experiments demonstrate in situ diffraction, reflectivity, and scanning nanobeam imaging of the ripening of Au crystallites on Si substrates.
Synthetic Conditions for High-Accuracy Size Control of PbS Quantum Dots
Zhang, Jianbing; Crisp, Ryan W.; Gao, Jianbo; ...
2015-05-04
Decreasing the variability in quantum dot (QD) syntheses is desirable for better uniformity of samples for use in QD-based studies and applications. Here we report a highly reproducible linear relationship between the concentration of ligand (in this case oleic acid, OA) and the lowest energy exciton peak position (nm) of the resulting PbS QDs for various hot-injection temperatures. Thus, for a given injection temperature, the size of the PbS QD product is purely controlled by the amount of OA. We used this relationship to study PbS QD solar cells that are fabricated from the same size of PbS QDs butmore » synthesized using four different injection temperatures: 95, 120, 150, and 185 °C. We find that the power conversion efficiency does not depend on injection temperature but that the V oc is higher for QDs synthesized at lower temperatures while the J sc is improved in higher temperature QDs.« less
NASA Astrophysics Data System (ADS)
Bramowicz, Miroslaw; Braic, Laurentiu; Azem, Funda Ak; Kulesza, Slawomir; Birlik, Isil; Vladescu, Alina
2016-08-01
This aim of this work is to establish a relationship between the surface morphology and mechanical properties of hydroxyapatite coatings prepared using RF magnetron sputtering at temperatures in the range from 400 to 800 °C. The topography of the samples was scanned using atomic force microscopy, and the obtained 3D maps were analyzed using fractal methods to derive the spatial characteristics of the surfaces. X-ray photoelectron spectroscopy revealed the strong influence of the deposition temperature on the Ca/P ratio in the growing films. The coatings deposited at 600-800 °C exhibited a Ca/P ratio between 1.63 and 1.69, close to the stoichiometric hydroxyapatite (Ca/P = 1.67), which is crucial for proper osseointegration. Fourier-transform infrared spectroscopy showed that the intensity of phosphate absorption bands increased with increasing substrate temperature. Each sample exhibited well defined and sharp hydroxyapatite band at 566 cm-1, although more pronounced for the coatings deposited above 500 °C. Both the hardness and elastic modulus of the coated samples decrease with increasing deposition temperature. The surface morphology strongly depends on the deposition temperature. The sample deposited at 400 °C exhibits circular cavities dug in an otherwise flat surface. At higher deposition temperatures, these cavities increase in size and start to overlap each other so that at 500 °C the surface is composed of closely packed peaks and ridges. At that point, the characteristics of the surface turns from the dominance of cavities to grains of similar size, and develops in a similar manner at higher temperatures.
Comparison of microstickies measurement methods. Part II, Results and discussion
Mahendra R. Doshi; Angeles Blanco; Carlos Negro; Concepcion Monte; Gilles M. Dorris; Carlos C. Castro; Axel Hamann; R. Daniel Haynes; Carl Houtman; Karen Scallon; Hans-Joachim Putz; Hans Johansson; R. A. Venditti; K. Copeland; H.-M. Chang
2003-01-01
In part I of the article we discussed sample preparation procedure and described various methods used for the measurement of microstickies. Some of the important features of different methods are highlighted in Table 1. Temperatures used in the measurement methods vary from room temperature in some cases, 45 °C to 65 °C in other cases. Sample size ranges from as low as...
Ecology and shell chemistry of Loxoconcha matagordensis
Cronin, T. M.; Kamiya, T.; Dwyer, G.S.; Belkin, H.; Vann, C.D.; Schwede, S.; Wagner, R.
2005-01-01
Studies of the seasonal ecology and shell chemistry of the ostracode Loxoconcha matagordensis and related species of Loxoconcha from regions off eastern North America reveal that shell size and trace elemental (Mg/Ca ratio) composition are useful in paleothermometry using fossil populations. Seasonal sampling of populations from Chesapeake Bay, augmented by samples from Florida Bay, indicate that shell size is inversely proportional to water temperature and that Mg/Ca ratios are positively correlated with the water temperature in which the adult carapace was secreted. Microprobe analyses of sectioned valves reveal intra-shell variability in Mg/Ca ratios but this does not strongly influence the utility of whole shell Mg/Ca analyses for paleoclimate application.
Creep of quartz by dislocation and grain boundary processes
NASA Astrophysics Data System (ADS)
Fukuda, J. I.; Holyoke, C. W., III; Kronenberg, A. K.
2015-12-01
Wet polycrystalline quartz aggregates deformed at temperatures T of 600°-900°C and strain rates of 10-4-10-6 s-1 at a confining pressure Pc of 1.5 GPa exhibit plasticity at low T, governed by dislocation glide and limited recovery, and grain size-sensitive creep at high T, governed by diffusion and sliding at grain boundaries. Quartz aggregates were HIP-synthesized, subjecting natural milky quartz powder to T=900°C and Pc=1.5 GPa, and grain sizes (2 to 25 mm) were varied by annealing at these conditions for up to 10 days. Infrared absorption spectra exhibit a broad OH band at 3400 cm-1 due to molecular water inclusions with a calculated OH content (~4000 ppm, H/106Si) that is unchanged by deformation. Rate-stepping experiments reveal different stress-strain rate functions at different temperatures and grain sizes, which correspond to differing stress-temperature sensitivities. At 600-700°C and grain sizes of 5-10 mm, flow law parameters compare favorably with those for basal plasticity and dislocation creep of wet quartzites (effective stress exponents n of 3 to 6 and activation enthalpy H* ~150 kJ/mol). Deformed samples show undulatory extinction, limited recrystallization, and c-axis maxima parallel to the shortening direction. Similarly fine-grained samples deformed at 800°-900°C exhibit flow parameters n=1.3-2.0 and H*=135-200 kJ/mol corresponding to grain size-sensitive Newtonian creep. Deformed samples show some undulatory extinction and grain sizes change by recrystallization; however, grain boundary deformation processes are indicated by the low value of n. Our experimental results for grain size-sensitive creep can be compared with models of grain boundary diffusion and grain boundary sliding using measured rates of silicon grain boundary diffusion. While many quartz mylonites show microstructural and textural evidence for dislocation creep, results for grain size-sensitive creep may apply to very fine-grained (<10 mm) quartz mylonites.
The effects of pore structure on the behavior of water in lignite coal and activated carbon.
Nwaka, Daniel; Tahmasebi, Arash; Tian, Lu; Yu, Jianglong
2016-09-01
The effects of physical structure (pore structure) on behavior of water in lignite coal and activated carbon (AC) samples were investigated by using Differential Scanning Calorimetry (DSC) and low-temperature X-ray diffraction (XRD) techniques. AC samples with different pore structures were prepared at 800°C in steam and the results were compared with that of parent lignite coal. The DSC results confirmed the presence of two types of freezable water that freeze at -8°C (free water) and -42°C (freezable bound water). A shift in peak position of free water (FW) towards lower temperature was observed in AC samples compared to the lignite coal with decreasing water loading. The amount of free water (FW) increased with increasing gasification conversion. The amounts of free and freezable bound water (FBW) in AC samples were calculated and correlated to pore volume and average pore size. The amount of FW in AC samples is well correlated to the pore volume and average pore size of the samples, while an opposite trend was observed for FBW. The low-temperature XRD analysis confirmed the existence of non-freezable water (NFW) in coal and AC with the boundary between the freezable and non-freezable water (NFW) determined. Copyright © 2016 Elsevier Inc. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Egarievwe, Stephen U.; Yang, Ge; Egarievwe, Alexander
Bridgman-grown cadmium zinc telluride (CdZnTe or CZT) and cadmium manganese telluride (CdMnTe or CMT) crystals often have Te inclusions that limit their performances as X-ray- and gamma-ray-detectors. We present here the results of post-growth thermal annealing aimed at reducing and eliminating Te inclusions in them. In a 2D analysis, we observed that the sizes of the Te inclusions declined to 92% during a 60-h annealing of CZT at 510 °C under Cd vapor. Further, tellurium inclusions were eliminated completely in CMT samples annealed at 570 °C in Cd vapor for 26 h, whilst their electrical resistivity fell by an ordermore » of 10 2. During the temperature-gradient annealing of CMT at 730 °C and an 18 °C/cm temperature gradient for 18 h in a vacuum of 10 -5 mbar, we observed the diffusion of Te from the sample, causing a reduction in size of the Te inclusions. For CZT samples annealed at 700 °C in a 10 °C/cm temperature gradient, we observed the migration of Te inclusions from a low-temperature region to a high one at 0.022 μm/s. During the temperature-gradient annealing of CZT in a vacuum of 10 -5 mbar at 570 °C and 30 °C/cm for 18 h, some Te inclusions moved toward the high-temperature side of the wafer, while other inclusions of the same size, i.e., 10 µm in diameter, remained in the same position. These results show that the migration, diffusion, and reaction of Te with Cd in the matrix of CZT- and CMT-wafers are complex phenomena that depend on certain conditions.« less
Stress dependence of microstructures in experimentally deformed calcite
NASA Astrophysics Data System (ADS)
Platt, John P.; De Bresser, J. H. P.
2017-12-01
Optical measurements of microstructural features in experimentally deformed Carrara marble help define their dependence on stress. These features include dynamically recrystallized grain size (Dr), subgrain size (Sg), minimum bulge size (Lρ), and the maximum scale length for surface-energy driven grain-boundary migration (Lγ). Taken together with previously published data Dr defines a paleopiezometer over the range 15-291 MPa and temperature over the range 500-1000 °C, with a stress exponent of -1.09 (CI -1.27 to -0.95), showing no detectable dependence on temperature. Sg and Dr measured in the same samples are closely similar in size, suggesting that the new grains did not grow significantly after nucleation. Lρ and Lγ measured on each sample define a relationship to stress with an exponent of approximately -1.6, which helps define the boundary between a region of dominant strain-energy-driven grain-boundary migration at high stress, from a region of dominant surface-energy-driven grain-boundary migration at low stress.
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.
Synthesis and characterization of nanocrystalline mesoporous zirconia using supercritical drying.
Tyagi, Beena; Sidhpuria, Kalpesh; Shaik, Basha; Jasra, Raksh Vir
2006-06-01
Synthesis of nano-crystalline zirconia aerogel was done by sol-gel technique and supercritical drying using n-propanol solvent at and above supercritical temperature (235-280 degrees C) and pressure (48-52 bar) of n-propanol. Zirconia xerogel samples have also been prepared by conventional thermal drying method to compare with the super critically dried samples. Crystalline phase, crystallite size, surface area, pore volume, and pore size distribution were determined for all the samples in detail to understand the effect of gel drying methods on these properties. Supercritical drying of zirconia gel was observed to give thermally stable, nano-crystalline, tetragonal zirconia aerogels having high specific surface area and porosity with narrow and uniform pore size distribution as compared to thermally dried zirconia. With supercritical drying, zirconia samples show the formation of only mesopores whereas in thermally dried samples, substantial amount of micropores are observed along with mesopores. The samples prepared using supercritical drying yield nano-crystalline zirconia with smaller crystallite size (4-6 nm) as compared to higher crystallite size (13-20 nm) observed with thermally dried zirconia.
Calibration of the clumped isotope thermometer for planktic foraminifers
NASA Astrophysics Data System (ADS)
Meinicke, N.; Ho, S. L.; Nürnberg, D.; Tripati, A. K.; Jansen, E.; Dokken, T.; Schiebel, R.; Meckler, A. N.
2017-12-01
Many proxies for past ocean temperature suffer from secondary influences or require species-specific calibrations that might not be applicable on longer time scales. Being thermodynamically based and thus independent of seawater composition, clumped isotopes in carbonates (Δ47) have the potential to circumvent such issues affecting other proxies and provide reliable temperature reconstructions far back in time and in unknown settings. Although foraminifers are commonly used for paleoclimate reconstructions, their use for clumped isotope thermometry has been hindered so far by large sample-size requirements. Existing calibration studies suggest that data from a variety of foraminifer species agree with synthetic carbonate calibrations (Tripati, et al., GCA, 2010; Grauel, et al., GCA, 2013). However, these studies did not include a sufficient number of samples to fully assess the existence of species-specific effects, and data coverage was especially sparse in the low temperature range (<10 °C). To expand the calibration database of clumped isotopes in planktic foraminifers, especially for colder temperatures (<10°C), we present new Δ47 data analysed on 14 species of planktic foraminifers from 13 sites, covering a temperature range of 1-29 °C. Our method allows for analysis of smaller sample sizes (3-5 mg), hence also the measurement of multiple species from the same samples. We analyzed surface-dwelling ( 0-50 m) species and deep-dwelling (habitat depth up to several hundred meters) planktic foraminifers from the same sites to evaluate species-specific effects and to assess the feasibility of temperature reconstructions for different water depths. We also assess the effects of different techniques in estimating foraminifer calcification temperature on the calibration. Finally, we compare our calibration to existing clumped isotope calibrations. Our results confirm previous findings that indicate no species-specific effects on the Δ47-temperature relationship measured in planktic foraminifers.
Laboratory evaluation of the Sequoia Scientific LISST-ABS acoustic backscatter sediment sensor
Snazelle, Teri T.
2017-12-18
Sequoia Scientific’s LISST-ABS is an acoustic backscatter sensor designed to measure suspended-sediment concentration at a point source. Three LISST-ABS were evaluated at the U.S. Geological Survey (USGS) Hydrologic Instrumentation Facility (HIF). Serial numbers 6010, 6039, and 6058 were assessed for accuracy in solutions with varying particle-size distributions and for the effect of temperature on sensor accuracy. Certified sediment samples composed of different ranges of particle size were purchased from Powder Technology Inc. These sediment samples were 30–80-micron (µm) Arizona Test Dust; less than 22-µm ISO 12103-1, A1 Ultrafine Test Dust; and 149-µm MIL-STD 810E Silica Dust. The sensor was able to accurately measure suspended-sediment concentration when calibrated with sediment of the same particle-size distribution as the measured. Overall testing demonstrated that sensors calibrated with finer sized sediments overdetect sediment concentrations with coarser sized sediments, and sensors calibrated with coarser sized sediments do not detect increases in sediment concentrations from small and fine sediments. These test results are not unexpected for an acoustic-backscatter device and stress the need for using accurate site-specific particle-size distributions during sensor calibration. When calibrated for ultrafine dust with a less than 22-µm particle size (silt) and with the Arizona Test Dust with a 30–80-µm range, the data from sensor 6039 were biased high when fractions of the coarser (149-µm) Silica Dust were added. Data from sensor 6058 showed similar results with an elevated response to coarser material when calibrated with a finer particle-size distribution and a lack of detection when subjected to finer particle-size sediment. Sensor 6010 was also tested for the effect of dissimilar particle size during the calibration and showed little effect. Subsequent testing revealed problems with this sensor, including an inadequate temperature compensation, making this data questionable. The sensor was replaced by Sequoia Scientific with serial number 6039. Results from the extended temperature testing showed proper temperature compensation for sensor 6039, and results from the dissimilar calibration/testing particle-size distribution closely corroborated the results from sensor 6058.
NASA Astrophysics Data System (ADS)
Teimouri, M.; Godfrey, A.
2017-07-01
Samples of a model dual-phase system, consisting of copper and AISI-420 martensitic steel have been synthesized using spark plasma sintering, with the objective of developing a microstructural analogue for dual-phase steels, in which the volume fraction and size of each phase can be controlled independently. Microstructural investigation of the samples, including fractography of samples deformed in tension until failure, show that densification is strongly temperature dependent. Samples sintered at temperatures of 900 °C or above at a pressure of 60 MPa show a density of more than 98%. The best mechanical properties, in terms of ultimate tensile strength and ductility is found in samples sintered at a temperature of 1000 °C, where a density of nearly 99% is achieved.
NASA Astrophysics Data System (ADS)
Li, Liang-Liang; Qin, Xiao-Ying; Liu, Yong-Fei; Liu, Quan-Zhen
2015-06-01
(Sr0.95Gd0.05)TiO3 (SGTO) ceramics are successfully prepared via spark plasma sintering (SPS) respectively at 1548, 1648, and 1748 K by using submicron-sized SGTO powders synthesized from a sol-gel method. The densities, microstructures, and thermoelectric properties of the SGTO ceramics are studied. Though the Seebeck coefficient shows no obvious difference in the case that SPS temperatures range from 1548 K to 1648 K, the electrical conductivity and the thermal conductivity increase remarkably due to the increase in grain size and density. The sample has a density higher than 98% theoretical density as the sintering temperature increases up to 1648 K and shows average grain sizes increasing from ˜ 0.7 μm to 7 μm until 1748 K. As a result, the maximum of the dimensionless figure of merit of ˜ 0.24 is achieved at ˜ 1000 K for the samples sintered at 1648 K and 1748 K, which was ˜ 71% larger than that (0.14 at ˜ 1000 K) for the sample sintered at 1548 K due to the enhancement of the power factor. Project supported by the National Natural Science Foundation of China (Grant Nos. 11174292, 51101150, and 11374306).
Shrimpton, J.M.; Zydlewski, Joseph D.; Heath, J.W.
2007-01-01
We examined the effect of temperature oscillation and increased suspended sediment concentration on growth and smolting in juvenile ocean-type chinook salmon (Oncorhynchus tshawytscha). Fish were ponded on February 26; each treatment group had three replicates of 250 fish. Mean temperatures for the entire experiment were 12.3????C for all tanks with a total of 1348 and 1341 degree days for the constant temperature and oscillating temperature tanks, respectively. Daily fluctuation in temperature averaged 7.5????C in the variable temperature groups and less than 1????C for the constant temperature group. Starting on April 5, bentonite clay was added each day to tanks as a pulse event to achieve a suspended sediment concentration of 200??mg l- 1; clay cleared from the tanks within approximately 8??h. Fish were sampled at approximately two??week intervals from ponding until mid-June. On the last sample date, June 12, a single gill arch was removed and fixed for histological examination of gill morphology. By early May, significant differences were seen in size between the groups; control > temperature = sediment > (temperature ?? sediment). This relationship was consistent throughout the experiment except for the last sample date when the temperature group had a mean weight significantly greater than the sediment group. Gill Na+,K+-ATPase activity was not affected by daily temperature oscillations, but groups subjected to increased suspended sediment had significantly lower enzyme activities compared to controls. Mean cell size for gill chloride cells did not differ between groups. Plasma cortisol increased significantly during the spring, but there were no significant differences between groups. ?? 2007 Elsevier B.V. All rights reserved.
Influence of Temperature and Grain Size on Austenite Stability in Medium Manganese Steels
NASA Astrophysics Data System (ADS)
Zhang, Yulong; Wang, Li; Findley, Kip O.; Speer, John G.
2017-05-01
With an aim to elucidate the influence of temperature and grain size on austenite stability, a commercial cold-rolled 7Mn steel was annealed at 893 K (620 °C) for times varying between 3 minutes and 96 hours to develop different grain sizes. The austenite fraction after 3 minutes was 34.7 vol pct, and at longer times was around 40 pct. An elongated microstructure was retained after shorter annealing times while other conditions exhibited equiaxed ferrite and austenite grains. All conditions exhibit similar temperature dependence of mechanical properties. With increasing test temperature, the yield and tensile strength decrease gradually, while the uniform and total elongation increase, followed by an abrupt drop in strength and ductility at 393 K (120 °C). The Olson-Cohen model was applied to fit the transformed austenite fractions for strained tensile samples, measured by means of XRD. The fit results indicate that the parameters α and β decrease with increasing test temperature, consistent with increased austenite stability. The 7Mn steels exhibit a distinct temperature dependence of the work hardening rate. Optimized austenite stability provides continuous work hardening in the temperature range of 298 K to 353 K (25 °C to 80 °C). The yield and tensile strengths have a strong dependence on grain size, although grain size variations have less effect on uniform and total elongation.
NASA Astrophysics Data System (ADS)
Beheshti, M.; Zabihiazadboni, M.; Ismail, M. C.; Kakooei, S.; Shahrestani, S.
2018-03-01
Optimal conditions to increase life time of casting parts have been investigated by applying various cycles of heat treatment and shot peening on Hadfield steel surface. Metallographic and SEM microstructure examinations were used to determine the effects of shot peen, austenitizing time and temperature simultaneously. The results showed that with increasing austenitizing time and temperature of casting sample, carbides resolved in austenite phase and by further increase of austenitizing temperature and time, the austenite grain size becomes larger. Metallographic images illustrated that shot peening on Hadfield steel surface; Austenite - Martensite transformation has not occurred, but its matrix hardened through twining formation process.
Effect of annealing temperature on titania nanoparticles
DOE Office of Scientific and Technical Information (OSTI.GOV)
Manikandan, K., E-mail: sanjaymani367@gmail.com; Arumugam, S., E-mail: sanjaymani367@gmail.com; Chandrasekaran, G.
2014-04-24
Titania polycrystalline samples are prepared by using sol-gel route hydrolyzing a alkoxide titanium precursor under acidic conditions. The as prepared samples are treated with different calcination temperatures. The anatase phase of titania forms when treated below 600°C, above that temperature the anatase phase tends to transform into the rutile phase of titania. The experimental determination of average grain size, phase formation, lattice parameters and the crystal structures of titania samples at different calcinations is done using X-ray diffraction (XRD). Fourier Transform Infra-red Spectroscopy (FTIR), UV-vis-NIR spectroscopy and Scanning Electron Microscopy (SEM) and Energy Dispersive Analysis X-ray are used to characterizemore » the samples to bring impact on the respective properties.« less
NASA Astrophysics Data System (ADS)
Khanal, Lokendra Raj; Williams, Thomas; Qiang, You
2018-06-01
Iron/iron-oxide (Fe–Fe3O4) core–shell nanoclusters (NCs) synthesized by a cluster deposition technique were subjected to a study of their high temperature structural and morphological behavior. Annealing effects have been investigated up to 800 °C in vacuum, oxygen and argon environments. The ~18 nm average size of the as-prepared NCs increases slowly in temperatures up to 500 °C in all three environments. The size increases abruptly in the argon environment but slowly in vacuum and oxygen when annealed at 800 °C. The x-ray diffraction (XRD) studies have shown that the iron core remains in the core–shell NCs only when they were annealed in the vacuum. A dramatic change in the surface morphology, an island like structure and/or a network like pattern, was observed at the elevated temperature. The as-prepared and annealed samples were analyzed using XRD, scanning electron microscopy and imageJ software for a close inspection of the temperature aroused properties. This work presents the temperature induced size growth mechanism, oxidation kinetics and phase transformation of the NCs accompanied by cluster aggregation, particle coalescence, and diffusion.
Optical properties of self-assembled ZnTe quantum dots grown by molecular-beam epitaxy
DOE Office of Scientific and Technical Information (OSTI.GOV)
Yang, C.S.; Lai, Y.J.; Chou, W.C.
2005-02-01
The morphology and the size-dependent photoluminescence (PL) spectra of the type-II ZnTe quantum dots (QDs) grown in a ZnSe matrix were obtained. The coverage of ZnTe varied from 2.5 to 3.5 monolayers (MLs). The PL peak energy decreased as the dot size increased. Excitation power and temperature-dependent PL spectra are used to characterize the optical properties of the ZnTe quantum dots. For 2.5- and 3.0-ML samples, the PL peak energy decreased monotonically as the temperature increased. However, for the 3.5-ML sample, the PL peak energy was initially blueshifted and then redshifted as the temperature increased above 40 K. Carrier thermalizationmore » and carrier transfer between QDs are used to explain the experimental data. A model of temperature-dependent linewidth broadening is employed to fit the high-temperature data. The activation energy, which was found by the simple PL intensity quenching model, of the 2.5, 3.0, and 3.5 MLs were determined to be 6.35, 9.40, and 18.87 meV, respectively.« less
NASA Astrophysics Data System (ADS)
Christen, Hans M.; Ohkubo, Isao; Rouleau, Christopher M.; Jellison, Gerald E., Jr.; Puretzky, Alex A.; Geohegan, David B.; Lowndes, Douglas H.
2005-01-01
Parallel (multi-sample) approaches, such as discrete combinatorial synthesis or continuous compositional-spread (CCS), can significantly increase the rate of materials discovery and process optimization. Here we review our generalized CCS method, based on pulsed-laser deposition, in which the synchronization between laser firing and substrate translation (behind a fixed slit aperture) yields the desired variations of composition and thickness. In situ alloying makes this approach applicable to the non-equilibrium synthesis of metastable phases. Deposition on a heater plate with a controlled spatial temperature variation can additionally be used for growth-temperature-dependence studies. Composition and temperature variations are controlled on length scales large enough to yield sample sizes sufficient for conventional characterization techniques (such as temperature-dependent measurements of resistivity or magnetic properties). This technique has been applied to various experimental studies, and we present here the results for the growth of electro-optic materials (SrxBa1-xNb2O6) and magnetic perovskites (Sr1-xCaxRuO3), and discuss the application to the understanding and optimization of catalysts used in the synthesis of dense forests of carbon nanotubes.
NASA Technical Reports Server (NTRS)
Archer, P. Douglas, Jr.; Niles, Paul B.; Ming, Douglas W.; Sutter, Brad; Eigenbrode, Jen
2015-01-01
Evolved Gas Analysis (EGA), which involves heating a sample and monitoring the gases released, has been performed on Mars by the Viking gas chromatography/mass spectrometry instruments, the Thermal and Evolved Gas Analyzer (TEGA) on the Phoenix lander, and the Sample Analysis at Mars (SAM) instrument on the Mars Science Laboratory. All of these instruments detected CO2 released during sample analysis at abundances of approx. 0.1 to 5 wt% assuming a carbonate source. The source of the CO2 can be constrained by evaluating the temperature of the gas release, a capability of both the TEGA and SAM instruments. The samples analyzed by SAM show that the majority of the CO2 is released below 400C, much lower than traditional carbonate decomposition temperatures which can be as low as 400C for some siderites, with magnesites and calcites decomposing at even higher temperatures. In addition to mineralogy, decomposition temperature can depend on particle size (among other factors). If carbonates formed on Mars under low temperature and relative humidity conditions, the resulting small particle size (nanophase) carbonates could have low decomposition temperatures. We have found that calcite can be synthesized by exposing CaO to water vapor and CO2 and that the resulting mineral has an EGA peak of approx. 550C for CO2, which is about 200C lower than for other calcites. Work is ongoing to produce Fe and Mg-bearing carbonates using the same process. Current results suggest that nanophase calcium carbonates cannot explain the CO2 released from martian samples. If the decomposition temperatures of Mg and Fe-bearing nanophase carbonates are not significantly lower than 400C, other candidate sources include oxalates and carboxylated organic molecules. If present, the abundance of organic carbon in these samples could be greater than 0.1 wt % (1000s of ppm), a signficant departure from the paradigm of the organic-poor Mars based on Viking results.
Magnetic behaviors of cataclasites within Wenchuan earthquake fault zone in heating experiments
NASA Astrophysics Data System (ADS)
Zhang, L.; Li, H.; Sun, Z.; Chou, Y. M.; Cao, Y., Jr.; Huan, W.; Ye, X.; He, X.
2017-12-01
Previous rock magnetism of fault rocks were used to trace the frictional heating temperature, however, few studies are focus on different temperatures effect of rock magnetic properties. To investigate rock magnetic response to different temperature, we conducted heating experiments on cataclasites from the Wenchuan earthquake Fault Scientific Drilling borehole 2 (WFSD-2) cores. Samples of cataclasites were obtained using an electric drill with a 1 cm-diameter drill pipe from 580.65 m-depth. Experiments were performed by a Thermal-optical measurement system under argon atmosphere and elevated temperatures. Both microstructural observations and powder X-ray diffraction analyses show that feldspar and quartz start to melt at 1100 ° and 1300 ° respectively. Magnetic susceptibility values of samples after heating are higher than that before heating. Samples after heating at 700 and 1750 ° have the highest values of magnetic susceptibility. Rock magnetic measurements show that the main ferromagnetic minerals within samples heated below 1100 ° (400, 700, 900 and 1100 °) are magnetite, which is new-formed by transformation of paramagnetic minerals. The χferri results show that the quantity of magnetite is bigger at sample heated by 700° experiment than by 400, 900 and 1100° experiments. Based on the FORC diagrams, we consider that magnetite grains are getting finer from 400 to 900°, and growing coarser when heated from 900 to 1100 °. SEM-EDX results indicate that the pure iron are formed in higher temperature (1300, 1500 and 1750 °), which present as framboids with size <10 μm. Rock magnetic measurements imply pure iron is the main ferromagnetic materials in these heated samples. The amount and size of iron framboids increase with increasing temperature. Therefore, we conclude that the paramagnetic minerals are decomposed into fine magnetite, then to coarse-grained magnetite, finally to pure iron at super high temperature. New-formed magnetite contributes to the higher magnetic susceptibility values of samples when heated at 400, 700, 900 and 1100°, while the neoformed pure iron is responsible to the higher magnetic susceptibility values of samples when heated at 1300, 1500 and 1750°.
Mechanisms and kinetics of granulated sewage sludge combustion.
Kijo-Kleczkowska, Agnieszka; Środa, Katarzyna; Kosowska-Golachowska, Monika; Musiał, Tomasz; Wolski, Krzysztof
2015-12-01
This paper investigates sewage sludge disposal methods with particular emphasis on combustion as the priority disposal method. Sewage sludge incineration is an attractive option because it minimizes odour, significantly reduces the volume of the starting material and thermally destroys organic and toxic components of the off pads. Additionally, it is possible that ashes could be used. Currently, as many as 11 plants use sewage sludge as fuel in Poland; thus, this technology must be further developed in Poland while considering the benefits of co-combustion with other fuels. This paper presents the results of experimental studies aimed at determining the mechanisms (defining the fuel combustion region by studying the effects of process parameters, including the size of the fuel sample, temperature in the combustion chamber and air velocity, on combustion) and kinetics (measurement of fuel temperature and mass changes) of fuel combustion in an air stream under different thermal conditions and flow rates. The combustion of the sludge samples during air flow between temperatures of 800 and 900°C is a kinetic-diffusion process. This process determines the sample size, temperature of its environment, and air velocity. The adopted process parameters, the time and ignition temperature of the fuel by volatiles, combustion time of the volatiles, time to reach the maximum temperature of the fuel surface, maximum temperature of the fuel surface, char combustion time, and the total process time, had significant impacts. Copyright © 2015 Elsevier Ltd. All rights reserved.
NASA Astrophysics Data System (ADS)
Goveas, Lora Rita; Anuradha, K. N.; Bhagyashree, K. S.; Bhat, S. V.
2015-05-01
To explore the effect of size reduction to nanoscale on the hole doped Sm0.65Ca0.35MnO3 compound, dc magnetic measurements and electron magnetic resonance (EMR) were done on bulk and nanoparticle samples in the temperature range 10 ≤ T ≤ 300 K. Magnetization measurement showed that the bulk sample undergoes a charge ordering transition at 240 K and shows a mixed magnetic phase at low temperature. However, the nanosample underwent a ferromagnetic transition at 75 K, and the charge ordered state was destabilized on size reduction down to nanoscale. The low-temperature ferromagnetic component is found to be enhanced in nanoparticles as compared to their bulk counterpart. Interestingly around room temperature, bulk particles show higher magnetization where as at low temperature nanoparticles show higher magnetization. Ferromagnetism in the bulk is due to super exchange where as ferromagnetism in nanoparticles is due to uncompensated spins of the surface layer. Temperature variation of EMR parameters correlates well with the results of magnetic measurements. The magnetic behaviour of the nanoparticles is understood in terms of the core shell scenario.
A Reassessment of Bergmann's Rule in Modern Humans
Foster, Frederick; Collard, Mark
2013-01-01
It is widely accepted that modern humans conform to Bergmann's rule, which holds that body size in endothermic species will increase as temperature decreases. However, there are reasons to question the reliability of the findings on which this consensus is based. One of these is that the main studies that have reported that modern humans conform to Bergmann's rule have employed samples that contain a disproportionately large number of warm-climate and northern hemisphere groups. With this in mind, we used latitudinally-stratified and hemisphere-specific samples to re-assess the relationship between modern human body size and temperature. We found that when groups from north and south of the equator were analyzed together, Bergmann's rule was supported. However, when groups were separated by hemisphere, Bergmann's rule was only supported in the northern hemisphere. In the course of exploring these results further, we found that the difference between our northern and southern hemisphere subsamples is due to the limited latitudinal and temperature range in the latter subsample. Thus, our study suggests that modern humans do conform to Bergmann's rule but only when there are major differences in latitude and temperature among groups. Specifically, groups must span more than 50 degrees of latitude and/or more than 30°C for it to hold. This finding has important implications for work on regional variation in human body size and its relationship to temperature. PMID:24015229
Gallegos, Críspulo; Valencia, Concepción; Partal, Pedro; Franco, José M; Maglio, Omay; Abrahamsson, Malin; Brito-de la Fuente, Edmundo
2012-08-01
The droplet size of commercial fish oil-containing injectable lipid emulsions, including conformance to United States Pharmacopeia (USP) standards on fat-globule size, was investigated. A total of 18 batches of three multichamber parenteral products containing the emulsion SMOFlipid as a component were analyzed. Samples from multiple lots of the products were evaluated to determine compliance with standards on the volume-weighted percentage of fat exceeding 0.05% (PFAT(5)) specified in USP chapter 729 to ensure the physical stability of i.v. lipid emulsions. The products were also analyzed to determine the effects of various storage times (3, 6, 9, and 12 months) and storage temperatures (25, 30, and 40 °C) on product stability. Larger-size lipid particles were quantified via single-particle optical sensing (SPOS). The emulsion's droplet-size distribution was determined via laser light scattering. SPOS and light-scattering analysis demonstrated mean PFAT(5) values well below USP-specified globule-size limits for all the tested products under all study conditions. In addition, emulsion aging at any storage temperature in the range studied did not result in a significant increase of PFAT(5) values, and mean droplet-size values did not change significantly during storage of up to 12 months at temperatures of 25-40 °C. PFAT(5) values were below the USP upper limits in SMOFlipid samples from multiple lots of three multichamber products after up to 12 months of storage at 25 or 30 °C or 6 months of storage at 40 °C.
NASA Astrophysics Data System (ADS)
Piqueux, Sylvain Loic Lucien
The physical characterization of the upper few centimeters to meters of the Martian surface has greatly benefited from remote temperature measurements. Typical grain sizes, rock abundances, subsurface layering, soil cementation, bedrock exposures, and ice compositions have been derived and mapped using temperature data in conjunction with subsurface models of heat conduction. Yet, these models of heat conduction are simplistic, precluding significant advances in the characterization of the physical nature of the Martian surface. A new model of heat conduction for homogeneous particulated media accounting for the grain size, porosity, gas pressure and composition, temperature, and the effect of any cementing phase is presented. The incorporation of the temperature effect on the bulk conductivity results in a distortion of the predicted diurnal and seasonal temperatures when compared to temperatures predicted with a temperature-independent conductivity model. Such distortions have been observed and interpreted to result from subsurface heterogeneities, but they may simply be explained by a temperature-dependency of the thermal inertia, with additional implications on the derived grain sizes. Cements are shown to significantly increase the bulk conductivity of a particulated medium and bond fractions <5% per volume are consistent with Martian thermal inertia data previously hypothesized to correspond to a global duricrust. A laboratory setup has been designed, built, calibrated and used to measure the thermal conductivity of particulated samples in order to test and refine the models mentioned above. Preliminary results confirm the influence of the temperature on the bulk conductivity, as well as the effect of changing the gas composition. Cemented samples are shown to conduct heat more efficiently than their uncemented counterparts.
NASA Astrophysics Data System (ADS)
Gholizadeh, Ahmad; Jafari, Elahe
2017-01-01
In this work, effects of sintering atmosphere and temperature on structural and magnetic properties of Ni0.3Cu0.2Zn0.5Fe2O4 nanoparticles prepared by citrate precursor method have been studied. The structural characterization of the samples by X-ray powder diffraction and FT-IR spectroscopy is evidence for formation of a cubic structure with no presence of impurity phase. Calculated values of crystallite size and unit cell parameter show an increase with sintering temperature under different atmospheres. Variation of saturation magnetization with sintering temperature and atmosphere can be attributed to change of three factors: magnetic core size, inversion parameter and the change of Fe3+-ion concentration due to the presence of Fe4+ and Fe2+ ions. The saturation magnetization gradually grows with sintering temperature due to increase of magnetic core size and a maximum 63 emu/g was achieved at 600 °C under carbon monoxide-ambient atmosphere.
Ortega-Mayagoitia, Elizabeth; Hernández-Martínez, Osvaldo; Ciros-Pérez, Jorge
2018-01-01
According to the Climatic Variability Hypothesis [CVH], thermal plasticity should be wider in organisms from temperate environments, but is unlikely to occur in tropical latitudes where temperature fluctuations are narrow. In copepods, food availability has been suggested as the main driver of phenotypic variability in adult size if the range of temperature change is less than 14°C. Leptodiaptomus garciai is a calanoid copepod inhabiting Lake Alchichica, a monomictic, tropical lake in Mexico that experiences regular, narrow temperature fluctuations but wide changes in phytoplankton availability. We investigated whether the seasonal fluctuations of temperature and food produce phenotypic variation in the life-history traits of this tropical species. We sampled L. garciai throughout a year and measured female size, egg size and number, and hatching success, along with temperature and phytoplankton biomass. The amplitude of the plastic responses was estimated with the Phenotypic Plasticity Index. This index was also computed for a published dataset of 84 copepod populations to look if there is a relationship between the amplitude of the phenotypic plasticity of adult size and seasonal change in temperature. The temperature annual range in Lake Alchichica was 3.2°C, whereas phytoplankton abundance varied 17-fold. A strong pattern of thermal plasticity in egg size and adult female size followed the inverse relationship with temperature commonly observed in temperate environments, although its adaptive value was not demonstrated. Egg number, relative reproductive effort and number of nauplii per female were clearly plastic to food availability, allowing organisms to increase their fitness. When comparing copepod species from different latitudes, we found that the magnitude of thermal plasticity of adult size is not related to the range of temperature variation; furthermore, thermal plasticity exists even in environments of limited temperature variation, where the response is more intense compared to temperate populations.
Hernández-Martínez, Osvaldo; Ciros-Pérez, Jorge
2018-01-01
According to the Climatic Variability Hypothesis [CVH], thermal plasticity should be wider in organisms from temperate environments, but is unlikely to occur in tropical latitudes where temperature fluctuations are narrow. In copepods, food availability has been suggested as the main driver of phenotypic variability in adult size if the range of temperature change is less than 14°C. Leptodiaptomus garciai is a calanoid copepod inhabiting Lake Alchichica, a monomictic, tropical lake in Mexico that experiences regular, narrow temperature fluctuations but wide changes in phytoplankton availability. We investigated whether the seasonal fluctuations of temperature and food produce phenotypic variation in the life-history traits of this tropical species. We sampled L. garciai throughout a year and measured female size, egg size and number, and hatching success, along with temperature and phytoplankton biomass. The amplitude of the plastic responses was estimated with the Phenotypic Plasticity Index. This index was also computed for a published dataset of 84 copepod populations to look if there is a relationship between the amplitude of the phenotypic plasticity of adult size and seasonal change in temperature. The temperature annual range in Lake Alchichica was 3.2°C, whereas phytoplankton abundance varied 17-fold. A strong pattern of thermal plasticity in egg size and adult female size followed the inverse relationship with temperature commonly observed in temperate environments, although its adaptive value was not demonstrated. Egg number, relative reproductive effort and number of nauplii per female were clearly plastic to food availability, allowing organisms to increase their fitness. When comparing copepod species from different latitudes, we found that the magnitude of thermal plasticity of adult size is not related to the range of temperature variation; furthermore, thermal plasticity exists even in environments of limited temperature variation, where the response is more intense compared to temperate populations. PMID:29708999
NASA Astrophysics Data System (ADS)
Purwaningsih, Hariyati; Pratiwi, Vania Mitha; Purwana, Siti Annisa Bani; Nurdiansyah, Haniffudin; Rahmawati, Yenny; Susanti, Diah
2018-04-01
Rice husk is an agricultural waste that is potentially used as natural silica resources. Natural silica claimed to be safe in handling, cheap and can be generate from cheap resource. In this study mesoporous silica was synthesized using sodium silicate extracted from rice husk ash. This research's aim are to study the optimization of silica extraction from rice husk, characterizing mesoporous silica from sol-gel method and surfactant templating from rice husk and the effect of hydrothermal temperature on mesoporous silica nanoparticle (MSNp) formation. In this research, rice husk was extracted with sol-gel method and was followed by hydrothermal treatment; several of hydrothermal temperatures were 85°C, 100°C, 115°C, 130°C and 145° for 24 hours. X-ray diffraction analysis was identified of α-SiO2 phase and NaCl compound impurities. Scherer's analysis method for crystallite size have resulted 6.27-40.3 nm. FTIR results of silica from extraction and MSNp indicated Si-O-Si bonds on the sample. SEM result showed the morphology of the sample that has spherical shape and smooth surface. TEM result showed particle size ranged between 69,69-84,42 nm. BET showed that the pore size classified as mesoporous with pore diameter size is 19,29 nm.
NASA Astrophysics Data System (ADS)
Ding, Chenliang; Wei, Jingsong; Xiao, Mufei
2018-05-01
We herein propose a far-field super-resolution imaging with metal thin films based on the temperature-dependent electron-phonon collision frequency effect. In the proposed method, neither fluorescence labeling nor any special properties are required for the samples. The 100 nm lands and 200 nm grooves on the Blu-ray disk substrates were clearly resolved and imaged through a laser scanning microscope of wavelength 405 nm. The spot size was approximately 0.80 μm , and the imaging resolution of 1/8 of the laser spot size was experimentally obtained. This work can be applied to the far-field super-resolution imaging of samples with neither fluorescence labeling nor any special properties.
Rakow, Tobias; El Deeb, Sami; Hahne, Thomas; El-Hady, Deia Abd; AlBishri, Hassan M; Wätzig, Hermann
2014-09-01
In this study, size-exclusion chromatography and high-resolution atomic absorption spectrometry methods have been developed and evaluated to test the stability of proteins during sample pretreatment. This especially includes different storage conditions but also adsorption before or even during the chromatographic process. For the development of the size exclusion method, a Biosep S3000 5 μm column was used for investigating a series of representative model proteins, namely bovine serum albumin, ovalbumin, monoclonal immunoglobulin G antibody, and myoglobin. Ambient temperature storage was found to be harmful to all model proteins, whereas short-term storage up to 14 days could be done in an ordinary refrigerator. Freezing the protein solutions was always complicated and had to be evaluated for each protein in the corresponding solvent. To keep the proteins in their native state a gentle freezing temperature should be chosen, hence liquid nitrogen should be avoided. Furthermore, a high-resolution continuum source atomic absorption spectrometry method was developed to observe the adsorption of proteins on container material and chromatographic columns. Adsorption to any container led to a sample loss and lowered the recovery rates. During the pretreatment and high-performance size-exclusion chromatography, adsorption caused sample losses of up to 33%. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.
NASA Astrophysics Data System (ADS)
Gui, Xulong; Luo, Xiaobing; Wang, Xiaoping; Liu, Sheng
2015-12-01
Micro-electrical-mechanical system (MEMS) has become important for many industries such as automotive, home appliance, portable electronics, especially with the emergence of Internet of Things. Volume testing with temperature compensation has been essential in order to provide MEMS based sensors with repeatability, consistency, reliability, and durability, but low cost. Particularly, in the temperature calibration test, temperature uniformity of thermal cycling based calibration chamber becomes more important for obtaining precision sensors, as each sensor is different before the calibration. When sensor samples are loaded into the chamber, we usually open the door of the chamber, then place fixtures into chamber and mount the samples on the fixtures. These operations may affect temperature uniformity in the chamber. In order to study the influencing factors of sample-loading on the temperature uniformity in the chamber during calibration testing, numerical simulation work was conducted first. Temperature field and flow field were simulated in empty chamber, chamber with open door, chamber with samples, and chamber with fixtures, respectively. By simulation, it was found that opening chamber door, sample size and number of fixture layers all have effects on flow field and temperature field. By experimental validation, it was found that the measured temperature value was consistent with the simulated temperature value.
Magnetic Properties and Microstructure of Some 2:17 High Temperature Magnets
NASA Astrophysics Data System (ADS)
Meng-Burany, X.; Hadjipanayis, George C.; Chui, S. T.
1997-03-01
Recent DOD demands for electric vehicle/plane applications require the use of magnets with operating temperatures > 450^circ C . Of existing high performance magnets, only the Sm(Co,Fe,Cu,Zr)z precipitation--hardened magnets have an operating temperature (300^circ C) which is close to the desired temperature and this makes these magnets potential candidates for further optimization studies. We have started a systematic study and modeling of the high temperature magnetic properties of several commercial magnets and other specially designed magnets supplied to us by Crucible Research. All the samples studied had a room temperature coercivity above 15 kOe. The coercivity was found to decrease with increasing temperature, with values of less than 4 kOe at 450^circ C , except for one sample which had a better temperature dependence with a coercivity above 6 kOe. TEM studies showed a cellular microstructure in all samples. The sample with better temperature properties had a smaller cell size but thicker cell walls. Lorentz electron microscopy studies are underway to image the domain walls and study their interaction with the cellular structure. The results of these studies will hopefully help us to understand the composition--microstructure--property relation in these magnets.
NASA Astrophysics Data System (ADS)
Majzoobi, G. H.; Rahmani, K.; Atrian, A.
2018-01-01
In this paper, dynamic compaction is employed to produce Mg-SiC nanocomposite samples using a mechanical drop hammer. Different volume fractions of SiC nano reinforcement and magnesium (Mg) micron-size powder as the matrix are mechanically milled and consolidated at different temperatures. It is found that with the increase of temperature the sintering requirements is satisfied and higher quality samples are fabricated. The density, hardness, compressive strength and the wear resistance of the compacted specimens are characterized in this work. It was found that by increasing the content of nano reinforcement, the relative density of the compacted samples decreases, whereas, the micro-hardness and the strength of the samples enhance. Furthermore, higher densification temperatures lead to density increase and hardness reduction. Additionally, it is found that the wear rate of the nanocomposite is increased remarkably by increasing the SiC nano reinforcement.
NASA Astrophysics Data System (ADS)
Yonatan Mulushoa, S.; Murali, N.; Tulu Wegayehu, M.; Margarette, S. J.; Samatha, K.
2018-03-01
Cu-Cr substituted magnesium ferrite materials (Mg1 - xCuxCrxFe21 - xO4 with x = 0.0-0.7) have been synthesized by the solid state reaction method. XRD analysis revealed the prepared samples are cubic spinel with single phase face centered cubic. A significant decrease of ∼41.15 nm in particle size is noted in response to the increase in Cu-Cr substitution level. The room temperature resistivity increases gradually from 0.553 × 105 Ω cm (x = 0.0) to 0.105 × 108 Ω cm (x = 0.7). Temperature dependent DC-electrical resistivity of all the samples, exhibits semiconductor like behavior. Cu-Cr doped materials can be suitable to limit the eddy current losses. VSM result shows pure and doped magnesium ferrite particles show soft ferrimagnetic nature at room temperature. The saturation magnetization of the samples decreases initially from 34.5214 emu/g for x = 0.0 to 18.98 emu/g (x = 0.7). Saturation magnetization, remanence and coercivity are decreased with doping, which may be due to the increase in grain size.
NASA Astrophysics Data System (ADS)
Egarievwe, Stephen U.; Yang, Ge; Egarievwe, Alexander A.; Okwechime, Ifechukwude O.; Gray, Justin; Hales, Zaveon M.; Hossain, Anwar; Camarda, Giuseppe S.; Bolotnikov, Aleksey E.; James, Ralph B.
2015-06-01
Bridgman-grown cadmium zinc telluride (CdZnTe or CZT) and cadmium manganese telluride (CdMnTe or CMT) crystals often have Te inclusions that limit their performances as X-ray- and gamma-ray-detectors. We present here the results of post-growth thermal annealing aimed at reducing and eliminating Te inclusions in them. In a 2D analysis, we observed that the sizes of the Te inclusions declined to 92% during a 60-h annealing of CZT at 510 °C under Cd vapor. Further, tellurium inclusions were eliminated completely in CMT samples annealed at 570 °C in Cd vapor for 26 h, whilst their electrical resistivity fell by an order of 102. During the temperature-gradient annealing of CMT at 730 °C and an 18 °C/cm temperature gradient for 18 h in a vacuum of 10-5 mbar, we observed the diffusion of Te from the sample, so causing a reduction in size of the Te inclusions. For CZT samples annealed at 700 °C in a 10 °C/cm temperature gradient, we observed the migration of Te inclusions from a low-temperature region to a high one at 0.022 μm/s. During the temperature-gradient annealing of CZT in a vacuum of 10-5 mbar at 570 °C and 30 °C/cm for 18 h, some Te inclusions moved toward the high-temperature side of the wafer, while other inclusions of the same size, i.e., 10 μm in diameter, remained in the same position. These results show that the migration, diffusion, and reaction of Te with Cd in the matrix of CZT- and CMT-wafers are complex phenomena that depend on the conditions in local regions, such as composition and structure, as well as on the annealing conditions.
Thermal decomposition of wood: influence of wood components and cellulose crystallite size.
Poletto, Matheus; Zattera, Ademir J; Forte, Maria M C; Santana, Ruth M C
2012-04-01
The influence of wood components and cellulose crystallinity on the thermal degradation behavior of different wood species has been investigated using thermogravimetry, chemical analysis and X-ray diffraction. Four wood samples, Pinus elliottii (PIE), Eucalyptus grandis (EUG), Mezilaurus itauba (ITA) and Dipteryx odorata (DIP) were used in this study. The results showed that higher extractives contents associated with lower crystallinity and lower cellulose crystallite size can accelerate the degradation process and reduce the wood thermal stability. On the other hand, the thermal decomposition of wood shifted to higher temperatures with increasing wood cellulose crystallinity and crystallite size. These results indicated that the cellulose crystallite size affects the thermal degradation temperature of wood species. Copyright © 2012. Published by Elsevier Ltd.
NASA Astrophysics Data System (ADS)
Manjili, Mohsen Hajipour; Halali, Mohammad
2018-02-01
Samples of INCONEL 718 were levitated and melted in a slag by the application of an electromagnetic field. The effects of temperature, time, and slag composition on the inclusion content of the samples were studied thoroughly. Samples were compared with the original alloy to study the effect of the process on inclusions. Size, shape, and chemical composition of remaining non-metallic inclusions were investigated. The samples were prepared by Standard Guide for Preparing and Evaluating Specimens for Automatic Inclusion Assessment of Steel (ASTM E 768-99) method and the results were reported by means of the Standard Test Methods for Determining the Inclusion Content of Steel (ASTM E 45-97). Results indicated that by increasing temperature and processing time, greater level of cleanliness could be achieved, and numbers and size of the remaining inclusions decreased significantly. It was also observed that increasing calcium fluoride content of the slag helped reduce inclusion content.
NASA Astrophysics Data System (ADS)
Marsh, Jonathan; Zhang, Yang; Verma, Devendra; Biswas, Sudipta; Haque, Aman; Tomar, Vikas
2015-12-01
Zirconium alloys for nuclear applications with different microstructures were produced by manufacturing processes such as chipping, rolling and annealing. The two Zr samples, rolled and rolled-annealed were subjected to different levels of irradiation, 1 keV and 100 eV, to study the effect of irradiation dosages. The effect of microstructure and irradiation on the mechanical properties (reduced modulus, hardness, indentation yield strength) was analyzed with nanoindentation experiments, which were carried out in the temperature range of 25°C to 450°C to investigate temperature dependence. An indentation size effect analysis was performed and the mechanical properties were also corrected for the oxidation effects at high temperatures. The irradiation-induced hardness was observed, with rolled samples exhibiting higher increase compared to rolled and annealed samples. The relevant material parameters of the Anand viscoplastic model were determined for Zr samples containing different level of irradiation to account for viscoplasticity at high temperatures. The effect of the microstructure and irradiation on the stress-strain curve along with the influence of temperature on the mechanisms of irradiation creep such as formation of vacancies and interstitials is presented. The yield strength of irradiated samples was found to be higher than the unirradiated samples which also showed a decreasing trend with the temperature.
NASA Astrophysics Data System (ADS)
Badejo, S. A.; Muxworthy, A. R.; Fraser, A.
2017-12-01
Pyrolysis experiments show that magnetic minerals can be produced inorganically during oil formation in the `oil-kitchen'. Here we try to identify a magnetic proxy that can be used to trace hydrocarbon migration pathways by determining the morphology, abundance, mineralogy and size of the magnetic minerals present in reservoirs. We address this by examining the Tay formation in the Western Central Graben in the North Sea. The Tertiary sandstones are undeformed and laterally continuous in the form of an east-west trending channel, facilitating long distance updip migration of oil and gas to the west. We have collected 179 samples from 20 oil-stained wells and 15 samples from three dry wells from the British Geological Survey Core Repository. Samples were selected based on geological observations (water-wet sandstone, oil-stained sandstone, siltstones and shale). The magnetic properties of the samples were determined using room-temperature measurements on a Vibrating Sample Magnetometer (VSM), low-temperature (0-300K) measurements on a Magnetic Property Measurement System (MPMS) and high-temperature (300-973K) measurements on a Kappabridge susceptibility meter. We identified magnetite, pyrrhotite, pyrite and siderite in the samples. An increasing presence of ferrimagnetic iron sulphides is noticed along the known hydrocarbon migration pathway. Our initial results suggest mineralogy coupled with changes in grain size are possible proxies for hydrocarbon migration.
Effect of Frozen Storage Temperature on the Quality of Premium Ice Cream.
Park, Sung Hee; Jo, Yeon-Ji; Chun, Ji-Yeon; Hong, Geun-Pyo; Davaatseren, Munkhtugs; Choi, Mi-Jung
2015-01-01
The market sales of premium ice cream have paralleled the growth in consumer desire for rich flavor and taste. Storage temperature is a major consideration in preserving the quality attributes of premium ice cream products for both the manufacturer and retailers during prolonged storage. We investigated the effect of storage temperature (-18℃, -30℃, -50℃, and -70℃) and storage times, up to 52 wk, on the quality attributes of premium ice cream. Quality attributes tested included ice crystal size, air cell size, melting resistance, and color. Ice crystal size increased from 40.3 μm to 100.1 μm after 52 wk of storage at -18℃. When ice cream samples were stored at -50℃ or -70℃, ice crystal size slightly increased from 40.3 μm to 57-58 μm. Initial air cell size increased from 37.1 μm to 87.7 μm after storage at -18℃ for 52 wk. However, for storage temperatures of -50℃ and -70℃, air cell size increased only slightly from 37.1 μm to 46-47 μm. Low storage temperature (-50℃ and -70℃) resulted in better melt resistance and minimized color changes in comparison to high temperature storage (-18℃ and -30℃). In our study, quality changes in premium ice cream were gradually minimized according to decrease in storage temperature up to-50℃. No significant beneficial effect of -70℃ storage was found in quality attributes. In the scope of our experiment, we recommend a storage temperature of -50℃ to preserve the quality attributes of premium ice cream.
Effect of Frozen Storage Temperature on the Quality of Premium Ice Cream
Park, Sung Hee; Jo, Yeon-Ji; Chun, Ji-Yeon; Hong, Geun-Pyo
2015-01-01
The market sales of premium ice cream have paralleled the growth in consumer desire for rich flavor and taste. Storage temperature is a major consideration in preserving the quality attributes of premium ice cream products for both the manufacturer and retailers during prolonged storage. We investigated the effect of storage temperature (−18℃, −30℃, −50℃, and −70℃) and storage times, up to 52 wk, on the quality attributes of premium ice cream. Quality attributes tested included ice crystal size, air cell size, melting resistance, and color. Ice crystal size increased from 40.3 μm to 100.1 μm after 52 wk of storage at −18℃. When ice cream samples were stored at −50℃ or −70℃, ice crystal size slightly increased from 40.3 μm to 57-58 μm. Initial air cell size increased from 37.1 μm to 87.7 μm after storage at −18℃ for 52 wk. However, for storage temperatures of −50℃ and −70℃, air cell size increased only slightly from 37.1 μm to 46-47 μm. Low storage temperature (−50℃ and −70℃) resulted in better melt resistance and minimized color changes in comparison to high temperature storage (−18℃ and −30℃). In our study, quality changes in premium ice cream were gradually minimized according to decrease in storage temperature up to−50℃. No significant beneficial effect of −70℃ storage was found in quality attributes. In the scope of our experiment, we recommend a storage temperature of −50℃ to preserve the quality attributes of premium ice cream. PMID:26877639
NASA Astrophysics Data System (ADS)
Syazwan, M. M.; Hapishah, A. N.; Azis, R. S.; Abbas, Z.; Hamidon, M. N.
2018-06-01
The effect of grain growth via sintering temperature on some magnetic properties is reported in this research. Ni0.6Zn0.4Fe2O4 nanoparticles were mechanically alloyed for 6 h and the sintering process starting from 600 to 1200 °C with 25 °C increment with only one sample subjected to all sintering scheme. The resulting change in the material was observed after each sintering. Single phase has been formed at 600 °C and above and the intensity peaks increased with sintering temperature as well as crystallinity increment. The morphological studies showed grain size increment as the sintering temperature increased. Moreover, the density increased while the porosity decreased with increasing sintering temperature. The saturation induction, Bs increased with the increased of grain size. On the other hand, the coercivity-vs-grain size plot reveals the critical single-domain-to-multidomain grain size to be about ∼400 nm. The initial permeability, μi value was increased with grain size enhancement. The microstructural grain growth, as exposed for the first time by this research, is shown as a process of multiple activation energy barriers.
Till, J.L.; Jackson, M.J.; Rosenbaum, J.G.; Solheid, P.
2011-01-01
The Tiva Canyon Tuff contains dispersed nanoscale Fe-Ti-oxide grains with a narrow magnetic grain size distribution, making it an ideal material in which to identify and study grain-size-sensitive magnetic behavior in rocks. A detailed magnetic characterization was performed on samples from the basal 5 m of the tuff. The magnetic materials in this basal section consist primarily of (low-impurity) magnetite in the form of elongated submicron grains exsolved from volcanic glass. Magnetic properties studied include bulk magnetic susceptibility, frequency-dependent and temperature-dependent magnetic susceptibility, anhysteretic remanence acquisition, and hysteresis properties. The combined data constitute a distinct magnetic signature at each stratigraphic level in the section corresponding to different grain size distributions. The inferred magnetic domain state changes progressively upward from superparamagnetic grains near the base to particles with pseudo-single-domain or metastable single-domain characteristics near the top of the sampled section. Direct observations of magnetic grain size confirm that distinct transitions in room temperature magnetic susceptibility and remanence probably denote the limits of stable single-domain behavior in the section. These results provide a unique example of grain-size-dependent magnetic properties in noninteracting particle assemblages over three decades of grain size, including close approximations of ideal Stoner-Wohlfarth assemblages, and may be considered a useful reference for future rock magnetic studies involving grain-size-sensitive properties.
Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods
NASA Astrophysics Data System (ADS)
Sakthiraj, K.; Hema, M.; Balachandrakumar, K.
2016-04-01
The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol-gel, microwave assisted sol-gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6-12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M-H curve of all the samples. But the sol-gel derived sample shows the higher values of saturation magnetization (Ms) and remanence (Mr) than other two samples. This study reveals that the sol-gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.
Crystallite Size-Lattice Strain Estimation and Optical Properties of Mn0.5Zn0.5Fe2O4 Nanoparticles
NASA Astrophysics Data System (ADS)
Indrayana, I. P. T.; Suharyadi, E.
2018-04-01
In the present work, we performed William-Hall plot using uniform deformation model (UDM) to estimate the crystallite size and lattice strain of Mn0.5Zn0.5Fe2O4 with various calcination temperature. The calculated crystallite sizes are 25.86 nm, 29.55 nm and 24.97 nm for nanoparticles which were calcined at a temperature of 600°C, 800°C and 1000°C, consecutively. The strain of nanoparticles has value in the order of 10-3. Controlling the calcination temperature will facilitate a change in crystallinity of nanoparticles and influence their crystallite size and strain of the crystal lattice. The optical band gap energy of samples nanoparticles is in a range of 1.09 eV – 3.30 eV. Increasing calcination temperature increased the direct and indirect band gap energy. The Urbach energy was found to increase with increased of gap energy. These results demonstrated that higher structural and optical properties of Mn0.5Zn0.5Fe2O4 can be obtained from a higher calcination temperature.
Controlled synthesis and luminescence properties of CaMoO4:Eu3+ microcrystals
NASA Astrophysics Data System (ADS)
Xie, Ying; Ma, Siming; Wang, Yu; Xu, Mai; Lu, Chengxi; Xiao, Linjiu; Deng, Shuguang
2018-03-01
Pure tetragonal-phased Ca0.9MoO4:0.1Eu3+ (CaMoO4:Eu3+) microcrystals with varying particle sizes were prepared via a co-deposition in water/oil (w/o) phase method. The particle sizes of as-prepared samples were controlled by calcination temperature and calcination time, and the crystallinity of the samples enhances with increasing particle size. The luminescence properties of CaMoO4:Eu3+ microcrystals were studied with varying particle size. The results reveal that the intensity of emission spectra of the CaMoO4:Eu3+ samples increases with increasing particle size, and they have closely correlation with each other. It is the same with the luminescence lifetime. The luminescence lifetime of the CaMoO4:Eu3+ samples decreases from 0.637 ms to 0.447 ms with increasing particle size from 0.12 μm to 1.79 μm, respectively. This study not only provides information for size-dependent luminescence properties of CaMoO4:Eu3+ but also gives a reference for potential applications in high voltage electric porcelain material.
Molecular dynamics simulations using temperature-enhanced essential dynamics replica exchange.
Kubitzki, Marcus B; de Groot, Bert L
2007-06-15
Today's standard molecular dynamics simulations of moderately sized biomolecular systems at full atomic resolution are typically limited to the nanosecond timescale and therefore suffer from limited conformational sampling. Efficient ensemble-preserving algorithms like replica exchange (REX) may alleviate this problem somewhat but are still computationally prohibitive due to the large number of degrees of freedom involved. Aiming at increased sampling efficiency, we present a novel simulation method combining the ideas of essential dynamics and REX. Unlike standard REX, in each replica only a selection of essential collective modes of a subsystem of interest (essential subspace) is coupled to a higher temperature, with the remainder of the system staying at a reference temperature, T(0). This selective excitation along with the replica framework permits efficient approximate ensemble-preserving conformational sampling and allows much larger temperature differences between replicas, thereby considerably enhancing sampling efficiency. Ensemble properties and sampling performance of the method are discussed using dialanine and guanylin test systems, with multi-microsecond molecular dynamics simulations of these test systems serving as references.
Hower, J.C.; Trimble, A.S.; Eble, C.F.; Palmer, C.A.; Kolker, A.
1999-01-01
Fly ash samples were collected in November and December of 1994, from generating units at a Kentucky power station using high- and low-sulfur feed coals. The samples are part of a two-year study of the coal and coal combustion byproducts from the power station. The ashes were wet screened at 100, 200, 325, and 500 mesh (150, 75, 42, and 25 ??m, respectively). The size fractions were then dried, weighed, split for petrographic and chemical analysis, and analyzed for ash yield and carbon content. The low-sulfur "heavy side" and "light side" ashes each have a similar size distribution in the November samples. In contrast, the December fly ashes showed the trend observed in later months, the light-side ash being finer (over 20 % more ash in the -500 mesh [-25 ??m] fraction) than the heavy-side ash. Carbon tended to be concentrated in the coarse fractions in the December samples. The dominance of the -325 mesh (-42 ??m) fractions in the overall size analysis implies, though, that carbon in the fine sizes may be an important consideration in the utilization of the fly ash. Element partitioning follows several patterns. Volatile elements, such as Zn and As, are enriched in the finer sizes, particularly in fly ashes collected at cooler, light-side electrostatic precipitator (ESP) temperatures. The latter trend is a function of precipitation at the cooler-ESP temperatures and of increasing concentration with the increased surface area of the finest fraction. Mercury concentrations are higher in high-carbon fly ashes, suggesting Hg adsorption on the fly ash carbon. Ni and Cr are associated, in part, with the spinel minerals in the fly ash. Copyright ?? 1999 Taylor & Francis.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Narayanan, Manoj Kumar, E-mail: manukokkal01@gmail.com; Shashikala, H. D.
Silver nanoparticle embedded 30BaO-20CaF{sub 2}-50P{sub 2}O{sub 5}-4Ag{sub 2}O-4SnO glasses were prepared by melt-quenching and subsequent heat treatment process. Silver-doped glasses were heat treated at temperatures 500 °C, 525°C and 550 °C for a fixed duration of 10 hours to incorporate metal nanoparticles into the glass matrix. Appearance and shift in peak positions of the surface plasmon resonance (SPR) bands in the optical absorption spectra of heat treated glass samples indicated that both formation and growth of nanoparticle depended on heat treatment temperature. Glass sample heat treated at 525 °C showed a SPR peak around 3 eV, which indicated that sphericalmore » nanoparticles smaller than 20 nm were formed inside the glass matrix. Whereas sample heat treated at 550 °C showed a size dependent red shift in SPR peak due to the presence of silver nanoparticles of size larger than 20 nm. Size of the nanoparticles calculated using full-width at half-maximum (FWHM) of absorption band showed a good agreement with the particle size obtained from transmission electron microscopy (TEM) analysis.« less
NASA Astrophysics Data System (ADS)
Ghosh, P.; Bhowmik, R. N.; Das, M. R.; Mitra, P.
2017-04-01
We have studied the grain size dependent electrical conductivity, dielectric relaxation and magnetic field dependent current voltage (I - V) characteristics of nickel ferrite (NiFe2O4) . The material has been synthesized by sol-gel self-combustion technique, followed by ball milling at room temperature in air environment to control the grain size. The material has been characterized using X-ray diffraction (refined with MAUD software analysis) and Transmission electron microscopy. Impedance spectroscopy and I - V characteristics in the presence of variable magnetic fields have confirmed the increase of resistivity for the fine powdered samples (grain size 5.17±0.6 nm), resulted from ball milling of the chemical routed sample. Activation energy of the material for electrical charge hopping process has increased with the decrease of grain size by mechanical milling of chemical routed sample. The I - V curves showed many highly non-linear and irreversible electrical features, e.g., I - V loop and bi-stable electronic states (low resistance state-LRS and high resistance state-HRS) on cycling the electrical bias voltage direction during I-V curve measurement. The electrical dc resistance for the chemically routed (without milled) sample in HRS (∼3.4876×104 Ω) at 20 V in presence of magnetic field 10 kOe has enhanced to ∼3.4152×105 Ω for the 10 h milled sample. The samples exhibited an unusual negative differential resistance (NDR) effect that gradually decreased on decreasing the grain size of the material. The magneto-resistance of the samples at room temperature has been found substantially large (∼25-65%). The control of electrical charge transport properties under magnetic field, as observed in the present ferrimagnetic material, indicate the magneto-electric coupling in the materials and the results could be useful in spintronics applications.
NASA Astrophysics Data System (ADS)
Gherca, Daniel; Pui, Aurel; Cornei, Nicoleta; Cojocariu, Alina; Nica, Valentin; Caltun, Ovidiu
2012-11-01
We focused on obtaining MFe2O4 nanoparticles using ricin oil solution as surfactant and on their structural characterization and magnetic properties. The annealed samples at 500 °C in air for 6 h were analyzed for the crystal phase identification by powder X-ray diffraction using CuKα radiation. The particle size, the chemical composition and the morphology of the calcinated powders were characterized by scanning electron microscopy. All sintered samples contain only one phase, which has a cubic structure with crystallite sizes of 12-21 nm. From the infrared spectra of all samples were observed two strong bands around 600 and 400 cm-1, which correspond to the intrinsic lattice vibrations of octahedral and tetrahedral sites of the spinel structure, respectively, and characteristic vibration for capping agent. The magnetic properties of fine powders were investigated at room temperature by using a vibrating sample magnetometer. The room temperature M-H hysteresis loops show ferromagnetic behavior of the calcined samples, with specific saturation magnetization (Ms) values ranging between 11 and 53 emu/g.
Chen, Hua-xing; Tang, Hong-ming; Duan, Ming; Liu, Yi-gang; Liu, Min; Zhao, Feng
2015-01-01
In this study, the effects of gravitational settling time, temperature, speed and time of centrifugation, flocculant type and dosage, bubble size and gas amount were investigated. The results show that the simple increase in settling time and temperature is of no use for oil-water separation of the three wastewater samples. As far as oil-water separation efficiency is concerned, increasing centrifugal speed and centrifugal time is highly effective for L sample, and has a certain effect on J sample, but is not valid for S sample. The flocculants are highly effective for S and L samples, and the oil-water separation efficiency increases with an increase in the concentration of inorganic cationic flocculants. There exist critical reagent concentrations for the organic cationic and the nonionic flocculants, wherein a higher or lower concentration of flocculant would cause a decrease in the treatment efficiency. Flotation is an effective approach for oil-water separation of polymer-contained wastewater from the three oilfields. The oil-water separation efficiency can be enhanced by increasing floatation agent concentration, flotation time and gas amount, and by decreasing bubble size.
NASA Astrophysics Data System (ADS)
Dung, Nguyen Thi; Linh, Dinh Chi; Huyen Yen, Pham Duc; Yu, Seong Cho; Van Dang, Nguyen; Dang Thanh, Tran
2018-06-01
Influence of the crystallite size on the magnetic and critical properties of nanocrystals has been investigated. The results show that Curie temperature and magnetization slightly decrease with decreasing average crystallite size . Based on the mean-field theory and the magnetic-field dependences of magnetization at different temperatures , we pointed out that the ferromagnetic-paramagnetic phase transition in the samples undergoes the second-order phase transition with the critical exponents (, , and ) close to those of the mean-field theory. However, there is a small deviation from those expected for the mean-field theory of the values of , and obtained for the samples. It means that short-range ferromagnetic interactions appear in the smaller particles. In other words, nanocrystals become more magnetically inhomogeneous with smaller crystallite sizes that could be explained by the presence of surface-related effects, lattice strain and distortions, which lead the strength of ferromagnetic interaction is decreased in the small crystallite sizes.
A Fracture Mechanics Approach to Thermal Shock Investigation in Alumina-Based Refractory
NASA Astrophysics Data System (ADS)
Volkov-Husović, T.; Heinemann, R. Jančić; Mitraković, D.
2008-02-01
The thermal shock behavior of large grain size, alumina-based refractories was investigated experimentally using a standard water quench test. A mathematical model was employed to simulate the thermal stability behavior. Behavior of the samples under repeated thermal shock was monitored using ultrasonic measurements of dynamic Young's modulus. Image analysis was used to observe the extent of surface degradation. Analysis of the obtained results for the behavior of large grain size samples under conditions of rapid temperature changes is given.
Reduction of the capillary water absorption of foamed concrete by using the porous aggregate
NASA Astrophysics Data System (ADS)
Namsone, E.; Sahmenko, G.; Namsone, E.; Korjakins, A.
2017-10-01
The article reports on the research of reduction of the capillary water absorption of foamed concrete (FC) by using the porous aggregate such as the granules of expanded glass (EG) and the cenospheres (CS). The EG granular aggregate is produced by using recycled glass and blowing agents, melted down in high temperature. The unique structure of the EG granules is obtained where the air is kept closed inside the pellet. The use of the porous aggregate in the preparation process of the FC samples provides an opportunity to improve some physical and mechanical properties of the FC, classifying it as a product of high-performance. In this research the FC samples were produced by adding the EG granules and the CS. The capillary water absorption of hardened samples has been verified. The pore size distribution has been determined by microscope. It is a very important characteristic, specifically in the cold climate territories-where temperature often falls below zero degrees. It is necessary to prevent forming of the micro sized pores in the final structure of the material as it reduces its water absorption capacity. In addition, at a below zero temperature water inside these micro sized pores can increase them by expanding the stress on their walls during the freezing process. Research of the capillary water absorption kinetics can be practical for prevision of the FC durability.
NASA Astrophysics Data System (ADS)
Maulia, R.; Putra, R. A.; Suharyadi, E.
2017-05-01
Mg0.5Ni0.5Fe2O4 nanoparticles have been successfully synthesized by using co-precipitation method and varying the synthesis parameter, i.e. synthesis temperature and NaOH concentration. X-ray Diffraction (XRD) pattern showed that nanoparticles have cubic spinel structures with an additional phase of γ-Fe2O3 and particle size varies within the range of 4.3 - 6.7 nm. This variation is due to the effect of various synthesis parameters. Transmission Electron Microscopy (TEM) image showed that the nanoparticles exhibited agglomeration. The observed diffraction ring from selected area electron diffraction showed that the sample was polycrystalline and confirmed the peak appearing in XRD. The coercivities showed an increasing trend with an increase in particle size from 44.7 Oe to 49.6 Oe for variation of NaOH concentration, and a decreasing trend with an increase in particle size from 46.8 to 45.1 Oe for variation of synthesis temperature. The maximum magnetization showed an increasing trend with an increase in the ferrite phase from 3.7 emu/g to 5.4 emu/g possessed in the sample with variations on NaOH concentration. The maximum magnetization for the sample with variations on synthesis temperature varied from 4.4 emu/g to 5.7 emu/g due to its crystal structures.
Thermal conductivity of lunar regolith simulant JSC-1A under vacuum
NASA Astrophysics Data System (ADS)
Sakatani, Naoya; Ogawa, Kazunori; Arakawa, Masahiko; Tanaka, Satoshi
2018-07-01
Many air-less planetary bodies, including the Moon, asteroids, and comets, are covered by regolith. The thermal conductivity of the regolith is an essential parameter controlling the surface temperature variation. A thermal conductivity model applicable to natural soils as well as planetary surface regolith is required to analyze infrared remote sensing data. In this study, we investigated the temperature and compressional stress dependence of the thermal conductivity of the lunar regolith simulant JSC-1A, and the temperature dependence of sieved JSC-1A samples under vacuum conditions. We confirmed that a series of the experimental data for JSC-1A are fitted well by our analytical model of the thermal conductivity (Sakatani et al., 2017). Comparison with the calibration data of the sieved samples with those for original JSC-1A indicates that the thermal conductivity of natural samples with a wide grain size distribution can be modeled as mono-sized grains with a volumetric median size. The calibrated model can be used to estimate the volumetric median grain size from infrared remote sensing data. Our experiments and the calibrated model indicates that uncompressed JSC-1A has similar thermal conductivity to lunar top-surface materials, but the lunar subsurface thermal conductivity cannot be explained only by the effects of the density and self-weighted compressional stress. We infer that the nature of the lunar subsurface regolith grains is much different from JSC-1A and lunar top-surface regolith, and/or the lunar subsurface regolith is over-consolidated and the compressional stress higher than the hydrostatic pressure is stored in the lunar regolith layer.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Pawellek, Nicole; Krivov, Alexander V.; Marshall, Jonathan P.
The radii of debris disks and the sizes of their dust grains are important tracers of the planetesimal formation mechanisms and physical processes operating in these systems. Here we use a representative sample of 34 debris disks resolved in various Herschel Space Observatory (Herschel is an ESA space observatory with science instruments provided by European-led Principal Investigator consortia and with important participation from NASA) programs to constrain the disk radii and the size distribution of their dust. While we modeled disks with both warm and cold components, and identified warm inner disks around about two-thirds of the stars, we focusmore » our analysis only on the cold outer disks, i.e., Kuiper-belt analogs. We derive the disk radii from the resolved images and find a large dispersion for host stars of any spectral class, but no significant trend with the stellar luminosity. This argues against ice lines as a dominant player in setting the debris disk sizes, since the ice line location varies with the luminosity of the central star. Fixing the disk radii to those inferred from the resolved images, we model the spectral energy distribution to determine the dust temperature and the grain size distribution for each target. While the dust temperature systematically increases toward earlier spectral types, the ratio of the dust temperature to the blackbody temperature at the disk radius decreases with the stellar luminosity. This is explained by a clear trend of typical sizes increasing toward more luminous stars. The typical grain sizes are compared to the radiation pressure blowout limit s {sub blow} that is proportional to the stellar luminosity-to-mass ratio and thus also increases toward earlier spectral classes. The grain sizes in the disks of G- to A-stars are inferred to be several times s {sub blow} at all stellar luminosities, in agreement with collisional models of debris disks. The sizes, measured in the units of s {sub blow}, appear to decrease with the luminosity, which may be suggestive of the disk's stirring level increasing toward earlier-type stars. The dust opacity index β ranges between zero and two, and the size distribution index q varies between three and five for all the disks in the sample.« less
NASA Astrophysics Data System (ADS)
Lu, Wei; Huang, Ping; Wang, Yuxin; Yan, Biao
2013-07-01
In this paper, Nb element was partially replaced by V element in Finemet-type Fe73Cu1Nb3.5-xVxSi13.5B9 (x = 1, 1.5, 2) alloys and the effect of annealing temperatures on the microstructure and AC magnetic properties of the samples are studied. The annealing temperatures affect the grain sizes of the bcc α-Fe phase greatly. When the annealing temperature is between 540-560°C, the samples have better AC magnetic properties than the samples annealed at other temperatures. The optimized annealing temperature of the studied samples is around 560°C. The coercivity and iron loss of the V2 sample is a little bit higher than that of V1 and V1.5 alloys while the amplitude permeability of V2 alloy is larger than that of V1 and V1.5, which indicate that the content of V element has strong influence on the magnetic properties of nanocrystalline soft magnetic alloys.
Annealing effects in plated-wire memory elements. II - Recrystallization in Permalloy films.
NASA Technical Reports Server (NTRS)
Marquardt, S. J.; Kench, J. R.
1971-01-01
Results of grain-size measurements in Permalloy platings suggest that recrystallization is possible at temperatures as low as 200 C, but that it is an extremely heterogeneous process. No worthwhile correlation was found to exist between observed grain size and magnetic dispersion in samples aged in the temperature range from 180 to 230 C. It is suggested that the magnetic aging which occurs under these conditions may be due to some other diffusion-controlled process than recrystallization; a process such as chemical homogenization is tentatively preferred.
High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys
Aydogan, E.; El-Atwani, O.; Takajo, S.; ...
2018-02-09
In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less
NASA Astrophysics Data System (ADS)
Krishnan, Vinoadh Kumar; Sinnaeruvadi, Kumaran; Verma, Shailendra Kumar; Dash, Biswaranjan; Agrawal, Priyanka; Subramanian, Karthikeyan
2017-08-01
The present work deals with synthesis, characterisation and elevated temperature mechanical property evaluation of V-4Cr-4Ti and oxide (yttria = 0.3, 0.6 and 0.9 at%) dispersion strengthened V-4Cr-4Ti alloy processed by mechanical alloying and field-assisted sintering, under optimal conditions. Microstructural parameters of both powder and sintered samples were deduced by X-ray diffraction (XRD) and further confirmed with high resolution transmission electron microscopy. Powder diffraction and electron microscopy study show that ball milling of starting elemental powders (V-4Cr-4Ti) with and without yttria addition has resulted in single phase α-V (V-4Cr-4Ti) alloy. Wherein, XRD and electron microscopy images of sintered samples have revealed phase separation (viz., Cr-V and Ti-V) and domain size reduction, with yttria addition. The reasons behind phase separation and domain size reduction with yttria addition during sintering are extensively discussed. Microhardness and high temperature compression tests were done on sintered samples. Yttria addition (0.3 and 0.6 at.%) increases the elevated temperature compressive strength and strain hardening exponent of α-V alloys. High temperature compression test of 0.9 at% yttria dispersed α-V alloy reveals a glassy behaviour.
High temperature microstructural stability and recrystallization mechanisms in 14YWT alloys
DOE Office of Scientific and Technical Information (OSTI.GOV)
Aydogan, E.; El-Atwani, O.; Takajo, S.
In-situ neutron diffraction experiments were performed on room temperature compressed 14YWT nanostructured ferritic alloys at 1100°C and 1150°C to understand their thermally activated static recrystallization mechanisms. The existence of high density of Y-Ti-O rich nano-oxides (<5 nm) shift the recrystallization temperature up due to Zener pinning of the grain boundaries, making these materials attractive for high temperature applications. This study serves to quantify the texture evolution in-situ and understand the effect of particles on the recrystallization mechanisms in 14YWT alloys. We have shown, both experimentally and theoretically, that there is considerable recovery in the 20% compressed sample after 6.5 hmore » annealing at 1100°C while recrystallization occurs within an hour of annealing at 1100°C and 1150°C in the 60% compressed samples. Moreover, the 60% compressed samples show {112}<110> and {112}<111> texture components during annealing, in contrast to the conventional recrystallization textures in body centered cubic alloys. Furthermore, nano-oxide size, shape, density and distribution are considerably different in unrecrystallized and abnormally grown grains. Transmission electron microscopy analysis shows that oxide particles having a size between 5 and 30 nm play a critical role for recrystallization mechanisms in 14YWT nanostructured ferritic alloys.« less
A small-plane heat source method for measuring the thermal conductivities of anisotropic materials
NASA Astrophysics Data System (ADS)
Cheng, Liang; Yue, Kai; Wang, Jun; Zhang, Xinxin
2017-07-01
A new small-plane heat source method was proposed in this study to simultaneously measure the in-plane and cross-plane thermal conductivities of anisotropic insulating materials. In this method the size of the heat source element is smaller than the sample size and the boundary condition is thermal insulation due to no heat flux at the edge of the sample during the experiment. A three-dimensional model in a rectangular coordinate system was established to exactly describe the heat transfer process of the measurement system. Using the Laplace transform, variable separation, and Laplace inverse transform methods, the analytical solution of the temperature rise of the sample was derived. The temperature rises calculated by the analytical solution agree well with the results of numerical calculation. The result of the sensitivity analysis shows that the sensitivity coefficients of the estimated thermal conductivities are high and uncorrelated to each other. At room temperature and in a high-temperature environment, experimental measurements of anisotropic silica aerogel were carried out using the traditional one-dimensional plane heat source method and the proposed method, respectively. The results demonstrate that the measurement method developed in this study is effective and feasible for simultaneously obtaining the in-plane and cross-plane thermal conductivities of the anisotropic materials.
Magnetoabsorption and magnetic hysteresis in Ni ferrite nanoparticles
NASA Astrophysics Data System (ADS)
Hernández-Gómez, P.; Muñoz, J. M.; Valente, M. A.; Torres, C.; de Francisco, C.
2013-01-01
Nickel ferrite nanoparticles were prepared by a modified sol-gel technique employing coconut oil, and then annealed at different temperatures in 400-1200 °C range. This route of preparation has revealed to be one efficient and cheap technique to obtain high quality nickel ferrite nanosized powder. Sample particles sizes obtained with XRD data and Scherrer's formula lie in 13 nm to 138 nm, with increased size with annealing temperature. Hysteresis loops have been obtained at room temperature with an inductive method. Magnetic field induced microwave absorption in nanoscale ferrites is a recent an active area of research, in order to characterize and explore potential novel applications. In the present work microwave magnetoabsorption data of the annealed nickel ferrite nanoparticles are presented. These data have been obtained with a system based on a network analyzer that operates in the frequency range 0 - 8.5 GHz. At fields up to 400 mT we can observe a peak according to ferromagnetic resonance theory. Sample annealed at higher temperature exhibits different absorption, coercivity and saturation magnetization figures, revealing its multidomain character.
Crystal growth in zinc borosilicate glasses
NASA Astrophysics Data System (ADS)
Kullberg, Ana T. G.; Lopes, Andreia A. S.; Veiga, João P. B.; Monteiro, Regina C. C.
2017-01-01
Glass samples with a molar composition (64+x)ZnO-(16-x)B2O3-20SiO2, where x=0 or 1, were successfully synthesized using a melt-quenching technique. Based on differential thermal analysis data, the produced glass samples were submitted to controlled heat-treatments at selected temperatures (610, 615 and 620 °C) during various times ranging from 8 to 30 h. The crystallization of willemite (Zn2SiO4) within the glass matrix was confirmed by means of X-ray diffraction (XRD) and scanning electron microscopy (SEM). Under specific heat-treatment conditions, transparent nanocomposite glass-ceramics were obtained, as confirmed by UV-vis spectroscopy. The influence of temperature, holding time and glass composition on crystal growth was investigated. The mean crystallite size was determined by image analysis on SEM micrographs. The results indicated an increase on the crystallite size and density with time and temperature. The change of crystallite size with time for the heat-treatments at 615 and 620 °C depended on the glass composition. Under fixed heat-treatment conditions, the crystallite density was comparatively higher for the glass composition with higher ZnO content.
NASA Astrophysics Data System (ADS)
Erdemi, H.; Sözeri, H.; Şenel, M.; Baykal, A.
2012-08-01
Polyvinylimidazole (PVIm)-grafted superparamagnetic iron oxide nanoparticles (SPION) (Si-PVIm-grafted Fe3O4 NPs) were prepared by grafting of telomere of PVIm on the SPION. The product identified as magnetite, which has an average crystallite size of 9 ± 2 nm as estimated from X-ray line profile fitting. Particle size was estimated as 10.0 ± 0.5 nm from TEM micrographs. Mean particle size is found as 8.4 ± 1.0 nm which agrees well with the values calculated from XRD patterns (9 ± 2 nm). Vibrating Sample Magnetometer (VSM) analysis explained the superparamagnetic nature of the nanocomposite. Thermogravimetric analysis showed that the Si-Imi is 25 % of the Si-PVIm-grafted SPION, which means an inorganic content is about 75 %. Detailed electrical and dielectric properties of the properties of the product are also presented. The conductivity of the sample increases significantly with temperature and has the value in the range of 1.14 × 10-7-1.78 × 10-4 S cm-1. Analysis of the real and imaginary parts of the permittivities indicated temperature and frequency dependency representing interfacial polarization and temperature-assisted reorganization effects.
Ultra sound absorption measurements in rock samples at low temperatures
NASA Technical Reports Server (NTRS)
Herminghaus, C.; Berckhemer, H.
1974-01-01
A new technique, comparable with the reverberation method in room acoustics, is described. It allows Q-measurements at rock samples of arbitrary shape in the frequency range of 50 to 600 kHz in vacuum (.1 mtorr) and at low temperatures (+20 to -180 C). The method was developed in particular to investigate rock samples under lunar conditions. Ultrasound absorption has been measured at volcanics, breccia, gabbros, feldspar and quartz of different grain size and texture yielding the following results: evacuation raises Q mainly through lowering the humidity in the rock. In a dry compact rock, the effect of evacuation is small. With decreasing temperature, Q generally increases. Between +20 and -30 C, Q does not change much. With further decrease of temperature in many cases distinct anomalies appear, where Q becomes frequency dependent.
Effect of ultrasonic treatment and temperature on nanocrystalline TiO 2
NASA Astrophysics Data System (ADS)
Kim, D. H.; Ryu, H. W.; Moon, J. H.; Kim, J.
Nanocrystalline TiO 2 particles were precipitated from the ethanol solution of titanium isopropoxide (Ti(O- iPr) 4) and H 2O 2 by refluxing at 80 °C for 48 h. The obtained particles were filtered and dried at 100 °C for 12 h. The dried powder itself, the sample with heating at 400 °C, and the sample with ultrasonically treating were prepared to investigate the effects of post treatments on materials characteristics and electrochemical properties of nanocrystalline TiO 2. The X-ray diffraction patterns of all of the samples were fitted well to the anatase phase. The field emission-TEM image of as-prepared sample shows a uniform spherical morphology with 5 nm particle size and the sample heated at 400 °C shows slightly increased particle size of about 10 nm while maintaining spherical shape. The sample treated with ultrasonic for 5 h or more at room temperature shows high aspect ratio particle shape with an average diameter of 5 nm and a length of 20 nm. According to the results of the electrochemical testing, as-prepared sample, the sample heated at 400 °C for 3 h, and the sample treated with ultrasonic show initial capacities of 270, 310 and 340 mAh g -1, respectively.
Thermal Infrared Spectra of a Suite of Forsterite Samples and Ab-initio Modelling of theirs Spectra
NASA Astrophysics Data System (ADS)
Maturilli, A.; Stangarone, C.; Helbert, J.; Tribaudino, M.; Prencipe, M.
2017-12-01
Forsterite is the dominating component in olivine, a major constituent in ultrafemic rocks, as well as planetary bodies. Messenger X-ray spectrometer has shown that Mg-rich silicate minerals, such as enstatite and forsterite, dominate Mercury's surface (Weider et al 2012). A careful and detailed acquaintance with the forsterite spectral features and their dependence wrt environmental conditions on Mercury is needed to interpret the remote sensing data from previous and forthcoming missions. We propose an experimental vs calculation approach to reproduce and describe the spectral features of forsterite. TIR emissivity measurements are performed by the Planetary Spectroscopy Laboratory (PSL) of DLR. PSL offers the unique capability to measure the emissivity of samples at temperature up to 1000K under vacuum conditions. TIR emissivity and reflectance measurements are performed on 11 olivine samples having a different composition within the forsterite-fayalite series. When available, the sample has been measured in 2 different grain sizes (<25µm and 125-250µm ranges). Emissivity measurements are taken for temperatures from 300K to 900K step 100K in the 1-100µm spectral range. Modelling is based on ab initio calculation techniques, which allow reproducing properties of crystals, at any P/T condition, with the least possible amount of a priori empirical information. Spectra are calculated evaluating vibrational frequencies at different volume cell, here 0K, 300K and 1000K (extreme situations), taking into account zero point effects. The aim of this work is to study experimentally the effects of temperature, composition and grain sizes on emissivity band minima shifts. The outcomes will benefit the modelling of emissivity spectra with ab initio methods, already successfully enabling to foresee the bands shift due to temperature and composition, but not taking into account band shape due to grain size variations. Considering the chameleon-like effects of Mercury surface already observed (Helbert et al. 2013), this study wants to point out the main spectral features due to the composition and temperature. Our results are used to create a theoretical background to interpret the high temperature infrared emissivity spectra from MERTIS onboard the ESA BepiColombo mission to Mercury (Helbert et al. 2010).
Room-temperature processing of CdSe quantum dots with tunable sizes
NASA Astrophysics Data System (ADS)
Joo, So-Yeong; Jeong, Da-Woon; Lee, Chan-Gi; Kim, Bum-Sung; Park, Hyun-Su; Kim, Woo-Byoung
2017-06-01
In this work, CdSe quantum dots (QDs) with tunable sizes have been fabricated via photo-induced chemical etching at room temperature, and the related reaction mechanism was investigated. The surface of QDs was oxidized by the holes generated through photon irradiation of oxygen species, and the obtained oxide layer was dissolved in an aqueous solution of 3-amino-1-propanol (APOL) with an APOL:H2O volume ratio of 5:1. The generated electrons promoted QD surface interactions with amino groups, which ultimately passivated surface defects. The absorption and photoluminescence emission peaks of the produced QDs were clearly blue-shifted about 26 nm with increasing time, and the resulting quantum yield for an 8 h etched sample was increased from 20% to 26%, as compared to the initial sample.
Ahn, WonSool; Lee, Joon-Man
2015-11-01
The effects of MWCNT on the cell sizes, cell uniformities, thermal conductivities, bulk densities, foaming kinetics, and compressive mechanical properties of the rigid PUFs were investigated. To obtain the better uniform dispersed state of MWCNT, grease-type master batch of MWCNT/surfactant was prepared by three-roll mill. Average cell size of the PUF samples decreased from 185.1 for the neat PUF to 162.9 μm for the sample of 0.01 phr of MWCNT concentration. Cell uniformity was also enhanced showing the standard cell-size deviation of 61.7 and 35.2, respectively. While the thermal conductivity of the neat PUF was 0.0222 W/m(o)K, that of the sample with 0.01 phr of MWCNT showed 0.0204 W/m(o)K, resulting 8.2% reduction of the thermal conductivity. Bulk density of the PUF samples was observed as nearly the same values as 30.0 ± 1.0 g/cm3 regardless of MWCNT. Temperature profiles during foaming process showed that an indirect indication of the nucleation effect of MWCNT for the PUF foaming system, showing faster and higher temperature rising with time. The compressive yield stress is nearly the same as 0.030 x 10(5) Pa regardless of MWCNT.
Green synthesis and characterization of ANbO3 (A = Na, K) nanopowders fabricated using a biopolymer
NASA Astrophysics Data System (ADS)
Khorrami, Gh. H.; Mousavi, M.; Khayatian, S. A.; Kompany, A.; Khorsand Zak, A.
2017-10-01
Lead-free sodium niobate (NaNbO3, NN) and potassium niobate (KNbO3, KN) nanopowders were successfully synthesized by a simple and green synthesis process in gelatin media. Gelatin, which is a biopolymer, was used as stabilizer. In order to determine the lowest calcination temperature needed to obtain pure NN and KN nanopowders, the produced gels were analyzed by thermogravometric analyzer (TGA). The produced gels were calcined at 500∘C and 600∘C. The structural and optical properties of the prepared powders were examined using X-ray diffraction (XRD) technique, transmission electron microscopy (TEM), and UV-Vis spectroscopy. The XRD results revealed that pure phase NN and KN nanopowders were formed at low temperature calcination of 500∘C and 600∘C, respectively. The Scherrer formula and size-strain plot (SSP) method were employed to estimate crystallite size and lattice strain of the samples. The TEM images show that the NN and KN samples calcined at 600∘C have cubic shape with an average particle size of 60.95 and 39.29 nm, respectively. The optical bandgap energy of the samples was calculated using UV-Vis diffused reflectance spectra of the samples and Kubelka-Munck relation.
Deactivation of Escherichia coli by the plasma needle
NASA Astrophysics Data System (ADS)
Sladek, R. E. J.; Stoffels, E.
2005-06-01
In this paper we present a parameter study on deactivation of Escherichia coli (E. coli) by means of a non-thermal plasma (plasma needle). The plasma needle is a small-sized (1 mm) atmospheric glow sustained by radio-frequency excitation. This plasma will be used to disinfect heat-sensitive objects; one of the intended applications is in vivo deactivation of dental bacteria: destruction of plaque and treatment of caries. We use E. coli films plated on agar dishes as a model system to optimize the conditions for bacterial destruction. Plasma power, treatment time and needle-to-sample distance are varied. Plasma treatment of E. coli films results in formation of a bacteria-free void with a size up to 12 mm. 104-105 colony forming units are already destroyed after 10 s of treatment. Prolongation of treatment time and usage of high powers do not significantly improve the destruction efficiency: short exposure at low plasma power is sufficient. Furthermore, we study the effects of temperature increase on the survival of E. coli and compare it with thermal effects of the plasma. The population of E. coli heated in a warm water bath starts to decrease at temperatures above 40°C. Sample temperature during plasma treatment has been monitored. The temperature can reach up to 60°C at high plasma powers and short needle-to-sample distances. However, thermal effects cannot account for bacterial destruction at low power conditions. For safe and efficient in vivo disinfection, the sample temperature should be kept low. Thus, plasma power and treatment time should not exceed 150 mW and 60 s, respectively.
Size effects on electrical properties of chemically grown zinc oxide nanoparticles
NASA Astrophysics Data System (ADS)
Rathod, K. N.; Joshi, Zalak; Dhruv, Davit; Gadani, Keval; Boricha, Hetal; Joshi, A. D.; Solanki, P. S.; Shah, N. A.
2018-03-01
In the present article, we study ZnO nanoparticles grown by cost effective sol–gel technique for various electrical properties. Structural studies performed by x-ray diffraction (XRD) revealed hexagonal unit cell phase with no observed impurities. Transmission electron microscopy (TEM) and particle size analyzer showed increased average particle size due to agglomeration effect with higher sintering. Dielectric constant (ε‧) decreases with increase in frequency because of the disability of dipoles to follow higher electric field. With higher sintering, dielectric constant reduced owing to the important role of increased formation of oxygen vacancy defects. Universal dielectric response (UDR) was verified by straight line fitting of log (fε‧) versus log (f) plots. All samples exhibit UDR behavior and with higher sintering more contribution from crystal cores. Impedance studies suggest an important role of boundary density while Cole–Cole (Z″ versus Z‧) plots have been studied for the relaxation behavior of the samples. Average normalized change (ANC) in impedance has been studied for all the samples wherein boundaries play an important role. Frequency dependent electrical conductivity has been understood on the basis of Jonscher’s universal power law. Jonscher’s law fits suggest that conduction of charge carrier is possible in the context of correlated barrier hopping (CBH) mechanism for lower temperature sintered sample while for higher temperature sintered ZnO samples, Maxwell–Wagner (M–W) relaxation process has been determined.
NASA Astrophysics Data System (ADS)
Yuan, Y.; Greuner, H.; Böswirth, B.; Krieger, K.; Luo, G.-N.; Xu, H. Y.; Fu, B. Q.; Li, M.; Liu, W.
2013-02-01
Short pulse heat loads expected for vertical displacement events (VDEs) in ITER were applied in the high heat flux (HHF) test facility GLADIS at IPP-Garching onto samples of rolled W. Pulsed neutral beams with the central heat flux of 23 MW/m2 were applied for 0.5, 1.0 and 1.5 s, respectively. Rapid recrystallization of the adiabatically loaded 3 mm thick samples was observed when the pulse duration was up to 1.0 s. Grains grew markedly following recrystallization with increasing pulse length. The recrystallization temperature and temperature dependence of the recrystallized grain size were also investigated. The results showed that the recrystallization temperature of the W grade was around 2480 °C under the applied heat loading condition, which was nearly 1150 °C higher than the conventional recrystallization temperature, and the grains were much finer. A linear relationship between the logarithm of average grain size (ln d) and the inverse of maximum surface temperature (1/Tmax) was found and accordingly the activation energy for grain growth in temperature evolution up to Tmax in 1.5 s of the short pulse HHF load was deduced to be 4.1 eV. This provided an effective clue to predict the structure evolution under short pulse HHF loads.
Fortpied, Juliette; Wauters, Florence; Rochart, Christelle; Hermand, Philippe; Hoet, Bernard; Moniotte, Nicolas; Vojtek, Ivo
2018-01-01
ABSTRACT Accidental exposure of a vaccine containing an aluminum-salt adjuvant to temperatures below 0°C in the cold chain can lead to freeze damage. Our study evaluated the potential for freeze damage in a licensed aluminum-salt-containing protein-D-conjugated pneumococcal vaccine (PHiD-CV; Synflorix, GSK) in conditions that included static storage, single subzero-temperature excursions, and simulated air-freight transportation. Several parameters were assessed including freezing at subzero temperatures, aluminum-salt-particle size, antigen integrity and immunogenicity in the mouse. The suitability of the WHO's shake test for identifying freeze-damaged vaccines was also assessed. During subzero-temperature excursions, the mean temperatures at which PHiD-CV froze (−16.7°C to −18.1°C) appeared unaffected by the type of vaccine container (two-dose or four-dose vial, or single-dose syringe), vaccine batch, rotational agitation, or the rate of temperature decline (−0.5 to −10°C/hour). At constant subzero temperature and in simulated air-freight transportation, the freezing of PHiD-CV appeared to be promoted by vibration. At −5°C, no PHiD-CV sample froze in static storage (>1 month), whereas when subjected to vibration, a minority of samples froze (7/21, 33%) within 18 hours. At −8°C with vibration, nearly all (5/6, 83%) samples froze. In these vibration regimes, the shake test identified most samples that froze (10/12, 93%) except two in the −5°C regime. Nevertheless, PHiD-CV-antigen integrity appeared unaffected by freezing up to −20°C or by vibration. And although aluminum-salt-particle size was increased only by freezing at −20°C, PHiD-CV immunogenicity appeared only marginally affected by freezing at −20°C. Therefore, our study supports the use of the shake test to exclude freeze-damaged PHiD-CV in the field. PMID:29337646
Morishige, Kunimitsu; Tateishi, Masayoshi; Hirose, Fumi; Aramaki, Kenji
2006-10-24
To verify pore blocking controlled desorption in ink-bottle pores, we measured the temperature dependence of the adsorption-desorption isotherms of nitrogen on four kinds of KIT-5 samples with expanded cavities hydrothermally treated for different periods of time at 393 K. In the samples, almost spherical cavities are arranged in a face-centered cubic array and the cavities are connected through small channels. The pore size of the channels increased with an increase in the hydrothermal treatment time. At lower temperatures a steep desorption branch changed to a gradual one as the hydrothermal treatment was prolonged. For the sample hydrothermally treated only for 1 day, the rectangular hysteresis loop shrank gradually with increasing temperature while keeping its shape. The temperature dependence of the evaporation pressure observed was identical with that expected for cavitation-controlled desorption. On the other hand, for the samples hydrothermally treated for long times, the gradual desorption branch became a sharp one with increasing temperature. This strongly suggests that the desorption mechanism is altered from pore blocking to cavitation with temperature. Application of percolation theory to the pore blocking controlled desorption observed here is discussed.
Lewan, Michael; Sonnenfeld, Mark D.
2017-01-01
Low-temperature hydrous pyrolysis (LTHP) at 300°C (572°F) for 24 h released retained oils from 12- to 20-meshsize samples of mature Niobrara marly chalk and marlstone cores. The released oil accumulated on the water surface of the reactor, and is compositionally similar to oil produced from the same well. The quantities of oil released from the marly chalk and marlstone by LTHP are respectively 3.4 and 1.6 times greater than those determined by tight rock analyses (TRA) on aliquots of the same samples. Gas chromatograms indicated this difference is a result of TRA oils losing more volatiles and volatilizing less heavy hydrocarbons during collection than LTHP oils. Characterization of the rocks before and after LTPH by programmable open-system pyrolysis (HAWK) indicate that under LTHP conditions no significant oil is generated and only preexisting retained oil is released. Although LTHP appears to provide better predictions of quantity and quality of retained oil in a mature source rock, it is not expected to replace the more time and sample-size efficacy of TRA. However, LTHP can be applied to composited samples from key intervals or lithologies originally recognized by TRA. Additional studies on duration, temperature, and sample size used in LTHP may further optimize its utility.
Influence of warm rolling temperature on ferrite recrystallization in low C and IF steels
NASA Astrophysics Data System (ADS)
Barnett, Matthew Robert
Experiments involving single pass laboratory rolling and isothermal salt bath annealing were carried out; three steels were studied: a titanium stabilized interstitial free grade and two low carbon grades, one of which contained a particularly low level of manganese (˜0.009wt.%). The two low carbon grades were produced such that any complication from AlN precipitation was avoided. X-ray, neutron diffraction, optical metallography and mechanical testing measurements were carried out on the samples before and after annealing. The main aim of this work was to further the understanding of the metallurgy of recrystallization after ferrite rolling at temperatures between room temperature and 700sp°C. Deformation textures, recrystallization kinetics, final grain sizes and recrystallization textures were quantified for all the samples and experimental conditions. A major conclusion based on these data is that the influence of rolling temperature is far greater in the low carbon samples than in the IF grade. Indeed, the IF results alter only marginally with increasing temperature. In the low carbon grades, however, the rolling texture sharpens, recrystallization slows, the final grain size coarsens, and the recrystallization texture changes when the rolling temperature is increased. This distinct difference between the two steel types is explained in terms of their contrasting deformation behaviors. Solute carbon and nitrogen in the low carbon grades interact with dislocations causing high stored energy levels after low temperature rolling (due to dynamic strain aging) and high strain rate sensitivities during high temperature rolling (due to the solute drag of dislocations in the transition region between DSA and DRC). Nucleation during subsequent recrystallization is strongly influenced by both the stored energy and the strain rate sensitivity. The latter affects the occurrence of the flow localisations that enhance nucleation.
Size-selective separation of polydisperse gold nanoparticles in supercritical ethane.
Williams, Dylan P; Satherley, John
2009-04-09
The aim of this study was to use supercritical ethane to selectively disperse alkanethiol-stabilized gold nanoparticles of one size from a polydisperse sample in order to recover a monodisperse fraction of the nanoparticles. A disperse sample of metal nanoparticles with diameters in the range of 1-5 nm was prepared using established techniques then further purified by Soxhlet extraction. The purified sample was subjected to supercritical ethane at a temperature of 318 K in the pressure range 50-276 bar. Particles were characterized by UV-vis absorption spectroscopy, TEM, and MALDI-TOF mass spectroscopy. The results show that with increasing pressure the dispersibility of the nanoparticles increases, this effect is most pronounced for smaller nanoparticles. At the highest pressure investigated a sample of the particles was effectively stripped of all the smaller particles leaving a monodisperse sample. The relationship between dispersibility and supercritical fluid density for two different size samples of alkanethiol-stabilized gold nanoparticles was considered using the Chrastil chemical equilibrium model.
Lee, Jae Chun; Kim, Yun-Il; Lee, Dong-Hun; Kim, Won-Jun; Park, Sung; Lee, Dong Bok
2011-08-01
Several kinds of nano-sized silica-based thermal insulation were prepared by dry processing of mixtures consisting of fumed silica, ceramic fiber, and a SiC opacifier. Infiltration of phenolic resin solution into the insulation, followed by hot-pressing, was attempted to improve the mechanical strength of the insulation. More than 22% resin content was necessary to increase the strength of the insulation by a factor of two or more. The structural integrity of the resin-infiltrated samples could be maintained, even after resin burn-out, presumably due to reinforcement from ceramic fibers. For all temperature ranges and similar sample bulk density values, the thermal conductivities of the samples after resin burn-out were consistently higher than those of the samples obtained from the dry process. Mercury intrusion curves indicated that the median size of the nanopores formed by primary silica aggregates in the samples after resin burn-out is consistently larger than that of the sample without resin infiltration.
NASA Astrophysics Data System (ADS)
Archer, P. D., Jr.; Ming, D. W.; Sutter, B.; Niles, P. B.; Eigenbrode, J. L.
2015-12-01
Evolved Gas Analysis (EGA), which involves heating a sample and monitoring the gases released, has been performed on Mars by the Viking gas chromatography/mass spectrometry instruments, the Thermal and Evolved Gas Analyzer (TEGA) on the Phoenix lander, and the Sample Analysis at Mars (SAM) instrument on the Mars Science Laboratory. All of these instruments detected CO2 released during sample analysis at abundances of ~0.1 to 5 wt% assuming a carbonate source. The source of the CO2 can be constrained by evaluating the temperature of the gas release, a capability of both the TEGA and SAM instruments. The samples analyzed by SAM show that the majority of the CO2is released below 400 °C, much lower than traditional carbonate decomposition temperatures which can be as low as 400 °C for some siderites, with magnesites and calcites decomposing at even higher temperatures. In addition to mineralogy, decomposition temperature can depend on particle size (among other factors). If carbonates formed on Mars under low temperature and relative humidity conditions, the resulting small particle size (nanophase) carbonates could have low decomposition temperatures. We have found that calcite can be synthesized by exposing CaO to water vapor and CO2 and that the resulting mineral has an EGA peak of ~550 °C for CO2, which is about 200 °C lower than for other calcites. Work is ongoing to produce Fe and Mg-bearing carbonates using the same process. Current results suggest that nanophase calcium carbonates cannot explain the CO2 released from martian samples. If the decomposition temperatures of Mg and Fe-bearing nanophase carbonates are not significantly lower than 400 °C, other candidate sources include oxalates and carboxylated organic molecules. If present, the abundance of organic carbon in these samples could be > 0.1 wt % (1000s of ppm), a signficant departure from the paradigm of the organic-poor Mars based on Viking results.
First-Principles Determination of Ultralow Thermal Conductivity of monolayer WSe2
NASA Astrophysics Data System (ADS)
Zhou, Wu-Xing; Chen, Ke-Qiu
2015-10-01
By using first-principles calculations combined with the phonon Boltzmann transport equation, we systematically investigate the phonon transport of monolayer WSe2. Compared with other 2D materials, the monolayer WSe2 is found to have an ultralow thermal conductivity due to the ultralow Debye frequency and heavy atom mass. The room temperature thermal conductivity for a typical sample size of 1 μm is 3.935 W/m K, which is one order of magnitude lower than that of MoS2. And the room temperature thermal conductivity can be further decreased by about 95% in 10 nm sized samples. Moreover, we also find the ZA phonons have the dominant contribution to the thermal conductivity, and the relative contribution is almost 80% at room temperature, which is remarkably higher than that for monolayer MoS2. This is because the ZA phonons have longer lifetime than that of LA and TA phonons in monolayer WSe2.
Feichtmeier, Nadine S; Leopold, Kerstin
2014-06-01
In this work, we present a fast and simple approach for detection of silver nanoparticles (AgNPs) in biological material (parsley) by solid sampling high-resolution-continuum source atomic absorption spectrometry (HR-CS AAS). A novel evaluation strategy was developed in order to distinguish AgNPs from ionic silver and for sizing of AgNPs. For this purpose, atomisation delay was introduced as significant indication of AgNPs, whereas atomisation rates allow distinction of 20-, 60-, and 80-nm AgNPs. Atomisation delays were found to be higher for samples containing silver ions than for samples containing silver nanoparticles. A maximum difference in atomisation delay normalised by the sample weight of 6.27 ± 0.96 s mg(-1) was obtained after optimisation of the furnace program of the AAS. For this purpose, a multivariate experimental design was used varying atomisation temperature, atomisation heating rate and pyrolysis temperature. Atomisation rates were calculated as the slope of the first inflection point of the absorbance signals and correlated with the size of the AgNPs in the biological sample. Hence, solid sampling HR-CS AAS was proved to be a promising tool for identifying and distinguishing silver nanoparticles from ionic silver directly in solid biological samples.
NASA Astrophysics Data System (ADS)
Ismail, Ismayadi; Hashim, Mansor; Kanagesan, Samikannu; Ibrahim, Idza Riati; Nazlan, Rodziah; Wan Ab Rahman, Wan Norailiana; Abdullah, Nor Hapishah; Mohd Idris, Fadzidah; Bahmanrokh, Ghazaleh; Shafie, Mohd Shamsul Ezzad; Manap, Masni
2014-02-01
We report on an investigation to unravel the dependence of magnetic properties on microstructure while they evolve in parallel under the influence of sintering temperature of a single sample of Ni0.5Zn0.5Fe2O4 synthesized via mechanical alloying. A single sample, instead of the normally practiced approach of using multiple samples, was sintered at various sintering temperatures from 500 °C to 1400 °C. The morphology of the samples was studied by means of scanning electron microscopy (SEM) equipped with EDX; density measurement was conducted using the Archimedes principle; and hysteresis measurement was carried out using a B-H hysteresisgraph system. XRD data showed that the first appearance of a single phase was at 800 °C and an amorphous phase was traced at lower sintering temperatures. We correlated the microstructure and the magnetic properties and showed that the important grain-size threshold for the appearance of significant ordered magnetism (mainly ferromagnetism) was about ≥0.3 µm. We found that there were three stages of magnetic phase evolution produced via the sintering process with increasing temperatures. The first stage was dominated by paramagnetic states with some superparamagnetic behavior; the second stage was influenced by moderately ferromagnetic states and some paramagnetic states; and the third stage consisted of strongly ferromagnetic states with negligible paramagnetic states. We found that three factors sensitively influenced the sample's content of ordered magnetism—the ferrite-phase crystallinity degree, the number of grains above the critical grain size and the number of large enough grains for domain wall accommodation.
Processing and Characterization of Porous Ti2AlC with Controlled Porosity and Pore Size
2012-09-11
fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size on the room temperature elastic moduli...pressureless- sintered without NaCl pore former, or fabricated by spark plasma sintering , were also characterized. The effects of porosity and/or pore size...as well as several samples sintered using spark plasma sintering (SPS). Furthermore, we demon- strate that the developed methodology can be implemented
NASA Astrophysics Data System (ADS)
Madhusudan, Puttaswamy; Zhang, Jinfeng; Yu, Jiaguo; Cheng, Bei; Xu, Difa; Zhang, Jun
2016-11-01
The optical and catalytic performances of materials strongly depend on their size, morphology, dimensionality and structure. Herein, we demonstrate a facile one-pot template free synthesis of hierarchical CdMoO4 porous microspheres via a simple low temperature oil bath method. The photoactivity of the as-prepared samples was evaluated by photocatalytic decolorization of Methyl Orange (MO) and Methylene Blue (MB) mixed dye aqueous solutions at ambient temperature under full solar spectrum. The results indicated that the concentration of ammonium molybdate and reaction time greatly influence the diameter, average crystallite size, specific surface area, pore structure and photocatalytic activity of the prepared samples. Especially, under the suitable conditions the prepared hierarchical CdMoO porous microspheres exhibited enhanced photocatalytic activity and high stability. Furthermore, it is found that the photocatalytic activity and formation rate of hydroxyl radicals greatly depend on the particle sizes and morphology of as-prepared samples. This work not only demonstrates a simple way to fabricate the hierarchical CdMoO4 porous microspheres but also shows a possibility for utilization of CdMoO4 porous microspheres for the photocatalytic treatment of waste water pollutants.
Grain size dependence of dielectric relaxation in cerium oxide as high-k layer
2013-01-01
Cerium oxide (CeO2) thin films used liquid injection atomic layer deposition (ALD) for deposition and ALD procedures were run at substrate temperatures of 150°C, 200°C, 250°C, 300°C, and 350°C, respectively. CeO2 were grown on n-Si(100) wafers. Variations in the grain sizes of the samples are governed by the deposition temperature and have been estimated using Scherrer analysis of the X-ray diffraction patterns. The changing grain size correlates with the changes seen in the Raman spectrum. Strong frequency dispersion is found in the capacitance-voltage measurement. Normalized dielectric constant measurement is quantitatively utilized to characterize the dielectric constant variation. The relationship extracted between grain size and dielectric relaxation for CeO2 suggests that tuning properties for improved frequency dispersion can be achieved by controlling the grain size, hence the strain at the nanoscale dimensions. PMID:23587419
NASA Astrophysics Data System (ADS)
Kurokawa, Yuichiro; Hihara, Takehiko; Ichinose, Ikuo; Sumiyama, Kenji
2012-07-01
We have produced Sn/Si core-shell cluster assemblies by a plasma-gas-condensation cluster beam deposition apparatus. For the sample with Si content = 12 at. %, the temperature dependence of electrical resistivity exhibits a metallic behavior above 10 K and the onset of superconducting transition below 6.1 K. With decreasing temperature, the thermomagnetic curve for the sample with Si content = 8 at. % begins to decrease steadily toward negative value below 7.7 K, indicating the Meissner effect. An increase in the transition temperature, TC is attributable to exciton-type superconductivity.
Electrophysical Properties of Onion-Like Carbon
NASA Astrophysics Data System (ADS)
Tkachev, E. N.; Romanenko, A. I.; Zhdanov, K. R.; Anikeeva, O. B.; Buryakov, T. I.; Kuznetsov, V. L.; Moseenkov, S. I.
2016-06-01
The paper examines electrophysical properties of onion-like carbon (OLC) samples, where particles have the average size of 4-8 nm and are formed by 5-10 nested fullerene-like spheres connected by 1-3 common curved graphene shells into aggregates with a size of 50-300 nm. We measured the temperature dependence of electrical resistance from 4.2 to 300 K and dependence of magnetoresistance in magnetic fields up to 6 T at the temperature of 4.2 K. Temperature dependences of electrical resistance of samples can be described within the framework of the Mott law with variable hop length for the one-dimensional case or within the framework of the Efros-Shklovskii Coulomb gap. We observed the quadratically increasing positive magnetoresistance up to 6 T associated with compression of wave functions of conduction electrons. Negative magnetoresistance was observed in the range of magnetic fields up to 1-2 T in the case of some samples. This is due to the fact that magnetic field suppresses the contributions to magnetoresistance made by interference effects in the area of hopping conductivity. The measurements were used to estimate the localization radius that is comparable to the diameter of OLC particles (nano-onions).
DOE Office of Scientific and Technical Information (OSTI.GOV)
Asgari, H., E-mail: hamed.asgari@usask.ca; Odeshi, A.G.; Szpunar, J.A.
2015-08-15
The effects of grain size on the dynamic deformation behavior of rolled AZ31B alloy at high strain rates were investigated. Rolled AZ31B alloy samples with grain sizes of 6, 18 and 37 μm, were subjected to shock loading tests using Split Hopkinson Pressure Bar at room temperature and at a strain rate of 1100 s{sup −} {sup 1}. It was found that a double-peak basal texture formed in the shock loaded samples. The strength and ductility of the alloy under the high strain-rate compressive loading increased with decreasing grain size. However, twinning fraction and strain hardening rate were found tomore » decrease with decreasing grain size. In addition, orientation imaging microscopy showed a higher contribution of double and contraction twins in the deformation process of the coarse-grained samples. Using transmission electron microscopy, pyramidal dislocations were detected in the shock loaded sample, proving the activation of pyramidal slip system under dynamic impact loading. - Highlights: • A double-peak basal texture developed in all shock loaded samples. • Both strength and ductility increased with decreasing grain size. • Twinning fraction and strain hardening rate decreased with decreasing grain size. • ‘g.b’ analysis confirmed the presence of dislocations in shock loaded alloy.« less
Yao, Quantong; Sun, Jian; Fu, Yuzhu; Tong, Weiping; Zhang, Hui
2016-01-01
In this paper, a nanocrystalline surface layer without impurities was fabricated on Ti-6Al-4V alloy by means of surface mechanical attrition treatment (SMAT). The grain size in the nanocrystalline layer is about 10 nm and grain morphology displays a random crystallographic orientation distribution. Subsequently, the low-temperature boriding behaviors (at 600 °C) of the SMAT sample, including the phase composition, microstructure, micro-hardness, and brittleness, were investigated in comparison with those of coarse-grained sample borided at 1100 °C. The results showed that the boriding kinetics could be significantly enhanced by SMAT, resulting in the formation of a nano-structured boride layers on Ti-6Al-4V alloy at lower temperature. Compared to the coarse-grained boriding sample, the SMAT boriding sample exhibits a similar hardness value, but improved surface toughness. The satisfactory surface toughness may be attributed to the boriding treatment that was carried out at lower temperature. PMID:28774115
Probabilistic Design of a Mars Sample Return Earth Entry Vehicle Thermal Protection System
NASA Technical Reports Server (NTRS)
Dec, John A.; Mitcheltree, Robert A.
2002-01-01
The driving requirement for design of a Mars Sample Return mission is to assure containment of the returned samples. Designing to, and demonstrating compliance with, such a requirement requires physics based tools that establish the relationship between engineer's sizing margins and probabilities of failure. The traditional method of determining margins on ablative thermal protection systems, while conservative, provides little insight into the actual probability of an over-temperature during flight. The objective of this paper is to describe a new methodology for establishing margins on sizing the thermal protection system (TPS). Results of this Monte Carlo approach are compared with traditional methods.
Numerical study of the process parameters in spark plasma sintering (sps)
NASA Astrophysics Data System (ADS)
Chowdhury, Redwan Jahid
Spark plasma sintering (SPS) is one of the most widely used sintering techniques that utilizes pulsed direct current together with uniaxial pressure to consolidate a wide variety of materials. The unique mechanisms of SPS enable it to sinter powder compacts at a lower temperature and in a shorter time than the conventional hot pressing, hot isostatic pressing and vacuum sintering process. One of the limitations of SPS is the presence of temperature gradients inside the sample, which could result in non-uniform physical and microstructural properties. Detailed study of the temperature and current distributions inside the sintered sample is necessary to minimize the temperature gradients and achieve desired properties. In the present study, a coupled thermal-electric model was developed using finite element codes in ABAQUS software to investigate the temperature and current distributions inside the conductive and non-conductive samples. An integrated experimental-numerical methodology was implemented to determine the system contact resistances accurately. The developed sintering model was validated by a series of experiments, which showed good agreements with simulation results. The temperature distribution inside the sample depends on some process parameters such as sample and tool geometry, punch and die position, applied current and thermal insulation around the die. The role of these parameters on sample temperature distribution was systematically analyzed. The findings of this research could prove very useful for the reliable production of large size sintered samples with controlled and tailored properties.
NASA Astrophysics Data System (ADS)
Jin, Hyung-Ha; Ko, Eunsol; Lim, Sangyeob; Kwon, Junhyun; Shin, Chansun
2017-09-01
We investigated the microstructural and hardness changes in austenitic stainless steel after Fe ion irradiation at 400, 300, and 200 °C using transmission electron microscopy (TEM) and nanoindentation. The size of the Frank loops increased and the density decreased with increasing irradiation temperature. Radiation-induced segregation (RIS) was detected across high-angle grain boundaries, and the degree of RIS increases with increasing irradiation temperature. Ni-Si clusters were observed using high-resolution TEM in the sample irradiated at 400 °C. The results of this work are compared with the literature data of self-ion and proton irradiation at comparable temperatures and damage levels on stainless steels with a similar material composition with this study. Despite the differences in dose rate, alloy composition and incident ion energy, the irradiation temperature dependence of RIS and the size and density of radiation defects followed the same trends, and were very comparable in magnitude.
The effect of Nb additions on the thermal stability of melt-spun Nd2Fe14B
NASA Astrophysics Data System (ADS)
Lewis, L. H.; Gallagher, K.; Panchanathan, V.
1999-04-01
Elevated-temperature superconducting quantum interference device (SQUID) magnetometry was performed on two samples of melt-spun and optimally annealed Nd2Fe14B; one sample contained 2.3 wt % Nb and one was Nb-free. Continuous full hysteresis loops were measured with a SQUID magnetometer at T=630 K, above the Curie temperature of the 2-14-1 phase, as a function of field (1 T⩽H⩽-1 T) and time on powdered samples sealed in quartz tubes at a vacuum of 10-6 Torr. The measured hysteresis signals were deconstructed into a high-field linear paramagnetic portion and a low-field ferromagnetic signal of unclear origin. While the saturation magnetization of the ferromagnetic signal from both samples grows with time, the signal from the Nb-containing sample is always smaller. The coercivity data are consistent with a constant impurity particle size in the Nb-containing sample and an increasing impurity particle size in the Nb-free sample. The paramagnetic susceptibility signal from the Nd2Fe14B-type phase in the Nb-free sample increases with time, while that from the Nb-containing sample remains constant. It is suggested that the presence of Nb actively suppresses the thermally induced formation of poorly crystallized Fe-rich regions that apparently exist in samples of both compositions.
Low-velocity impacts into cryogenic icy regolith
NASA Astrophysics Data System (ADS)
Brisset, Julie; Colwell, Josh E.; Dove, Adrienne; Rascon, Allison; Mohammed, Nadia; Cox, Christopher
2016-10-01
The first stages of planet formation take place in the protoplanetary disk (PPD), where µm-sized dust grains accrete into km-sized planetesimals. In the current discussion on the processes involved in accretion beyond the cm scale, the size distribution of the particles colliding at low speeds (a few m/s) inside the PPD is thought to play an important role. A few larger bodies that survived bouncing and fragmentation collisions accumulate the fine dust residue of the erosion and fragmentation of other particles that were destroyed in more energetic collisions. A significant component of this dust on bodies farther out in the PPD will be composed of ices.We have carried out a series of experiments to study the ejecta mass-velocity distribution from impacts of cm-scale particles into granular media at speeds below 3 m/s in both microgravity and 1-g conditions in vacuo and room temperature. Aggregate-aggregate collision experiments have shown bouncing and fragmentation at speeds above ~ 1 m/s. However, most planetesimal formation occurred beyond the frost line and at much lower temperatures than our earlier experiments. We have performed impact experiments at 1-g into JSC-1 lunar regolith simulant at low temperatures (<150 K) with water ice particles mixed into the JSC-1 sample. We varied the impact energy and the water ice content of the sample and measured the ejecta mass-velocity distribution as well as the final crater size. Our goal is to determine if the cryogenic temperature and the presence of water ice in the regolith affects the dynamic response to low-velocity impacts and the production of regolith. We will present the results of the cryogenic impacts and compare them to the study performed at room temperature without water ice. The inclusion of water ice into the target sample is a first step towards better understanding the influence of the presence of water ice in the production of ejecta in response to low-velocity impacts. We will discuss the implications of our results for planetary ring particle collisions as well as planetesimal formation.
Magnetic studies of CuFe{sub 2}O{sub 4} nanoparticles prepared by co-precipitation method
DOE Office of Scientific and Technical Information (OSTI.GOV)
Subha, A.; Shalini, M. Govindaraj; Sahoo, Subasa C., E-mail: subasa@cukerala.ac.in
2016-05-06
Cu-ferrite nanoparticles were synthesized by co-precipitation method and were annealed at different temperatures ranging from 400 to l000°C in air for 4 hours. The as-prepared sample and the sample annealed at 400°C showed small peaks of cubic Cu-ferrite in X-ray diffraction studies. For the intermediate temperature 600°C, some additional peaks of α-Fe{sub 2}O{sub 3} were observed. As the annealing temperature increased further only tetragonal Cu-ferrite peaks were observed. In all the samples some traces of CuO was noted. Grain size was increased from 2lnm for the as prepared sample to 42nm for the sample annealed at l000°C. Spontaneous magnetization valuemore » was found to be very small for the as prepared sample and it was increased monotonically with the increase in annealing temperature. Maximum magnetization of 29.7emu/g was observed at 300K for the sample annealed at l000°C. The remanent magnetization was increased with the increase in annealing temperature up to 900°C and then decreased whereas for the coercivity a peak was observed for the sample annealed at 800°C. The highest coercivity of l402 Oe was observed at 300K for the sample annealed at 800°C. As the measurement temperature decreased from 300K to 60K, magnetization and coercivity values were increased. The observed magnetic behaviour may be understood on the basis of phase transformation, grain growth with the increase in annealing temperature and reduced thermal energy at low measurement temperature.« less
Impedance analysis and dielectric response of anatase TiO2 nanoparticles codoped with Mn and Co ions
NASA Astrophysics Data System (ADS)
Kumar, Anand; Kashyap, Manish K.; Sabharwal, Namita; Kumar, Sarvesh; Kumar, Ashok; Kumar, Parmod; Asokan, K.
2017-11-01
In order to elucidate the effect of transition metal (TM) doping, the impedance and dielectric responses of Co and/or Mn-doped TiO2 nanocrystalline powder samples with 3% doping concentration synthesized via sol gel technique, have been analyzed. X-ray diffraction (XRD) analysis confirms the formation of tetragonal TiO2 anatase phase for all studied samples without any extra impurity phase peaks. The variation in the grain size measured from field emission scanning electron microscope (FESEM) measurements for all the samples are in accordance with the change in crystallite size as obtained from XRD. The DC resistivity for pure TiO2 nanoparticles is the highest while codoped samples exhibit low resistivity. The temperature dependent dielectric constant and dielectric loss possess step like enhancement and show the relaxation behavior. At room temperature, the dielectric function and dielectric loss decrease rapidly with increase in frequency and become almost constant at the higher frequencies. Such a decrease in dielectric loss is suitable for energy storage devices.
Searles, J A; Carpenter, J F; Randolph, T W
2001-07-01
In a companion paper we show that the freezing of samples in vials by shelf-ramp freezing results in significant primary drying rate heterogeneity because of a dependence of the ice crystal size on the nucleation temperature during freezing.1 The purpose of this study was to test the hypothesis that post-freezing annealing, in which the product is held at a predetermined temperature for a specified duration, can reduce freezing-induced heterogeneity in sublimation rates. In addition, we test the impact of annealing on primary drying rates. Finally, we use the kinetics of relaxations during annealing to provide a simple measurement of T(g)', the glass transition temperature of the maximally freeze-concentrated amorphous phase, under conditions and time scales most appropriate for industrial lyophilization cycles. Aqueous solutions of hydroxyethyl starch (HES), sucrose, and HES:sucrose were either frozen by placement on a shelf while the temperature was reduced ("shelf-ramp frozen") or by immersion into liquid nitrogen. Samples were then annealed for various durations over a range of temperatures and partially lyophilized to determine the primary drying rate. The morphology of fully dried liquid nitrogen-frozen samples was examined using scanning electron microscopy. Annealing reduced primary drying rate heterogeneity for shelf-ramp frozen samples, and resulted in up to 3.5-fold increases in the primary drying rate. These effects were due to increased ice crystal sizes, simplified amorphous structures, and larger and more numerous holes on the cake surface of annealed samples. Annealed HES samples dissolved slightly faster than their unannealed counterparts. Annealing below T(g)' did not result in increased drying rates. We present a simple new annealing-lyophilization method of T(g)' determination that exploits this phenomenon. It can be carried out with a balance and a freeze-dryer, and has the additional advantage that a large number of candidate formulations can be evaluated simultaneously.
NASA Astrophysics Data System (ADS)
Stein, C. R.; Bezerra, M. T. S.; Holanda, G. H. A.; André-Filho, J.; Morais, P. C.
2018-05-01
This study reports on the synthesis and characterization of cobalt ferrite (CoFe2O4) nanoparticles (NPs) synthesized by chemical co-precipitation in alkaline medium at increasing temperatures in the range of 27 °C to 100 °C. High-quality samples in the size range of 5 to 10 nm were produced using very low stirring speed (250 rpm) and moderate alkaline aqueous solution concentration (4.8 mol/L). Three samples were synthesized and characterized by x-ray diffraction (XRD) and room-temperature (RT) magnetization measurements. All samples present superparamagnetic (SPM) behavior at RT and Rietveld refinements confirm the inverse cubic spinel structure (space group Fd-3m (227)) with minor detectable impurity phase. As the synthesis temperature increases, structural parameters such as lattice constant and grain size change monotonically from 8.385 to 8.383 Å and from 5.8 to 7.4 nm, respectively. Likewise, as the synthesis temperature increases the NPs' magnetic moment and saturation magnetization increases monotonically from 2.6 ×103 to 16×103 μB and from 37 to 66 emu/g, respectively. The RT magnetization (M) versus applied field (H) curves were analyzed by the first-order Langevin function averaged out by a lognormal distribution function of magnetic moments. The excellent curve-fitting of the M versus H data is credited to a reduced particle-particle interaction due to both the SPM behavior and the existence of a surface amorphous shell layer (dead layer), the latter reducing systematically as the synthesis temperature increases.
NASA Astrophysics Data System (ADS)
Seo, Wonil; Kim, Kyoung-Ho; Kim, Young-Ho; Yoo, Sehoon
2018-01-01
The growth of interfacial intermetallic compound and the brittle fracture behavior of Sn-3.0Ag-0.5-Cu solder (SAC305) joints on electroless nickel immersion gold (ENIG) surface finish have been investigated using Ni-P plating solution at temperatures from 75°C to 85°C and fixed pH of 4.5. SAC305 solder balls with diameter of 450 μm were mounted on the prepared ENIG-finished Cu pads and reflowed with peak temperature of 250°C. The interfacial intermetallic compound (IMC) thickness after reflow decreased with increasing Ni-P plating temperature. After 800 h of thermal aging, the IMC thickness of the sample prepared at 85°C was higher than for that prepared at 75°C. Scanning electron microscopy of the Ni-P surface after removal of the Au layer revealed a nodular structure on the Ni-P surface. The nodule size of the Ni-P decreased with increasing Ni-P plating temperature. The Cu content near the IMC layer increased to 0.6 wt.%, higher than the original Cu content of 0.5 wt.%, indicating that Cu diffused from the Cu pad to the solder ball through the Ni-P layer at a rate depending on the nodule size. The sample prepared at 75°C with thicker interfacial IMC showed greater high-speed shear strength than the sample prepared at 85°C. Brittle fracture increased with decreasing Ni-P plating temperature.
Self-navigation of a scanning tunneling microscope tip toward a micron-sized graphene sample.
Li, Guohong; Luican, Adina; Andrei, Eva Y
2011-07-01
We demonstrate a simple capacitance-based method to quickly and efficiently locate micron-sized conductive samples, such as graphene flakes, on insulating substrates in a scanning tunneling microscope (STM). By using edge recognition, the method is designed to locate and to identify small features when the STM tip is far above the surface, allowing for crash-free search and navigation. The method can be implemented in any STM environment, even at low temperatures and in strong magnetic field, with minimal or no hardware modifications.
NASA Astrophysics Data System (ADS)
Zhou, Tihe; Zhang, Peng; O'Malley, Ronald J.; Zurob, Hatem S.; Subramanian, Mani
2015-01-01
In order to achieve a fine uniform grain-size distribution using the process of thin slab casting and directing rolling (TSCDR), it is necessary to control the grain-size prior to the onset of thermomechanical processing. In the companion paper, Model Fe- Al Steel with Exceptional Resistance to High Temperature Coarsening. Part I: Coarsening Mechanism and Particle Pinning Effects, a new steel composition which uses a small volume fraction of austenite particles to pin the growth of delta-ferrite grains at high temperature was proposed and grain growth was studied in reheated samples. This paper will focus on the development of a simple laboratory-scale setup to simulate thin-slab casting of the newly developed steel and demonstrate the potential for grain size control under industrial conditions. Steel bars with different diameters are briefly dipped into the molten steel to create a shell of solidified material. These are then cooled down to room temperature at different cooling rates. During cooling, the austenite particles nucleate along the delta-ferrite grain boundaries and greatly retard grain growth. With decreasing temperature, more austenite particles precipitate, and grain growth can be completely arrested in the holding furnace. Additional applications of the model alloy are discussed including grain-size control in the heat affected zone in welds and grain-growth resistance at high temperature.
NASA Astrophysics Data System (ADS)
Tsubokawa, Yumiko; Ishikawa, Masahiro
2017-09-01
Graphite-bearing polycrystalline olivine and polycrystalline clinopyroxene with submicron to micron grain size were successfully sintered from a single crystal of naturally occurring olivine (Fo88-92Fa12-8: Mg1.76-1.84Fe0.16-0.24SiO4) and a single crystal of naturally occurring clinopyroxene (Di99Hed1: Ca0.92Na0.07Mn0.01Mg0.93Fe0.01Al0.06Si2O6). The milled powders of both these crystals were sintered under argon gas flow at temperatures ranging from 1130 to 1350 °C for 2 h. As the sintering temperature increased, the average grain size of olivine increased from 0.2 to 1.4 µm and that of clinopyroxene increased from 0.1 to 2.4 µm. The porosity of sintered samples remained at an almost-constant volume of 2-5% for olivine and 3-4% for clinopyroxene. The samples sintered from powders milled with ethanol exhibited trace amount of graphite, identified via Raman spectroscopy analysis. As the sintering temperature increased, the intensity of the graphite Raman peak decreased, compared with both olivine and clinopyroxene peaks. The carbon content of the sintered samples was estimated to be a few hundred ppm. The in-plane size ( L a ) of graphite in the sintered olivine was estimated to be <15 nm. Our experiments demonstrate new possibilities for preparing graphite-bearing silicate-mantle mineral rocks, and this method might be useful in understanding the influence of the physical properties of graphite on grain-size-sensitive rheology or the seismic velocity of the Earth's mantle.[Figure not available: see fulltext.
NASA Astrophysics Data System (ADS)
Wang, L.; Li, J.; Liu, M.; Zhang, Y. M.; Lu, J. B.; Li, H. B.
2012-12-01
CoAl0.2Fe1.8O4/SiO2 nanocomposites were prepared by sol-gel method. The effects of annealing temperature on the structure and magnetic properties of the samples were studied by X-ray diffraction, transmission electron microscopy, vibrating sample magnetometer and Mössbauer spectroscopy. The results show that the CoAl0.2Fe1.8O4 in the samples exhibits a spinel structure after being annealed. As annealing temperature increases from 800 to 1200 °C, the average grain size of CoAl0.2Fe1.8O4 in the nanocomposites increases from 5 to 41 nm while the lattice constant decreases from 0.8397 to 0.8391 nm, the saturation magnetization increases from 21.96 to 41.53 emu/g. Coercivity reaches a maximum of 1082 Oe for the sample annealed at 1100 °C, and thereafter decreases with further increasing annealing temperature. Mössbauer spectra show that the isomer shift decreases, hyperfine field increases and the samples transfer from mixed state of superparamagnetic and magnetic order to the completely magnetic order with annealing temperature increasing from 800 to 1200 °C.
NASA Astrophysics Data System (ADS)
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.
NASA Astrophysics Data System (ADS)
Siregar, N.; Indrayana, I. P. T.; Suharyadi, E.; Kato, T.; Iwata, S.
2017-05-01
Mn0.5Zn0.5Fe2O4 nanoparticles have been successfully synthesized through coprecipitation method by varying NaOH concentrations from 0.5 M to 6 M and synthesis temperatures from 30 to 120 °C. The X-ray diffraction (XRD) pattern indicates samples consisting of multiphase structures such as spinel of Mn0.5Zn0.5Fe2O4, α-MnO2, ZnO, λ-MnO2, and γ-Fe2O3. The crystallite size of Mn0.5Zn0.5Fe2O4 is in the range of 14.1 to 26.7 nm. The Transmission electron microscope (TEM) image shows that sample was agglomerate. The hysteresis loops confirm that nanoparticles are soft magnetic materials with low coercivity (H c) in the range of 45.9 to 68.5 Oe. Those values increased relatively with increasing particles size. For NaOH concentration variation, the maximum magnetization of the sample increased from 10.4 emu/g to 11.6 emu/g with increasing ferrite content. Meanwhile, the maximum magnetization increased from 7.9 to 15.7 emu/g for samples with various synthesis temperature. The highest coercivity of 68.5 Oe was attained for a sample of 6 M NaOH under 90 °C. The highest magnetization of 15.7 emu/g was achieved for a sample of 1.5 M NaOH under 120 °C caused by the maximum crystallinity of sample.
Ballistic and Diffusive Thermal Conductivity of Graphene
NASA Astrophysics Data System (ADS)
Saito, Riichiro; Masashi, Mizuno; Dresselhaus, Mildred S.
2018-02-01
This paper is a contribution to the Physical Review Applied collection in memory of Mildred S. Dresselhaus. Phonon-related thermal conductivity of graphene is calculated as a function of the temperature and sample size of graphene in which the crossover of ballistic and diffusive thermal conductivity occurs at around 100 K. The diffusive thermal conductivity of graphene is evaluated by calculating the phonon mean free path for each phonon mode in which the anharmonicity of a phonon and the phonon scattering by a 13C isotope are taken into account. We show that phonon-phonon scattering of out-of-plane acoustic phonon by the anharmonic potential is essential for the largest thermal conductivity. Using the calculated results, we can design the optimum sample size, which gives the largest thermal conductivity at a given temperature for applying thermal conducting devices.
Magnetic properties of undoped and Al doped layered α-Co(OH)2
NASA Astrophysics Data System (ADS)
Gupta, Anu; Tiwari, S. D.
2017-11-01
Undoped, 10% and 20% Al doped samples of layered hexagonal α-Co(OH)2 are synthesized. X-ray diffraction patterns show that the samples are nanocrystalline with average crystallite size 15 nm. Fourier transform infrared spectroscopy and thermogravimetric analysis are performed to establish molecular formula of samples. Analysis of susceptibility χ as a function of temperature T (5-300 K) data indicates for ferromagnetic transitions in the system at lower temperatures. Curie transition temperature TC for undoped, 10% and 20% Al doped α-Co(OH)2 are found to be 9, 7.5 and 6.0 K respectively. Fitting of χ vs. T data for T >TC to the high temperature series yields strength of intralayer and interlayer exchange interactions among Co2+ ions. For undoped sample values of these interactions are estimated to be 1.070 and 0.240 K respectively. Strength of these interactions decrease with increasing concentration of Al3+ ions in the lattice. Magnetization as a function of applied magnetic field (up to ± 50 kG) data confirm ferromagnetic nature of the samples at 5 K.
Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen
2017-03-07
Based on precursor powders with a size of 200-300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO₃ ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO₃ ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe 3+ to Fe 2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO₃ ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Samanta, Sujan Krishna, E-mail: itssujan@rediffmail.com; Chanda, Abhijit, E-mail: abhijitchanda.biomed@gmail.com
2016-04-13
Pure β-tricalcium phosphate (β-TCP), Zn-doped (3wt %) β-TCP and Mg- doped (3wt %) β-TCP samples were prepared by using a wet chemical precipitation synthesis technique, followed by calcination at 800 °C in air. The developed materials were subjected to sintering at different temperatures. Density and porosity were compared. The X-ray diffractometry (XRD) and Fourier-transformed infrared (FTIR) spectrometer were used to examine the changes in crystalline phases and presence of functional groups of TCP ceramics. The scanning electron microscopy (SEM) was used to study the pore formation, pore size, grain size.
Critical current and flux dynamics in Ag-doped FeSe superconductor
NASA Astrophysics Data System (ADS)
Galluzzi, A.; Polichetti, M.; Buchkov, K.; Nazarova, E.; Mancusi, D.; Pace, S.
2017-02-01
The measurements of DC magnetization as a function of the temperature M(T), magnetic field M(H), and time M(t) have been performed in order to compare the superconducting and pinning properties of an undoped FeSe0.94 sample and a silver doped FeSe0.94 + 6 wt% Ag sample. The M(T) curves indicate an improvement of the superconducting critical temperature and a reduction of the non-superconducting phase Fe7Se8 due to the silver doping. This is confirmed by the field and temperature dependent critical current density Jc(H,T) extracted from the superconducting hysteresis loops at different temperatures within the Bean critical state model. Moreover, the combined analysis of the Jc(T) and of the pinning force Fp(H/Hirr) indicate that the pinning mechanisms in both samples can be described in the framework of the collective pinning theory. The U*(T, J) curves show a pinning crossover from an elastic creep regime of intermediate size flux bundles, for low temperatures, to a plastic creep regime at higher temperatures for both the samples. Finally, the vortex hopping attempt time has been evaluated for both samples and the results are comparable with the values reported in the literature for high Tc materials.
NASA Astrophysics Data System (ADS)
Blanks, J. K.; Hintz, C. J.; Chandler, G. T.; Shaw, T. J.; McCorkle, D. C.; Bernhard, J. M.
2007-12-01
Mg/Ca and Sr/Ca were analyzed from core-top individual Hoeglundina elegans aragonitic tests collected from three continental slope depths within the South Carolina and Little Bahama Bank continental slope environs (220 m to 1084 m). Our study utilized only individuals that labeled with the vital probe CellTracker Green - unlike bulk core-top material often stained with Rose Bengal, which has known inconsistencies in distinguishing live from dead foraminifera. DSr x 10 values were consistently 1.74 $ pm 0.23 across all sampling depths. The analytical error in DSr values (0.7%) determined by ICP-MS between repeated measurements on individual H. elegans tests across all depths was less than analytical error on repeated measurements from standards. Variation in DSr values was not directly explained by a linear temperature relationship (p=0.0003, R2=0.44) over the temperature range of 4.9-11.4°C with a sensitivity of 59.8 μmol/mol/1°C. The standard error by regressing DSr across temperature yields + 3.4°C, which is nearly 3x greater that reported in previous studies. Sr/Ca was more sensitive for calibrating temperature than Mg/Ca in H. elegans. Observed scatter in DSr was too great across individuals of the same size and of different sizes to resolve ontogenetic effects. However, higher DSr values were associated with smaller individuals and warmer/shallower sampling depths. The highest DSr values were observed at the intermediate sampling depth (~600 m). No significant ontogenetic relationship was found across DSr values in different sized individuals due to tighter overall constrained variance; however lower DSr values were observed from several smaller individuals. Several dead tests of H. elegans showed no significant differences in DSr values compared to live specimens cleaned by standard cleaning methods, unlike higher dead than live DMg values observed for the same individuals. There were no significant deviations in DSr across batches cleaned on separate days, unlike the observed sensitivity of DMg across batches. A subset of samples were reductively cleaned (hydrazine solution); and exhibited DMg values within analytical precision of those observed for non-reductively cleaned samples. Therefore, deviations in DMg values resulting from the removal of the reductive cleaning step did not explain analytical errors greater than published values for Mg/Ca or the high variance across same sized individuals. Variation in DMg values across the same cleaning methods and from dead individuals suggests the need for a careful look into how foraminiferal aragonite should be processed. These findings provide evidence that both Mg and Sr in benthic foraminiferal aragonite reflect factors in addition to temperature and pressure that may interfere with absolute temperature calibrations. Funded by NSF OCE 0351029, OCE 0437366, and OCE-0350794.
Girgis, E; Portugal, R D; Loosvelt, H; Van Bael, M J; Gordon, I; Malfait, M; Temst, K; Van Haesendonck, C; Leunissen, L H A; Jonckheere, R
2003-10-31
Magnetization reversal was studied in square arrays of square Co/CoO dots with lateral size varying between 200 and 900 nm. While reference nonpatterned Co/CoO films show the typical shift and increased width of the hysteresis loop due to exchange bias, the patterned samples reveal a pronounced size dependence. In particular, an anomaly appears in the upper branch of the magnetization cycle and becomes stronger as the dot size decreases. This anomaly, which is absent at room temperature in the patterned samples, can be understood in terms of a competition between magnetostatic interdot interaction and exchange anisotropy during the magnetic switching process.
NASA Technical Reports Server (NTRS)
Glaser, F. M.
1976-01-01
Oligoclase and bloedite, two mined samples, have been investigated, and the diffuse reflectance spectra are presented. These data are for powdered material, 50 microns to 5 microns size mixture, cooled to 160 K. The reflectivity of the oligoclase sample was also measured at room temperature, about 290 K, and the results at these two temperatures do indicate some tentative differences. A frost of ordinary water was prepared and its spectral reflectance is presented. This result compares reasonably well with measurements made by other investigators.
NASA Astrophysics Data System (ADS)
Baqer, Anwar Ali; Matori, Khamirul Amin; Al-Hada, Naif Mohammed; Shaari, Abdul Halim; Kamari, Halimah Mohamed; Saion, Elias; Chyi, Josephine Liew Ying; Abdullah, Che Azurahanim Che
2018-06-01
A binary (CuO)0.6 (CeO2)0.4 nanoparticles were prepared via thermal treatment method, using copper nitrate, cerium nitrate as precursors, PVP as capping agent and de-ionized water as a solvent. The structures, morphology, composition of the element and optical properties of these nanoparticles have been studied under different temperatures using various techniques. The XRD spectrum of the samples at 500 °C and above confirmed the existence of both monoclinic (CuO) and cubic fluorite (CeO2) structures. The findings of FESEM and TEM exhibited the average practical size and agglomeration increment with an elevation in the calcination temperature. The synthesized nanoparticles were also characterized by FTIR, which indicated the formation of binary Cu-O and Ce-O bonds. The EDX analysis was performed to indicate the chemical composition of the sample. The double energy band gaps of (CuO)0.6(CeO2)0.4 reduction with rising calcination temperature, can be referred to the enhancement of the crystallinity of the samples. PL intensity of (CuO)0.6(CeO2)0.4 nanoparticles peaks, which increased with the elevation of the calcination temperature to 800 °C was observed from the PL spectrum; this was due to the increment of the particle size that occurred.
Synthesis and characterization of γ-Fe2O3 NPs on silicon substrate for power device application
NASA Astrophysics Data System (ADS)
Hussein Nurul Athirah, Abu; Bee Chin, Ang; Yew Hoong, Wong; Boon Hoong, Ong; Aainaa Aqilah, Baharuddin
2018-06-01
Maghemite nanoparticles (γ-Fe2O3 NPs) were synthesized using Massart procedure. The formation reaction were optimized by varying the concentration of ferric nitrate solution (Fe(NO3)3) (0.1, 0.3, 0.5, 0.7 and 1.0 M). All samples were characterized by means of x-ray Diffractometer (XRD), Raman Spectroscopy, Transmission Electron Microscope (TEM) and Alternating Gradient Magnetometer (AGM). The smallest size of the NPs were chosen to be deposited on Silicon (100) substrate by spin coating technique. Annealing process of the samples were performed in Argon ambient at different temperatures (600, 700, 800 and 900°) for 20 min. Metal-oxide-semiconductor capacitors were then fabricated by depositing Aluminium as the gate electrode. The effect of the annealing process on the structural and electrical properties of γ-Fe2O3 NPs thin film were investigated. The structural properties of the deposited thin film were evaluated by XRD analysis, Atomic Force Microscopy (AFM) and Raman Analysis. On the other hand, the electrical properties was conducted by current-voltage analysis. It was revealed that the difference in the annealing temperature affect the grain size, surface roughness, distribution of the nanoparticles as well as the electrical performance of the samples where low annealing temperature (600 °C) gives low leakage current while high annealing temperature (900 °C) gives high electrical breakdown.
NASA Technical Reports Server (NTRS)
Hou, Tan-Hung; Bai, Jia-Mo
1990-01-01
The crystallization behavior and the melt flow properties of two batches of 1500 series LaRC-TPI polymers from Mitsui Toatsu Chemicals (MTC) were investigated. The characterization methods include Differential Scanning Calorimetry, the x ray diffractography and the melt rheology. The as-received materials possess initial crystalline melting peak temperatures of 295 and 305 C, respectively. These materials are less readily recrystallizable at elevated temperatures when compared to other semicrystalline thermoplastics. For the samples annealed at temperatures below 330 C, a semicrystalline polymer can be obtained. On the other hand, a purely amorphous structure is realized in the samples annealed at temperatures above 330 C. Isothermal crystallization kinetics were studied by means of the simple Avrami equation. The viscoelastic properties at elevated temperatures below and above glass transition temperature of the polymers were measured. Information with regard to the molecule sizes and distributions in these polymers were also extracted from melt rheology.
Temperature profiles for laser-induced heating of nanocrystals embedded in glass matrices
NASA Astrophysics Data System (ADS)
Bhatnagar, Promod K.; Nagpal, Swati
2001-05-01
Quantum confined nanostructures are very important because of their application towards optoelectronic devices. Commercial colored glass filters, which have large semiconductor particles, are being used to manufacture nanocrystals by suitable heat treatments. The progress in this area has been hampered by high size dispersion of these dots in the glass matrix which leads to reduction in higher order susceptibility thereby reducing non-linearity. In the present paper attempt has been made to theoretically model the temperature profiles of a laser irradiated CdS doped Borosilicate sample. Laser being used has a beam diameter of 1.5 mm and energy for 10 nsec pulse is 10 mJ. Two different particle radii of 5 nm and 10 nm have been considered. It is found that larger particles reach higher temperatures for the same pulse characteristics. This is because smaller particles have larger surface to volume ratio and hence dissipates out heat faster to the surrounding. Hence bigger particles will reach dissolution temperature faster than smaller particle and particle beyond a certain size should dissolve in the glass matrix when a sample is heat treated by laser. This could lead to a reduction in size dispersion of the nanocrystals. Also photodarkening effect found in semiconductor doped glasses is a big handicap for practical application of these materials in fast optical switching and non-linear optical devices. Photodarkening effect has been established to be a photochemical effect and it is important to study the temperature profiles around a particle since it will effect the impurity migration.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Zhang, Xiangkai; Yang, Xuyue, E-mail: yangxuyue@csu.edu.cn; Institute for Materials Microstructure, Central South University, Changsha 410083
2015-08-15
The effects of rolling temperature and subsequent annealing on mechanical properties of Cu–Zn–Si alloy were investigated by using X-ray diffraction, transmission electron microscope, electron back scattered diffraction and tensile tests. The Cu–Zn–Si alloy has been processed at cryogenic temperature (approximately 77 K) and room temperature up to different rolling strains. It has been identified that the cryorolled Cu–Zn–Si alloy samples show a higher strength compared with those room temperature rolled samples. The improved strength of cryorolled samples is resulted from grain size effect and higher densities of dislocations and deformation twins. And subsequent annealing, as a post-heat treatment, enhanced themore » ductility. An obvious increase in uniform elongation appears when the volume fraction of static recrystallization grains exceeds 25%. The strength–ductility combination of the annealed cryorolled samples is superior to that of annealed room temperature rolled samples, owing to the finer grains, high fractions of high angle grain boundaries and twins. - Highlights: • An increase in hardness of Cu–Zn–Si alloy is noticed during annealing process. • Thermal stability is reduced in Cu–Zn–Si alloy by cryorolling. • An obvious enhancement in UE is noticed when fraction of SRX grains exceeds 25%. • A superior strength–ductility combination is achieved in the cryorolling samples.« less
Annealing effect on the structural and dielectric properties of hematite nanoparticles
NASA Astrophysics Data System (ADS)
Kumar, Vijay; Chahal, Surjeet; Singh, Dharamvir; Kumar, Ashok; Kumar, Parmod; Asokan, K.
2018-05-01
In the present work, we have synthesized hematite (α-Fe2O3) nanoparticles by sol-gel method and sintered them at different temperatures (200 °C, 400 °C and 800 °C for six hours). The samples were then characterized using versatile characterization techniques such as X-ray diffraction (XRD), dielectric measurement and temperature dependent resistivity (RT) for their structural, dielectric and electrical properties. XRD measurements infer that intensity of peak increases with an increase in temperature resulting an increase in crystallite size. Temperature dependent resistivity also shows decrease in the resistivity of the samples. Furthermore, the dielectric measurements correspond to the increase in the dielectric constant. Based on these observations, it can be inferred that sintering temperature plays an important role in tailoring the various physical properties of hematite nanoparticles.
Improved ASTM G72 Test Method for Ensuring Adequate Fuel-to-Oxidizer Ratios
NASA Technical Reports Server (NTRS)
Juarez, Alfredo; Harper, Susana A.
2016-01-01
The ASTM G72/G72M-15 Standard Test Method for Autogenous Ignition Temperature of Liquids and Solids in a High-Pressure Oxygen-Enriched Environment is currently used to evaluate materials for the ignition susceptibility driven by exposure to external heat in an enriched oxygen environment. Testing performed on highly volatile liquids such as cleaning solvents has proven problematic due to inconsistent test results (non-ignitions). Non-ignition results can be misinterpreted as favorable oxygen compatibility, although they are more likely associated with inadequate fuel-to-oxidizer ratios. Forced evaporation during purging and inadequate sample size were identified as two potential causes for inadequate available sample material during testing. In an effort to maintain adequate fuel-to-oxidizer ratios within the reaction vessel during test, several parameters were considered, including sample size, pretest sample chilling, pretest purging, and test pressure. Tests on a variety of solvents exhibiting a range of volatilities are presented in this paper. A proposed improvement to the standard test protocol as a result of this evaluation is also presented. Execution of the final proposed improved test protocol outlines an incremental step method of determining optimal conditions using increased sample sizes while considering test system safety limits. The proposed improved test method increases confidence in results obtained by utilizing the ASTM G72 autogenous ignition temperature test method and can aid in the oxygen compatibility assessment of highly volatile liquids and other conditions that may lead to false non-ignition results.
Role of SiO2 coating in multiferroic CoCr2O4 nanoparticles
NASA Astrophysics Data System (ADS)
Kamran, M.; Ullah, Asmat; Mehmood, Y.; Nadeem, K.; Krenn, H.
2017-02-01
Effect of silica (SiO2) coating concentration on structural and magnetic properties of multiferroic cobalt chromite (CoCr2O4) nanoparticles have been studied. The nanoparticles with average crystallite size in the range 19 to 28 nm were synthesised by sol-gel method. X-ray diffraction (XRD) analysis has verified the composition of single-phase cubic normal spinel structure of CoCr2O4 nanoparticles. The average crystallite size and cell parameter decreased with increasing SiO2 concentration. TEM image revealed that the shape of nanoparticles was non-spherical. Zero field cooled/field cooled (ZFC/FC) curves revealed that nanoparticles underwent a transition from paramagnetic (PM) state to collinear short-range ferrimagnetic (FiM) state, and this PM-FiM transition temperature decreased from 101 to 95 K with increasing SiO2 concentration or decreasing crystallite size. A conical spin state at Ts = 27 K was also observed for all the samples which decreased with decreasing average crystallite size. Low temperature lock-in transition was also observed in these nanoparticles at 12 K for uncoated nanoparticles which slightly shifted towards low temperature with decreasing average crystallite size. Saturation magnetization (Ms) showed decreasing trend with increasing SiO2 concentration, which was due to decrease in average crystallite size of nanoparticles and enhanced surface disorder in smaller nanoparticles. The temperature dependent AC-susceptibility also showed the decrease in the transition temperature (Tc), broadening of the Tc peak and decrease in magnetization with increasing SiO2 concentration or decreasing average crystallite size. In summary, the concentration of SiO2 has significantly affected the structural and magnetic properties of CoCr2O4 nanoparticles.
Variable temperature sensitivity of soil organic carbon in North American forests
Cinzia Fissore; Christian P. Giardina; Christopher W. Swanston; Gary M. King; Randall K. Kolka
2009-01-01
We investigated mean residence time (MRT) for soil organic carbon (SOC) sampled from paired hardwood and pine forests located along a 22 °C mean annual temperature (MAT) gradient in North America. We used acid hydrolysis fractionation, radiocarbon analyses, long-term laboratory incubations (525-d), and a three-pool model to describe the size and kinetics of...
Ferrihydrite, an antiferromagnetic iron oxyhydroxide, is of great importance for the cycling of many trace metals in the environment. Four ferrihydrite samples prepared with 1.3 to 3.5 wt% of Si at different synthesis temperatures (7.5 °C, 22 °C, 50 °C and 75 °C) were studied by ...
Why large cells dominate estuarine phytoplankton
Cloern, James E.
2018-01-01
Surveys across the world oceans have shown that phytoplankton biomass and production are dominated by small cells (picoplankton) where nutrient concentrations are low, but large cells (microplankton) dominate when nutrient-rich deep water is mixed to the surface. I analyzed phytoplankton size structure in samples collected over 25 yr in San Francisco Bay, a nutrient-rich estuary. Biomass was dominated by large cells because their biomass selectively grew during blooms. Large-cell dominance appears to be a characteristic of ecosystems at the land–sea interface, and these places may therefore function as analogs to oceanic upwelling systems. Simulations with a size-structured NPZ model showed that runs of positive net growth rate persisted long enough for biomass of large, but not small, cells to accumulate. Model experiments showed that small cells would dominate in the absence of grazing, at lower nutrient concentrations, and at elevated (+5°C) temperatures. Underlying these results are two fundamental scaling laws: (1) large cells are grazed more slowly than small cells, and (2) grazing rate increases with temperature faster than growth rate. The model experiments suggest testable hypotheses about phytoplankton size structure at the land–sea interface: (1) anthropogenic nutrient enrichment increases cell size; (2) this response varies with temperature and only occurs at mid-high latitudes; (3) large-cell blooms can only develop when temperature is below a critical value, around 15°C; (4) cell size diminishes along temperature gradients from high to low latitudes; and (5) large-cell blooms will diminish or disappear where planetary warming increases temperature beyond their critical threshold.
NASA Astrophysics Data System (ADS)
Venkatesh, Davuluri; Ramesh, K. V.; Sastry, C. V. S. S.
2017-07-01
Ni-Zn nanoferrite Ni0.5Zn0.5Fe2O4 is prepared by citrate gel auto combustion method and sintered at various temperatures 800, 900, 1000, 1100 and 1200°C. The room temperature x-ray diffraction conforms that the single phase spinel structure is formed. Crystallite size and density were increased with increasing of sintering temperature. From Raman spectroscopy all sintered samples are single phase with cubic spinel structure belong to Fd3m space group. From surface morphology studies it is clearly observed that the particle size increased with increasing of sintering temperature. Impedance spectroscopy revel that increasing of conductivity is due to grain resistance is decreased with increasing of sintering temperature. Cole-Cole plots are studied from impedance data. The electrical modulus analysis shows that non-Debye nature of Ni0.5Zn0.5Fe2O4 ferrite.
Wang, Meng; Wang, Ting; Song, Shenhua; Ravi, Muchakayala; Liu, Renchen; Ji, Shishan
2017-01-01
Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid-state reaction method, phase-pure YMnO3 ceramics are fabricated using spark plasma sintering (SPS). X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YMnO3 ceramics can be prepared by SPS at 1000 °C for 5 minutes with annealing at 800 °C for 2 h. The relative density of the sample is as high as 97%, which is much higher than those of the samples sintered by other methods. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods and SPS with ball-milling precursors, and the ferroelectric loops at room temperature can be detected. These findings indicate that the YMnO3 ceramics prepared by the low temperature solid reaction method and SPS possess excellent dielectric lossy ferroelectric properties at room temperature, and magnetic properties at low temperature (10 K), making them suitable for potential multiferroic applications. PMID:28772832
NASA Astrophysics Data System (ADS)
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.
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.
Strickland, N M; Hoffmann, C; Wimbush, S C
2014-11-01
A cryogenic electrical transport measurement system is described that is particularly designed to meet the requirements for routine and effective characterization of commercial second generation high-temperature superconducting (HTS) wires in the form of coated conductors based on YBa2Cu3O7. Specific design parameters include a base temperature of 20 K, an applied magnetic field capability of 8 T (provided by a HTS split-coil magnet), and a measurement current capacity approaching 1 kA. The system accommodates samples up to 12 mm in width (the widest conductor size presently commercially available) and 40 mm long, although this is not a limiting size. The sample is able to be rotated freely with respect to the magnetic field direction about an axis parallel to the current flow, producing field angle variations in the standard maximum Lorentz force configuration. The system is completely free of liquid cryogens for both sample cooling and magnet cool-down and operation. Software enables the system to conduct a full characterization of the temperature, magnetic field, and field angle dependence of the critical current of a sample without any user interaction. The system has successfully been used to measure a wide range of experimental and commercially-available superconducting wire samples sourced from different manufacturers across the full range of operating conditions. The system encapsulates significant advances in HTS magnet design and efficient cryogen-free cooling technologies together with the capability for routine and automated high-current electrical transport measurements at cryogenic temperatures. It will be of interest to both research scientists investigating superconductor behavior and commercial wire manufacturers seeking to accurately characterize the performance of their product under all desired operating conditions.
NASA Astrophysics Data System (ADS)
Fuad, A.; Fibriyanti, A. A.; Mufti, N.; Taufiq, A.; Maryam, S.; Hidayat, N.
2018-04-01
In this work, we report the preparation of CH3NH3PbI3 perovskite using one-step spin coating route for solar cell application. CH3NH3I• PbI2•DMF•DMSO complexes were coated on stainless steel as a subtrate layered by ZnO nanoparticles as an electron transport layer. To obtain samples with a special performance, we annealed the samples at a temperature of 100, 120, and 140°C for 10 minutes. The samples were then characterized by means of XRD, SEM/EDX, and Spectroscopic Ellipsometry. The analysis of XRD data presented that the CH3NH3PbI3 perovskites were successfully prepared and crystallized in tetragonal structure confirming from crystalline planes (110) and (220). Meanwhile, the particle size of the samples prepared at a temperature of 100, 120, and 140°C presented 42.96, 54.73, and 55.19 nm, respectively with coincide with the SEM images. The results indicated that the increase in temperature during synthesis influenced the particle growth. Furthermore, the characterization using Spectroscopic Ellipsometry exhibited that the CH3NH3PbI3 successfully layered on the substrate sizing nano metric scale that open high opportunity to be applied to solar cells with high performance.
Samuvel, K; Ramachandran, K
2015-07-05
This study examined the effects of the combination of starting materials on the properties of solid-state reacted BaTiO3 using two different types of BaCO3 and TiO2. In addition, the effect of mechanochemical activation by high energy milling and the Ba/Ti molar ratio on the reaction temperature, particle size and tetragonality were investigated. The TiO2 phase and size plays a major role in increasing the reaction temperature and particle size. With the optimum selection of starting materials and processing conditions, BaTiO3 with a particle size <200 nm (Scherrer's formula) and a tetragonality c/a of approximately 1.007 was obtained. Broadband dielectric spectroscopy is applied to investigate the electrical properties of disordered perovskite-like ceramics in a wide temperature range. From the X-ray diffraction analysis it was found that the newly obtained BaTi0.5Fe0.5O3 ceramics consist of two chemically different phases. The electric modulus M∗ formalism used in the analysis enabled us to distinguish and separate the relaxation processes, dominated by marked conductivity in the ε∗(ω) representation. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in solid state routed samples. Copyright © 2015 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
Samuvel, K.; Ramachandran, K.
2015-07-01
This study examined the effects of the combination of starting materials on the properties of solid-state reacted BaTiO3 using two different types of BaCO3 and TiO2. In addition, the effect of mechanochemical activation by high energy milling and the Ba/Ti molar ratio on the reaction temperature, particle size and tetragonality were investigated. The TiO2 phase and size plays a major role in increasing the reaction temperature and particle size. With the optimum selection of starting materials and processing conditions, BaTiO3 with a particle size <200 nm (Scherrer's formula) and a tetragonality c/a of approximately 1.007 was obtained. Broadband dielectric spectroscopy is applied to investigate the electrical properties of disordered perovskite-like ceramics in a wide temperature range. From the X-ray diffraction analysis it was found that the newly obtained BaTi0.5Fe0.5O3 ceramics consist of two chemically different phases. The electric modulus M∗ formalism used in the analysis enabled us to distinguish and separate the relaxation processes, dominated by marked conductivity in the ε∗(ω) representation. Interfacial effects on the dielectric properties of the samples have been understood by Cole-Cole plots in complex impedance and modulus formalism. Modulus formalism has identified the effects of both grain and grain boundary microstructure on the dielectric properties, particularly in solid state routed samples.
Synthesis of nanocomposites comprising iron and barium hexaferrites
NASA Astrophysics Data System (ADS)
Pal, M.; Bid, S.; Pradhan, S. K.; Nath, B. K.; Das, D.; Chakravorty, D.
2004-02-01
Composites of nanometre-sized α-iron and barium hexaferrite phases, respectively, have been synthesized by the ceramic processing route. Pure barium hexaferrite (BaO·6Fe 2O 3) was first of all prepared by calcinations of the precursor oxides at a maximum temperature of 1200°C for 4 h. By subjecting the resulting powder having particle size of the order of 1 μm to a reduction treatment in the temperature range 500-650°C for a period varying from 10 to 15 min it was possible to obtain a composite consisting of nanosized barium hexaferrite and α-Fe. At reduction temperature of 650°C for a period greater than 15 min all the ferrite phase was converted to α-Fe and Ba—the particle sizes being 59.4 and 43.6 nm, respectively. These conclusions are based on X-ray diffraction and Mossbauer studies of different samples. During reduction H + ions are introduced into the hexaferrite crystallite. It is believed that due to a tensile stress the crystals are broken up into smaller dimensions and the reduction brings about the growth of nanosized α-Fe and barium, respectively, around the hexaferrite particles. Magnetic measurements show coercivity values for the reduced samples in the range 120-440 Oe and saturation magnetization varying from 158 to 53.7 emu/g. These values have been ascribed to the formation and growth of α-Fe particles as the reduction treatment is increased. By heating the nanocomposites at a temperature of 1000°C for 1 h in ordinary atmosphere it was found that they were reconverted to the barium hexaferrite phase with a particle size ˜182.3 nm. The reaction described in this study is thus reversible.
Gu, Da Hwi; Jo, Seungki; Jeong, Hyewon; Ban, Hyeong Woo; Park, Sung Hoon; Heo, Seung Hwae; Kim, Fredrick; Jang, Jeong In; Lee, Ji Eun; Son, Jae Sung
2017-06-07
Electronically doped nanoparticles formed by incorporation of impurities have been of great interest because of their controllable electrical properties. However, the development of a strategy for n-type or p-type doping on sub-10 nm-sized nanoparticles under the quantum confinement regime is very challenging using conventional processes, owing to the difficulty in synthesis. Herein, we report the colloidal chemical synthesis of sub-10 nm-sized tellurium (Te)-doped Bismuth (Bi) nanoparticles with precisely controlled Te content from 0 to 5% and systematically investigate their low-temperature charge transport and thermoelectric properties. Microstructural characterization of nanoparticles demonstrates that Te ions are successfully incorporated into Bi nanoparticles rather than remaining on the nanoparticle surfaces. Low-temperature Hall measurement results of the hot-pressed Te-doped Bi-nanostructured materials, with grain sizes ranging from 30 to 60 nm, show that the charge transport properties are governed by the doping content and the related impurity and nanoscale grain boundary scatterings. Furthermore, the low-temperature thermoelectric properties reveal that the electrical conductivity and Seebeck coefficient expectedly change with the Te content, whereas the thermal conductivity is significantly reduced by Te doping because of phonon scattering at the sites arising from impurities and nanoscale grain boundaries. Accordingly, the 1% Te-doped Bi sample exhibits a higher figure-of-merit ZT by ∼10% than that of the undoped sample. The synthetic strategy demonstrated in this study offers the possibility of electronic doping of various quantum-confined nanoparticles for diverse applications.
NASA Astrophysics Data System (ADS)
Vila Verde, A.; Ramos, Marta M. D.
2005-07-01
We present an analytical model for a ceramic material (hydroxyapatite, HA) containing nanometre-scale water pores, and use it to estimate the pressure at the pore as a function of temperature at the end of a single 0.35 μs laser pulse by Er:YAG (2.94 μm) and CO 2 (10.6 μm) lasers. Our results suggest that the pressure at the pore is directly related to pore temperature, and that very high pressures can be generated simply by the thermal expansion of liquid water. Since the temperature reached in the pores at the end of the laser pulse is a strong function of pore size for Er:YAG lasers, but is independent of pore size for CO 2 lasers, our present results provide a possible explanation for the fact that human dental enamel threshold ablation fluences vary more for Er:YAG lasers than for CO 2 lasers. This suggests that experimentalists should analyse their results accounting for factors, like age or type of tooth, that may change the pore size distribution in their samples.
NASA Astrophysics Data System (ADS)
Petrović, S.; Rožić, Lj; Vuković, Z.; Grbić, B.; Radić, N.; Stojadinović, S.; Vasilić, R.
2017-04-01
This article presents the comparison of structural and fractal properties of nanocrystalline titanium dioxide (TiO2) and TiO2 modified with tungstophosphoric acid (TiO2/HPW) and their impact on the photocatalytic degradation of hazardous water pollutants. TiO2 and TiO2/HPW samples were synthesized by a combined sol-gel and hydrothermal processing. The XRD analysis of pure TiO2 samples revealed that phase composition was mainly dependent on the calcination temperature, changing from amorphous TiO2 to crystalline anatase and rutile by increasing the temperature. On the other hand, the XRD of TiO2/HPW samples calcined at temperatures above 600 °C showed crystalline peaks associated to formation of WO3 and WO2.92 crystalline domains. The N2 adsorption-desorption isotherm and pore size distribution of TiO2/HPW samples detected the existence of mesoporous characteristic with very narrow bimodal pores in the mesoporous region. The structural heterogeneity of samples was analyzed by means of pore size distribution functions, while the variation in fractal dimension were determined from the nitrogen adsorption isotherms, using the modified Frenkel-Halsey-Hill method. The results demonstrate that the approach is capable of characterizing complex textures such as those present in the TiO2 and TiO2/HPW photocatalysts. Besides, the effect of calcinations condition on photocatalytic properties of the samples was also investigated. The highest efficiency with respect to methyl orange photodecomposition was observed for TiO2/HPW photocatalysts calcined at 700 °C.
Transport properties of bismuth telluride compound prepared by mechanical alloying
NASA Astrophysics Data System (ADS)
Khade, Poonam; Bagwaiya, Toshi; Bhattacharya, Shovit; Rayaprol, Sudhindra; Sahu, Ashok K.; Shelke, Vilas
2017-05-01
We have synthesized bismuth telluride compound using mechanical alloying and hot press sintering method. The phase formation, crystal structure was evaluated by X-ray diffraction and Raman spectroscopy. The scanning electron microscopy images indicated sub-micron sized grains. We observed low value of thermal conductivity 0.39 W/mK at room temperature as a result of grain size reduction by increasing deformation. The performance of the samples can be improved by reducing the grain size, which increases the grain boundary scattering.
An Efficient, Robust, and Inexpensive Grinding Device for Herbal Samples like Cinchona Bark.
Hansen, Steen Honoré; Holmfred, Else; Cornett, Claus; Maldonado, Carla; Rønsted, Nina
2015-01-01
An effective, robust, and inexpensive grinding device for the grinding of herb samples like bark and roots was developed by rebuilding a commercially available coffee grinder. The grinder was constructed to be able to provide various particle sizes, to be easy to clean, and to have a minimum of dead volume. The recovery of the sample when grinding as little as 50 mg of crude Cinchona bark was about 60%. Grinding is performed in seconds with no rise in temperature, and the grinder is easily disassembled to be cleaned. The influence of the particle size of the obtained powders on the recovery of analytes in extracts of Cinchona bark was investigated using HPLC.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Saxena, Shailendra K., E-mail: phd1211512@iiti.ac.in; Sahu, Gayatri; Sagdeo, Pankaj R.
Quantum confinement effect has been studied in cheese like silicon nano-structures (Ch-SiNS) fabricated by metal induced chemical etching using different etching times. Scanning electron microscopy is used for the morphological study of these Ch-SiNS. A visible photoluminescence (PL) emission is observed from the samples under UV excitation at room temperature due to quantum confinement effect. The average size of Silicon Nanostructures (SiNS) present in the samples has been estimated by bond polarizability model using Raman Spectroscopy from the red-shift observed from SiNSs as compared to its bulk counterpart. The sizes of SiNS present in the samples decreases as etching timemore » increase from 45 to 75 mintunes.« less
Sedlacik, Michal; Pavlinek, Vladimir; Peer, Petra; Filip, Petr
2014-05-14
Magnetic nanoparticles of spinel nanocrystalline cobalt ferrite were synthesized via the sol-gel method and subsequent annealing. The influence of the annealing temperature on the structure, magnetic properties, and magnetorheological effect was investigated. The finite crystallite size of the particles, determined by X-ray diffraction and the particle size observed via transmission electron microscopy, increased with the annealing temperature. The magnetic properties observed via a vibrating sample magnetometer showed that an increase in the annealing temperature leads to the increase in the magnetization saturation and, in contrast, a decrease in the coercivity. The effect of annealing on the magnetic properties of ferrite particles has been explained by the recrystallization process at high temperatures. This resulted in grain size growth and a decrease in an imposed stress relating to defects in the crystal lattice structure of the nanoparticles. The magnetorheological characteristics of suspensions of ferrite particles in silicone oil were measured using a rotational rheometer equipped with a magnetic field generator in both steady shear and small-strain oscillatory regimes. The magnetorheological performance expressed as a relative increase in the magnetoviscosity appeared to be significantly higher for suspensions of particles annealed at 1000 °C.
Mn Impurity in Bulk GaAs Crystals
NASA Astrophysics Data System (ADS)
Pawłowski, M.; Piersa, M.; Wołoś, A.; Palczewska, M.; Strzelecka, G.; Hruban, A.; Gosk, J.; Kamińska, M.; Twardowski, A.
2006-11-01
Magnetic and electron transport properties of GaAs:Mn crystals grown by Czochralski method were studied. Electron spin resonance showed the presence of Mn acceptor A in two charge states: singly ionized A- in the form of Mn2+(d5), and neutral A0 in the form of Mn2+(d5) plus a bound hole (h). It was possible to determine the relative concentration of both types of centers from intensity of the corresponding electron spin resonance lines. Magnetization measured as a function of magnetic field (up to 6 T) in the temperature range of 2-300 K revealed overall paramagnetic behavior of the samples. Effective spin was found to be about 1.5 value, which was consistent with the presence of two types of Mn configurations. In most of the studied samples the dominance of Mn2+(d5)+h configuration was established and it increased after annealing of native donors. The total value of Mn content was obtained from fitting of magnetization curves with the use of parameters obtained from electron spin resonance. In electron transport, two mechanisms of conductivity were observed: valence band transport dominated above 70 K, and hopping conductivity within Mn impurity band at lower temperatures. From the analysis of the hopping conductivity and using the obtained values of the total Mn content, the effective radius of Mn acceptor in GaAs was estimated as a = 11 ± 3 Å.
NASA Astrophysics Data System (ADS)
Kumar, E. Ranjith; Kamzin, A. S.; Janani, K.
2016-11-01
Microstructure, morphological and gas sensor studies of Mn substituted cobalt ferrite nanoparticles synthesized by a simple evaporation method and auto- combustion method. The influence of heat treatment on phase and particle size of spinel ferrite nanoparticles were determined by X-ray diffraction and Mossbauer spectroscopy. The XRD study reveals that the lattice constant and crystallite size of the samples increases with the increase of annealing temperature. Last one was confirmed by Mossbauer data. The lowest size of particles of MnCoFe2O4 (~3 nm) is obtained by auto combustion method. The spherical shaped nanoparticles are recorded by TEM. Furthermore, conductance response of Mn-Co ferrite nanomaterial was measured by exposing the material to reducing gas like liquefied petroleum gas (LPG) which showed a sensor response of ~0.19 at an optimum operating temperature of 250 °C.
Self-assembled indium arsenide quantum dots: Structure, formation dynamics, optical properties
NASA Astrophysics Data System (ADS)
Lee, Hao
1998-12-01
In this dissertation, we investigate the properties of InAs/GaAs quantum dots grown by molecular beam epitaxy. The structure and formation dynamics of InAs quantum dots are studied by a variety of structural characterization techniques. Correlations among the growth conditions, the structural characteristics, and the observed optical properties are explored. The most fundamental structural characteristic of the InAs quantum dots is their shape. Through detailed study of the reflection high energy electron diffraction patterns, we determined that self-assembled InAs islands possess a pyramidal shape with 136 bounding facets. Cross-sectional transmission electron microscopy images and atomic force microscopy images strongly support this model. The 136 model we proposed is the first model that is consistent with all reported shape features determined using different methods. The dynamics of coherent island formation is also studied with the goal of establishing the factors most important in determining the size, density, and the shape of self- organized InAs quantum dots. Our studies clearly demonstrate the roles that indium diffusion and desorption play in InAs island formation. An unexpected finding (from atomic force microscopy images) was that the island size distribution bifurcated during post- growth annealing. Photoluminescence spectra of the samples subjected to in-situ annealing prior to the growth of a capping layer show a distinctive double-peak feature. The power-dependence and temperature-dependence of the photoluminescence spectra reveals that the double- peak emission is associated with the ground-state transition of islands in two different size branches. These results confirm the island size bifurcation observed from atomic force microscopy images. The island size bifurcation provides a new approach to the control and manipulation of the island size distribution. Unexpected dependence of the photoluminescence line-shape on sample temperature and pump intensity was observed for samples grown at relatively high substrate temperatures. The behavior is modeled and explained in terms of competition between two overlapping transitions. The study underscores that the growth conditions can have a dramatic impact on the optical properties of the quantum dots. This dissertation includes both my previously published and unpublished authored materials.
Nedielko, Maksym; Hamamda, Smail; Alekseev, Olexander; Chornii, Vitalii; Dashevskii, Mykola; Lazarenko, Maksym; Kovalov, Kostiantyn; Nedilko, Sergii G; Tkachov, Sergii; Revo, Sergiy; Scherbatskyi, Vasyl
2017-12-01
The set of composite materials that consist of micro/nanocellulose and complex K 2 Eu(MoO 4 )(PO 4 ) luminescent oxide particles was prepared. The composites were studied by means of scanning electron microscopy, XRD analysis, dilatometry, differential scanning calorimetry and thermogravimetric analysis, and dielectric and luminescence spectroscopy.Dependencies of density, crystallinity, relative extension, thermal extension coefficient, dielectric relaxation parameters, intensity and shape of photoluminescence bands on temperature, and content of oxide component were studied. The structure of the composite without oxide is formed by grains of nearly 5-50 μm in size (crystallinity is about ~56%). Structure of the micro/nanocellulose samples which contain oxide particles is similar, but the cellulose grains are deformed by oxide particles. Dependencies of the abovementioned properties on temperature and oxide content were analyzed together with data on the size distribution of oxide particles for the samples for various oxide and molecules of water concentrations.
Bubble evolution in Kr-irradiated UO2 during annealing
NASA Astrophysics Data System (ADS)
He, L.; Bai, X. M.; Pakarinen, J.; Jaques, B. J.; Gan, J.; Nelson, A. T.; El-Azab, A.; Allen, T. R.
2017-12-01
Transmission electron microscopy observation of Kr bubble evolution in polycrystalline UO2 annealed at high temperature was conducted in order to understand the inert gas behavior in oxide nuclear fuel. The average diameter of intragranular bubbles increased gradually from 0.8 nm in as-irradiated sample at room temperature to 2.6 nm at 1600 °C and the bubble size distribution changed from a uniform distribution to a bimodal distribution above 1300 °C. The size of intergranular bubbles increased more rapidly than intragranular ones and bubble denuded zones near grain boundaries formed in all the annealed samples. It was found that high-angle grain boundaries held bigger bubbles than low-angle grain boundaries. Complementary atomistic modeling was conducted to interpret the effects of grain boundary character on the Kr segregation. The area density of strong segregation sites in the high-angle grain boundaries is much higher than that in the low angle grain boundaries.
Moessbauer Characterization of Magnetite/Polyaniline Magnetic Nanocomposite
DOE Office of Scientific and Technical Information (OSTI.GOV)
Rodriguez, Anselmo F. R.; Faria, Fernando S. E. D. V.; Lopez, Jorge L.
2010-12-02
Aniline surface coated Fe{sub 3}O{sub 4} nanoparticles have been successfully synthesized by UV irradiation varying the time and the acid media (HCl, HNO{sub 3}, or H{sub 2}SO{sub 4}). The synthesized material represents a promising platform for application in nerve regeneration. XRD patterns are consistent with the crystalline structure of magnetite. Nevertheless, for UV irradiation times longer than 2 h, extra XRD lines reveal the presence of goethite. The mean crystallite size of uncoated particles is estimated to be 25.4 nm, meanwhile that size is reduced to 19.9 nm for the UV irradiated sample in HCl medium for 4 h. Moessbauermore » spectra of uncoated nanoparticles reveal the occurrence of thermal relaxation at room temperature, while the 77 K-Moessbauer spectrum suggests the occurrence of electron localization effects similar to that expected in bulk magnetite. The Mossbauer spectra of UV irradiated sample in HCl medium during 4 h, confirms the presence of the goethite phase. For this sample, the thermal relaxation is more evident, since the room temperature spectrum shows larger spectral area for the nonmagnetic component due to the smaller crystallite size. Meanwhile, the 77 K-Moessbauer spectrum suggests the absence of the electron localization effect above 77 K.« less
Co-Precipitation Synthesis and Characterization of SrBi2Ta2O9 Ceramic
NASA Astrophysics Data System (ADS)
Afqir, Mohamed; Tachafine, Amina; Fasquelle, Didier; Elaatmani, Mohamed; Carru, Jean-Claude; Zegzouti, Abdelouahad; Daoud, Mohamed
2018-04-01
Strontium bismuth tantalate (SrBi2Ta2O9) was synthesized by a co-precipitation method. The sample was characterized by x-ray powder diffraction patterns (XRD), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The results of the dielectric properties are reported at room temperature. No secondary phases were found while heating the powder at 850°C and the pure SrBi2Ta2O9 phase was formed, as revealed by XRD. The characteristic bands for SrBi2Ta2O9 were observed by FTIR at approximately 619 cm-1 and 810 cm-1. SEM micrographs for the sample displayed thin plate-like grains. The grain size was less than 1 μm and the crystallite size of about 24 nm. Dielectric response at room temperature shows that the SrBi2Ta2O9 ceramic has low loss values, and the flattening of the dielectric constant at higher frequencies. The observed Curie temperature is comparable with those reported in the literature.
Synthesis and electrical properties of (LiCo 3/5Fe 1/5Mn 1/5)VO 4 ceramics
NASA Astrophysics Data System (ADS)
Ram, Moti
2010-03-01
(LiCo 3/5Fe 1/5Mn 1/5)VO 4 ceramic was synthesized via solution-based chemical method. X-ray diffraction analysis was carried out on the synthesized powder sample at room temperature, which confirms the orthorhombic structure with the lattice parameters of a = 10.3646 (20) Å, b = 3.7926 (20) Å, c = 9.2131 (20) Å. Field emission scanning electron microscopic analysis was carried out on the sintered pellet sample that indicates grains of unequal sizes (˜0.1 to 2 μm) presents average grains size with polydisperse distribution on the surface of the ceramic. Complex impedance spectroscopy (CIS) technique is used for the study of electrical properties. CIS analysis identifies: (i) grain interior, grain boundary and electrode-material interface contributions to electrical response (ii) the presence of temperature dependent electrical relaxation phenomena in the ceramics. Detailed conductivity study indicates that electrical conduction in the material is a thermally activated process. The variation of A.C. conductivity with frequency at different temperatures obeys Jonscher's universal law.
NASA Technical Reports Server (NTRS)
Ruschmeyer, O. R.; Pflug, I. J.; Gove, R.; Heisserer, Y.
1975-01-01
Research efforts were concentrated on attempts to obtain data concerning the dry heat resistance of particle microflora in Kennedy Space Center soil samples. The in situ dry heat resistance profiles at selected temperatures for the aggregate microflora on soil particles of certain size ranges were determined. Viability profiles of older soil samples were compared with more recently stored soil samples. The effect of increased particle numbers on viability profiles after dry heat treatment was investigated. These soil particle viability data for various temperatures and times provide information on the soil microflora response to heat treatment and are useful in making selections for spacecraft sterilization cycles.
Assessment of Heat Hazard during the Polymerization of Selected Light-Sensitive Dental Materials.
Janeczek, Maciej; Herman, Katarzyna; Fita, Katarzyna; Dudek, Krzysztof; Kowalczyk-Zając, Małgorzata; Czajczyńska-Waszkiewicz, Agnieszka; Piesiak-Pańczyszyn, Dagmara; Kosior, Piotr; Dobrzyński, Maciej
2016-01-01
Introduction. Polymerization of light-cured dental materials used for restoration of hard tooth tissue may lead to an increase in temperature that may have negative consequence for pulp vitality. Aim. The aim of this study was to determine maximum temperatures reached during the polymerization of selected dental materials, as well as the time that is needed for samples of sizes similar to those used in clinical practice to reach these temperatures. Materials and Methods. The study involved four composite restorative materials, one lining material and a dentine bonding agent. The polymerization was conducted with the use of a diode light-curing unit. The measurements of the external surface temperature of the samples were carried out using the Thermovision®550 thermal camera. Results. The examined materials significantly differed in terms of the maximum temperatures values they reached, as well as the time required for reaching the temperatures. A statistically significant positive correlation of the maximum temperature and the sample weight was observed. Conclusions. In clinical practice, it is crucial to bear in mind the risk of thermal damage involved in the application of light-cured materials. It can be reduced by using thin increments of composite materials.
Temperature impact on the micro structure of tungsten exposed to He irradiation in LHD
NASA Astrophysics Data System (ADS)
Bernard, Elodie; Sakamoto, Ryuichi; Tokitani, Masayuki; Masuzaki, Suguru; Hayashi, Hiromi; Yamada, Hiroshi; Yoshida, Naoaki
2017-02-01
A new temperature controlled material probe was designed for the exposure of tungsten samples to helium plasma in the LHD. Samples were exposed to estimated fluences of ∼1023 m-2 and temperatures ranging from 65 to 600 °C. Transmission Electron Microscopy analysis allowed the study of the impact of He irradiation under high temperatures on tungsten micro structure for the first time in real-plasma exposure conditions. Both dislocation loops and bubbles appeared from low to medium temperatures and saw an impressive increase of size (factor 4 to 6) most probably by coalescence as the temperature reaches 600 °C, with 500 °C appearing as a threshold for bubble growth. Annealing of the samples up to 800 C highlighted the stability of the dislocation damages formed by helium irradiation at high surface temperature, as bubbles and dislocation loops seem to conserve their characteristics. Additional studies on cross-sections showed that bubbles were formed much deeper (70-100 nm) than the heavily damaged surface layer (10-20 nm), raising concern about the impact on the material mechanical properties conservation and potential additional trapping of hydrogen isotopes.
Elmendorf, Sarah C; Henry, Gregory H R; Hollister, Robert D; Fosaa, Anna Maria; Gould, William A; Hermanutz, Luise; Hofgaard, Annika; Jónsdóttir, Ingibjörg S; Jónsdóttir, Ingibjörg I; Jorgenson, Janet C; Lévesque, Esther; Magnusson, Borgþór; Molau, Ulf; Myers-Smith, Isla H; Oberbauer, Steven F; Rixen, Christian; Tweedie, Craig E; Walker, Marilyn D; Walker, Marilyn
2015-01-13
Inference about future climate change impacts typically relies on one of three approaches: manipulative experiments, historical comparisons (broadly defined to include monitoring the response to ambient climate fluctuations using repeat sampling of plots, dendroecology, and paleoecology techniques), and space-for-time substitutions derived from sampling along environmental gradients. Potential limitations of all three approaches are recognized. Here we address the congruence among these three main approaches by comparing the degree to which tundra plant community composition changes (i) in response to in situ experimental warming, (ii) with interannual variability in summer temperature within sites, and (iii) over spatial gradients in summer temperature. We analyzed changes in plant community composition from repeat sampling (85 plant communities in 28 regions) and experimental warming studies (28 experiments in 14 regions) throughout arctic and alpine North America and Europe. Increases in the relative abundance of species with a warmer thermal niche were observed in response to warmer summer temperatures using all three methods; however, effect sizes were greater over broad-scale spatial gradients relative to either temporal variability in summer temperature within a site or summer temperature increases induced by experimental warming. The effect sizes for change over time within a site and with experimental warming were nearly identical. These results support the view that inferences based on space-for-time substitution overestimate the magnitude of responses to contemporary climate warming, because spatial gradients reflect long-term processes. In contrast, in situ experimental warming and monitoring approaches yield consistent estimates of the magnitude of response of plant communities to climate warming.
NASA Technical Reports Server (NTRS)
Rerko, Rodney S.; deGroh, Henry C., III; Beckermann, Christoph
2000-01-01
Macrosegregation in metal casting can be caused by thermal and solutal melt convection, and the transport of unattached solid crystals resulting from nucleation in the bulk liquid or dendrite fragmentation. To develop a comprehensive numerical model for the casting of alloys, an experimental study has been conducted to generate benchmark data with which such a solidification model could be tested. The objectives were: (1) experimentally study the effects of solid transport and thermosolutal convection on macrosegregation and grain size; and (2) provide a complete set of boundary conditions temperature data, segregation data, and grain size data - to validate numerical models. Through the control of end cooling and side wall heating, radial temperature gradients in the sample and furnace were minimized. Thus the vertical crucible wall was adiabatic. Samples at room temperature were 24 cc and 95 mm long. The alloys used were Al-1 wt. pct. Cu, and Al- 10 wt. pct. Cu; the starting point for solidification was isothermal at 710 and 685 C respectively. To induce an equiaxed structure various amounts of the grain refiner TiB2 were added. Samples were either cooled from the top, or the bottom. Several trends in the data stand out. In attempting to model these experiments, concentrating on these trends or differences may be beneficial.
NASA Astrophysics Data System (ADS)
Singh Yadav, Raghvendra; Kuřitka, Ivo; Havlica, Jaromir; Hnatko, Miroslav; Alexander, Cigáň; Masilko, Jiri; Kalina, Lukas; Hajdúchová, Miroslava; Rusnak, Jaroslav; Enev, Vojtěch
2018-02-01
In this article, Co1-xZnxFe2O4 (x = 0.0 and 0.5) disc-shaped pellets were formed by hot-press sintering of nanoparticles at temperature 925 °C for 10 min in vacuum atmosphere under 30 MPa mechanical pressure. X-ray diffraction study confirmed the formation of spinel cubic ferrite structure of hot-press sintered spinel ferrite Co1-xZnxFe2O4 (x = 0.0 and 0.5) samples. The scanning electron microscopy image indicated that the growth and densification of smaller ferrite nanoparticles were higher than larger ferrite nanoparticles. Magnetic properties of sintered samples were investigated by the superconducting quantum interface device (SQUID) magnetometer at room temperature. The hot press sintered Co1-xZnxFe2O4 (x = 0.0 and 0.5) pellet samples exhibited magnetic properties dependent on the grain size of spinel ferrite particles. The maximum saturation magnetization 82.47 emu/g was obtained for Co0.5Zn0.5Fe2O4 hot press sintered sample of ball-milled ferrite particles. Further, the impact of grain size and density of sample on hardness, dielectric property and ac conductivity of hot-press sintered samples was investigated. In addition, the longitudinal wave velocity (Vl), transverse wave velocity (Vt), mean elastic wave velocity (Vm), bulk modulus (B), rigidity modulus (G), Young's modulus (E), Poisson ratio (σ) and Debye temperature (θD) were calculated. The elastic moduli of hot press sintered ferrite samples were corrected to zero porosity using Hosselman and Fulrath model.
Zebarjadi, Mona; Esfarjani, Keivan; Bian, Zhixi; Shakouri, Ali
2011-01-12
Coherent potential approximation is used to study the effect of adding doped spherical nanoparticles inside a host matrix on the thermoelectric properties. This takes into account electron multiple scatterings that are important in samples with relatively high volume fraction of nanoparticles (>1%). We show that with large fraction of uniform small size nanoparticles (∼1 nm), the power factor can be enhanced significantly. The improvement could be large (up to 450% for GaAs) especially at low temperatures when the mobility is limited by impurity or nanoparticle scattering. The advantage of doping via embedded nanoparticles compared to the conventional shallow impurities is quantified. At the optimum thermoelectric power factor, the electrical conductivity of the nanoparticle-doped material is larger than that of impurity-doped one at the studied temperature range (50-500 K) whereas the Seebeck coefficient of the nanoparticle doped material is enhanced only at low temperatures (∼50 K).
Temperature dependent localized surface plasmon resonance properties of supported gold nanoparticles
DOE Office of Scientific and Technical Information (OSTI.GOV)
Laha, Ranjit; Ranjan, Pranay
2016-05-23
The well known localized surface plasmon resonance (LSPR) of gold nanoparticles (AuNPs) supported on a dielectric substrate depends on the particle shape, size and type of dielectric material. The particle size and shape mainly vary with the method of preparation and the parameters involved there in. In this report, we show preparation of AuNPs supported on quartz substrate by direct current sputtering followed by thermal annealing at an optimized temperature of 400 °C. The samples were characterized using optical absorption spectra, scanning electron microscopy (SEM) and the energy dispersive x-ray spectrum. The LSPR position could be tuned by varying annealingmore » temperature. The LSPR was found to be blue shifted up to 10 nm with annealing temperature varying from 400 °C to 800 °C. The change in LSPR was ascribed to the morphology of AuNPs over quartz.« less
Temperature dependent localized surface plasmon resonance properties of supported gold nanoparticles
NASA Astrophysics Data System (ADS)
Laha, Ranjit; Ranjan, Pranay
2016-05-01
The well known localized surface plasmon resonance (LSPR) of gold nanoparticles (AuNPs) supported on a dielectric substrate depends on the particle shape, size and type of dielectric material. The particle size and shape mainly vary with the method of preparation and the parameters involved there in. In this report, we show preparation of AuNPs supported on quartz substrate by direct current sputtering followed by thermal annealing at an optimized temperature of 400 °C. The samples were characterized using optical absorption spectra, scanning electron microscopy (SEM) and the energy dispersive x-ray spectrum. The LSPR position could be tuned by varying annealing temperature. The LSPR was found to be blue shifted up to 10 nm with annealing temperature varying from 400 °C to 800 °C. The change in LSPR was ascribed to the morphology of AuNPs over quartz.
NASA Astrophysics Data System (ADS)
Raefat, Saad; Garoum, Mohammed; Laaroussi, Najma; Thiam, Macodou; Amarray, Khaoula
2017-07-01
In this work experimental investigation of apparent thermal diffusivity and adiabatic limit temperature of expanded granular perlite mixes has been made using the flash technic. Perlite granulates were sieved to produce essentially three characteristic grain sizes. The consolidated samples were manufactured by mixing controlled proportions of the plaster and water. The effect of the particle size on the diffusivity was examined. The inverse estimation of the diffusivity and the adiabatic limit temperature at the rear face as well as the heat losses coefficients were performed using several numerical global minimization procedures. The function to be minimized is the quadratic distance between the experimental temperature rise at the rear face and the analytical model derived from the one dimension heat conduction. It is shown that, for all granulometry tested, the estimated parameters lead to a good agreement between the mathematical model and experimental data.
The Influences of Soil Characteristics on Nest-Site Selection in Painted Turtles (Chrysemys picta)
NASA Astrophysics Data System (ADS)
Page, R.
2017-12-01
A variety of animals dig nests and lay their eggs in soil, leaving them to incubate and hatch without assistance from the parents. Nesting habitat is important for these organisms many of which exhibit temperature dependent sex determination (TSD) whereby the incubation temperature determines the sex of each hatchling. However, suitable nesting habitat may be limited due to anthropogenic activities and global temperature increases. Soil thermal properties are critical to these organisms and are positively correlated with water retention and soil carbon; carbon-rich soils result in higher incubation temperatures. We investigated nest-site selection in painted turtles (Chrysemys picta) inhabiting an anthropogenic pond in south central Pennsylvania. We surveyed for turtle nests and documented location, depth, width, temperature, canopy coverage, clutch size, and hatch success for a total of 31 turtle nests. To address the influence of soil carbon and particle size on nest selection, we analyzed samples collected from: 1) actual nests that were depredated, 2) false nests, incomplete nests aborted during digging prior to nest completion, and 3) randomized locations. Soil samples were separated into coarse, medium, and fine grain size fractions through a stack of sieves. Samples were combusted in a total carbon analyzer to measure weight percent organic carbon. We found that anthropogenic activity at this site has created homogenous, sandy, compacted soils at the uppermost layer that may limit females' access to appropriate nesting habitat. Turtle nesting activity was limited to a linear region north of the pond and was constrained by an impassable rail line. Relative to other studies, turtle nests were notably shallow (5.8±0.9 cm) and placed close to the pond. Compared to false nests and random locations, turtle-selected sites averaged greater coarse grains (35% compared to 20.24 and 20.57%) and less fine grains (47% compared to 59 and 59, respectively). Despite remarkably high soil carbon along the rail line (47.08%) turtles nested here with slightly higher hatch success. We suggest that the turtles are limited to sandy, compact soils with low heat capacities and may compensate for this by also nesting adjacent to the rail line where high soil carbon could increase incubation temperatures.
Surface spin tunneling and heat dissipation in magnetic nanoparticles
NASA Astrophysics Data System (ADS)
Palakkal, Jasnamol P.; Obula Reddy, Chinna; Paulose, Ajeesh P.; Sankar, Cheriyedath Raj
2018-03-01
Quantum superparamagnetic state is observed in ultra-fine magnetic particles, which is often experimentally identified by a significant hike in magnetization towards low temperatures much below the superparamagnetic blocking temperature. Here, we report experimentally observed surface spin relaxation at low temperatures in hydrated magnesium ferrite nanoparticles of size range of about 5 nm. We observed time dependent oscillatory magnetization of the sample below 2.5 K, which is attributed to surface spin tunneling. Interestingly, we observed heat dissipation during the process by using an external thermometer.
Intercalated Nanocomposites Based on High-Temperature Superconducting Ceramics and Their Properties
Tonoyan, Anahit; Schiсk, Christoph; Davtyan, Sevan
2009-01-01
High temperature superconducting (SC) nanocomposites based on SC ceramics and various polymeric binders were prepared. Regardless of the size of the ceramics’ grains, the increase of their amount leads to an increase of resistance to rupture and modulus and a decrease in limiting deformation, whereas an increase in the average ceramic grain size worsens resistance properties. The SC, thermo-chemical, mechanical and dynamic-mechanical properties of the samples were investigated. Superconducting properties of the polymer ceramic nanocomposites are explained by intercalation of macromolecule fragments into the interstitial layer of the ceramics’ grains. This phenomenon leads to a change in the morphological structure of the superconducting nanocomposites.
High-temperature material characterization for multispectral window
NASA Astrophysics Data System (ADS)
Park, James; Arida, Marvin-Ray; Ku, Zahyun; Jang, Woo-Yong; Urbas, Augustine M.
2017-05-01
A microwave cylindrical cavity combined with a laser has been investigated to characterize the temperature dependence of widow materials in the Air Force Research Laboratory (AFRL). This paper discusses the requirements of high temperature RF material characterizations for transparent ceramic materials, such as ALON, that can potentially be used for multispectral windows. The RF cylindrical resonator was designed and the numerical model was studied to characterize the dielectric constant of materials. The dielectric constant can be extracted from the resonant frequency shift based on the cavity perturbation method (CPM), which is sensitive to the sample size and shape. Laser heating was applied to the material under test (MUT), which could easily be heated above 1000°C by the laser irradiation, in order to conduct CPM at high temperature. The temperature distribution in a material was also analyzed to investigate the impact of the thermal properties and the sample shape.
Free volumes and gas transport in polymers: amine-modified epoxy resins as a case study.
Patil, Pushkar N; Roilo, David; Brusa, Roberto S; Miotello, Antonio; Aghion, Stefano; Ferragut, Rafael; Checchetto, Riccardo
2016-02-07
The CO2 transport process was studied in a series of amine-modified epoxy resins having different cross-linking densities but the same chemical environment for the penetrant molecules. Positron Annihilation Lifetime Spectroscopy (PALS) was used to monitor the free volume structure of the samples and experimentally evaluate their fractional free volume fh(T) and its temperature evolution. The analysis of the free volume hole size distribution showed that all the holes have a size large enough to accommodate the penetrant molecules at temperatures T above the glass transition temperature Tg. The measured gas diffusion constants at T > Tg have been reproduced in the framework of the free volume theory of diffusion using a novel procedure based on the use of fh(T) as an input experimental parameter.
Phase transformations in a Cu−Cr alloy induced by high pressure torsion
DOE Office of Scientific and Technical Information (OSTI.GOV)
Korneva, Anna, E-mail: a.korniewa@imim.pl; Straumal, Boris; Institut für Nanotechnologie, Karlsruher Institut für Technologie, Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen
2016-04-15
Phase transformations induced by high pressure torsion (HPT) at room temperature in two samples of the Cu-0.86 at.% Cr alloy, pre-annealed at 550 °C and 1000 °C, were studied in order to obtain two different initial states for the HPT procedure. Observation of microstructure of the samples before HPT revealed that the sample annealed at 550 °C contained two types of Cr precipitates in the Cu matrix: large particles (size about 500 nm) and small ones (size about 70 nm). The sample annealed at 1000 °C showed only a little fraction of Cr precipitates (size about 2 μm). The subsequentmore » HPT process resulted in the partial dissolution of Cr precipitates in the first sample and dissolution of Cr precipitates with simultaneous decomposition of the supersaturated solid solution in another. However, the resulting microstructure of the samples after HPT was very similar from the standpoint of grain size, phase composition, texture analysis and hardness measurements. - Highlights: • Cu−Cr alloy with two different initial states was deformed by HPT. • Phase transformations in the deformed materials were studied. • SEM, TEM and X-ray diffraction techniques were used for microstructure analysis. • HPT leads to formation the same microstructure independent of the initial state.« less
NASA Astrophysics Data System (ADS)
Arfaei, Babak
This work examines the nucleation mechanism of Sn in SnAgCu alloys and its effect on the microstructure of those solder joints. The nucleation rate of Sn in a SAC alloy was obtained by simultaneous calorimetric examination of the isothermal solidification of 88 flip chip Sn-Ag-Cu solder joints. Qualitative agreement with classic nucleation theory was observed, although it was concluded that the spherical cap model cannot be applied to explain the structure of nucleus. It was shown that the solidification temperature significantly affects the microstructure; samples that undercooled less than approximately 40oC revealed one or three large Sn grains, while interlaced twinning was observed in the samples that solidified at lower temperatures. In order to better understand the effect of microstructure on the thermomechanical properties of solder joints, a study of the dependence of room temperature shear fatigue lifetime on Sn grain number and orientation was conducted. This study examined the correlations of variations in fatigue life of solder balls with the microstructure of Sn-Ag-Cu solder. The mean fatigue lifetime was found to be significantly longer for samples with multiple Sn grains than for samples with single Sn grains. For single grain samples, correlations between Sn grain orientation (with respect to the loading direction) and lifetime were observed, providing insight on early failures in SnAgCu solder joints. Correlations between the lifetimes of single Sn grained, SAC205 solder joints with differences in Ag3Sn and Cu6Sn5 precipitate microstructures were investigated. It was found that Ag3Sn precipitates were highly segregated from Cu6Sn 5 precipitates on a length scale of approximately twenty microns. Furthermore, large (factor of two) variations of the Sn dendrite arm size were observed within given samples. Such variations in values of dendrite arm size within a single sample were much larger than observed variations of this parameter between individual samples. Few significant differences were observed in the average size of precipitates in different samples. While the earliest and latest lifetimes of single Sn grained samples were correlated with Sn grain orientation, effects of precipitate microstructure on lifetimes were not clearly delineated.
A size-dependent constitutive model of bulk metallic glasses in the supercooled liquid region
Yao, Di; Deng, Lei; Zhang, Mao; Wang, Xinyun; Tang, Na; Li, Jianjun
2015-01-01
Size effect is of great importance in micro forming processes. In this paper, micro cylinder compression was conducted to investigate the deformation behavior of bulk metallic glasses (BMGs) in supercooled liquid region with different deformation variables including sample size, temperature and strain rate. It was found that the elastic and plastic behaviors of BMGs have a strong dependence on the sample size. The free volume and defect concentration were introduced to explain the size effect. In order to demonstrate the influence of deformation variables on steady stress, elastic modulus and overshoot phenomenon, four size-dependent factors were proposed to construct a size-dependent constitutive model based on the Maxwell-pulse type model previously presented by the authors according to viscosity theory and free volume model. The proposed constitutive model was then adopted in finite element method simulations, and validated by comparing the micro cylinder compression and micro double cup extrusion experimental data with the numerical results. Furthermore, the model provides a new approach to understanding the size-dependent plastic deformation behavior of BMGs. PMID:25626690
A Low Resistance Infrared Bolometer for Use with a Squid Detection System.
1982-09-24
sensitivity. After treatment at 350C (near the Au-Ge eutectic temperature) the sensitivity and resistance decreased, as shown in Fig. 6. The as-evaporated... recrystallize with a very fine grain size, however, the thicker film (Sample No. 7A) revealed larger topographic bumps, Figure 21(b). The light etch sample (No...LOS ANGEI.ES. CA. 900fi ....... areas were of a similar thickness on both sets of samples. The thin film (Sample 3A) recrystallized in the contact
Differential scanning calorimetry of coal
NASA Technical Reports Server (NTRS)
Gold, P. I.
1978-01-01
Differential scanning calorimetry studies performed during the first year of this project demonstrated the occurrence of exothermic reactions associated with the production of volatile matter in or near the plastic region. The temperature and magnitude of the exothermic peak were observed to be strongly affected by the heating rate, sample mass and, to a lesser extent, by sample particle size. Thermal properties also were found to be influenced by oxidation of the coal sample due to weathering effects.
Injection molding of iPP samples in controlled conditions and resulting morphology
DOE Office of Scientific and Technical Information (OSTI.GOV)
Sessa, Nino, E-mail: ninosessa.ns@gmail.com; De Santis, Felice, E-mail: fedesantis@unisa.it; Pantani, Roberto, E-mail: rpantani@unisa.it
2015-12-17
Injection molded parts are driven down in size and weight especially for electronic applications. In this work, an investigation was carried out on the process of injection molding of thin iPP samples and on the morphology of these parts. Melt flow in the mold cavity was analyzed and described with a mathematical model. Influence of mold temperature and injection pressure was analyzed. Samples orientation was studied using optical microscopy.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Harish, B. M.; Rajeeva, M. P.; Naveen, C. S.
2016-05-06
Cerium oxide nanoparticles were synthesized by solution combustion method with varying the oxidizer (cerium nitrate hexa hydrate) to fuel (Glycine) molar ratio. The prepared samples were characterized by UV-visible spectrometer, X-ray diffractometer (XRD), Scanning electron microscope (SEM) and Energy dispersive X-Ray analysis (EDAX). XRD pattern reveals the formation of cubic fluorite structure of CeO{sub 2}. It was observed that finest crystallites were found at extreme fuel-deficient condition and it is good enough to produce favorable powder characteristics. The average crystallite size was found to be 14.46 nm to 21.57 nm. The temperature dependent dc conductivity was carried out using Keithleymore » source meter between the temperature range from 300 K to 573 K. From this study it was found that the conductivity increases with increase of temperature due to semiconducting behavior of CeO{sub 2} and it decreases with particle size due to increase in the energy band gap.« less
Annealing Effects on the Formation of Copper Oxide Thin Films
NASA Astrophysics Data System (ADS)
Marzuki, Marina; Zamzuri Mohamad Zain, Mohd; Zarul Hisham, Nurazhra; Zainon, Nooraizedfiza; Harun, Azmi; Nani Ahmad, Rozie
2018-03-01
This study approached the simple method of developing CuO thin films by thermal oxidation on pure Cu sheets. The effects of annealing temperature on the formation of CuO layers have been investigated. The oxide layers have been fabricated by annealing of Cu sheets for 5 hours at different temperatures of 980 ~ 1010 °C. The morphologies and optical properties of annealed Cu sheets were studied by using SEM and UV-Vis spectrophotometer respectively. It is revealed that the annealing temperature influence the grain growth and the grain size increases as the temperature increase. The highest grain size was observed on sample annealed at 1000 °C with average area per grain size of 0.023 mm2. Theoretically, larger grain size provides less barriers for electron mobility and increase the efficiency of solar devices. The optical absorption spectra of the oxide films was also measured. Interference pattern was noted at wavelength about 900 nm corresponding to the formation of CuO film. The interference noise observed could be due to the coarse surface and the presence of powdery oxide deposits that causes the scattering loses from the surface. CuO film obtained by this method may be further studied and exploited as low cost photovoltaic device.
Sirugudu, Roopas Kiran; Vemuri, Rama Krishna Murthy; Venkatachalam, Subramanian; Gopalakrishnan, Anisha; Budaraju, Srinivasa Murty
2011-01-01
Microwave sintering of materials significantly depends on dielectric, magnetic and conductive Losses. Samples with high dielectric and magnetic loss such as ferrites could be sintered easily. But low dielectric loss material such as dielectric resonators (paraelectrics) finds difficulty in generation of heat during microwave interaction. Microwave sintering of materials of these two classes helps in understanding the variation in dielectric and magnetic characteristics with respect to the change in grain size. High-energy ball milled Ni0.6Cu0.2Zn0.2Fe1.98O4-delta and ZnTiO3 are sintered in conventional and microwave methods and characterized for respective dielectric and magnetic characteristics. The grain size variation with higher copper content is also observed with conventional and microwave sintering. The grain size in microwave sintered Ni0.6Cu0.2Zn0.2Fe1.98O4-delta is found to be much small and uniform in comparison with conventional sintered sample. However, the grain size of microwave sintered sample is almost equal to that of conventional sintered sample of Ni0.3Cu0.5Zn0.2Fe1.98O4-delta. In contrast to these high dielectric and magnetic loss ferrites, the paraelectric materials are observed to sinter in presence of microwaves. Although microwave sintered zinc titanate sample showed finer and uniform grains with respect to conventional samples, the dielectric characteristics of microwave sintered sample are found to be less than that of conventional sample. Low dielectric constant is attributed to the low density. Smaller grain size is found to be responsible for low quality factor and the presence of small percentage of TiO2 is observed to achieve the temperature stable resonant frequency.
Leaching behaviour of bottom ash from RDF high-temperature gasification plants
DOE Office of Scientific and Technical Information (OSTI.GOV)
Gori, M., E-mail: manuela.gori@dicea.unifi.it; Pifferi, L.; Sirini, P.
2011-07-15
This study investigated the physical properties, the chemical composition and the leaching behaviour of two bottom ash (BA) samples from two different refuse derived fuel high-temperature gasification plants, as a function of particle size. The X-ray diffraction patterns showed that the materials contained large amounts of glass. This aspect was also confirmed by the results of availability and ANC leaching tests. Chemical composition indicated that Fe, Mn, Cu and Cr were the most abundant metals, with a slight enrichment in the finest fractions. Suitability of samples for inert waste landfilling and reuse was evaluated through the leaching test EN 12457-2.more » In one sample the concentration of all metals was below the limit set by law, while limits were exceeded for Cu, Cr and Ni in the other sample, where the finest fraction showed to give the main contribution to leaching of Cu and Ni. Preliminary results of physical and geotechnical characterisation indicated the suitability of vitrified BA for reuse in the field of civil engineering. The possible application of a size separation pre-treatment in order to improve the chemical characteristics of the materials was also discussed.« less
NASA Astrophysics Data System (ADS)
Reitze, Maximilian; Morlok, Andreas; Hiesinger, Harald; Weber, Iris; Stojic, Aleksandra
2017-04-01
Infrared spectroscopy is a powerful technique for the exploration of planetary surfaces with remote sensing observations [e.g., 1]. The MERTIS (Mercury Radiometer and Thermal Infrared Spectrometer) instrument onboard the BepiColombo spacecraft is designed to explore the surface mineralogy of Mercury in the wavelength region from 7 μ m to 14 μ m [2]. Mercury's surface reaches dayside temperatures of about 700 K [3]. It is well known that bondings between atoms change with temperature, resulting in infrared spectra changes with temperature [4]. In particular, rock-forming minerals like silicates show distinct absorption bands in the infrared due to molecular vibrations, for example, of Si-O bondings [4]. To accurately understand and correctly interpret returned MERTIS data, it is necessary to collect laboratory data of analogue materials under condition similar to Mercury [5]. It is known from previous investigations [5] that the Reststrahlenbands of olivine shift with temperature. In this work we report on temperature effects on Mercury analogue materials in ambient air. At the IRIS (Infrared & Raman for Interplanetary Spectroscopy) laboratory in Münster we used a Bruker VERTEX 70v IR spectrometer together with a Harrick heating stage in a Praying Mantis Diffuse Reflectance Accessory to measure mid-infrared reflectance of mineral powder samples with different grain sizes at increasing temperatures. We report on our spectral results for a natural olivine with Fo91 with a grain size range between 63 μ m and 125 μ m as well as a natural labradorite with a grain size range between 90 μ m and 125 μ m. Spectra were collected at 26, 75, 150, 200, 250, 300, and 350 degrees Celsius with a liquid nitrogen cooled MCT detector under normal ambient pressure. To ensure complete thermal equilibrium of our measured samples, we heated them to higher temperatures and subsequently cooled them to the temperatures at which the spectra were taken. For background calibration, we used a commercial diffuse reflectance gold standard (INFRAGOLD). Our results confirm the temperature-dependent shift of the strongest silicate feature in olivine spectra observed by [5]. For the shift of the peak position of this feature we calculated a shift function depending on the temperature in the form of Rmax[μ m]=0.00027μ m/K\\cdot x[K]+10.454μ m (R^2=0.92). Differences in the intensity of the spectra between [5] and our work are most likely due to smaller grain sizes of our samples. We are also planning on presenting results obtained from evacuated samples (down to 10-6 mbar), which are close to pressures existing on Mercury. References} [1] A. Maturilli, J. Helbert, A. Witzke, and L. Moroz, Planet. Space Sci., 54:1057-1064, 2006. [2] H. Hiesinger, J. Helbert, and MERTIS Co-I Team, Planet. Space Sci., 58:144-165, 2010. [3] M. A. Slade, B. J. Butler, and D. O. Muhleman, Science, 258:635-640, 1992. [4] C. M. Pieters and P. A. J. Englert, editors. Topics in Remote Sensing 4. Remote Geo-chemical Analysis: Elemental and Mineralogical Composition. Cambridge University Press, 1993. [5] J. Helbert, F. Nestola, S. Ferrari, A. Maturilli, M. Massironi, G. J. Redhammer, M. T. Capria, F. Capaccioni, and M. Bruno, EPSL, 371-372:252-257, 2013.
NASA Astrophysics Data System (ADS)
Drury, Anna Joy; John, Cédric M.
2016-10-01
Understanding past changes in sea surface temperatures (SSTs) is crucial; however, existing proxies for reconstructing past SSTs are hindered by unknown ancient seawater composition (foraminiferal Mg/Ca and δ18O) or reflect subsurface temperatures (TEX86) or have a limited applicable temperature range (U37k'). We examine clumped isotope (Δ47) thermometry to fossil coccolith-rich material as an SST proxy, as clumped isotopes are independent of original seawater composition and applicable to a wide temperature range and coccolithophores are widespread and dissolution resistant. The Δ47-derived temperatures from <63, <20, <10, and 2-5 μm size fractions of two equatorial Pacific late Miocene-early Pliocene sediment samples (c1; c2) range between ˜18 and 29°C, with c1 temperatures consistently above c2. Removing the >63 μm fraction removes most nonmixed layer components; however, the Δ47-derived temperatures display an unexpected slight decreasing trend with decreasing size fraction. This unexpected trend could partly arise because larger coccoliths (5-12 μm) are removed during the size fraction separation process. The c1 and <63 μm c2 Δ47-derived temperatures are comparable to concurrent U37k' SSTs. The <20, <10, and 2-5 μm c2 Δ47-derived temperatures are consistently cooler than expected. The Δ47-U37k' temperature offset is probably caused by abiotic/diagenetic calcite present in the c2 2-5 μm fraction (˜53% by area), which potentially precipitated at bottom water temperatures of ˜6°C. Our results indicate that clumped isotopes on coccolith-rich sediment fractions have potential as an SST proxy, particularly in tropical regions, providing that careful investigation of the appropriate size fraction for the region and time scale is undertaken.
Fluid inclusions in Martian samples: Clues to early crustal development and the hydrosphere
NASA Technical Reports Server (NTRS)
Brown, Philip E.
1988-01-01
Major questions about Mars that could be illuminated by examining fluid inclusions in Martian samples include: (1) the nature, extent and timing of development (and decline) of the hydrosphere that existed on the planet; and (2) the evolution of the crust. Fluid inclusion analyses of appropriate samples could provide critical data to use in comparison with data derived from analogous terrestrial studies. For this study, sample handling and return restrictions are unlikely to be as restrictive as the needs of other investigators. The main constraint is that the samples not be subjected to excessively high temperatures. An aqueous fluid inclusion trapped at elevated pressure and temperature will commonly consist of liquid water and water vapor at room temperature. Heating (such as is done in the laboratory to fix P-V-T data for the inclusion) results in moderate pressure increases up to the liquid-vapor homogenization temperature followed by a sharp increase in pressure with continued heating because the inclusion is effectively a fixed volume system. This increased pressure can rupture the inclusion; precise limits are dependent on size, shape, and composition as well as the host material.
Low-temperature positron annihilation study of B+-ion implanted PMMA
NASA Astrophysics Data System (ADS)
Kavetskyy, T. S.; Tsmots, V. M.; Voloshanska, S. Ya.; Šauša, O.; Nuzhdin, V. I.; Valeev, V. F.; Osin, Y. N.; Stepanov, A. L.
2014-08-01
Temperature dependent positron annihilation lifetime spectroscopy (PALS) measurements in the range of 50-300 K are carried out to study positronium formation in 40 KeV B+-ion implanted polymethylmethacrylate (B:PMMA) with two ion doses of 3.13 × 1015 and 3.75 × 1016 ions/cm2. The investigated samples show the various temperature trends of ortho-positronium (o-Ps) lifetime τ3 and intensity I3 in PMMA before and after ion implantation. Two transitions in the vicinity of ˜150 and ˜250 K, ascribed to γ and β transitions, respectively, are observed in the PMMA and B:PMMA samples in consistent with reference data for pristine sample. The obtained results are compared with room temperature PALS study of PMMA with different molecular weight (Mw) which known from literature. It is found that B+-ion implantation leads to decreasing Mw in PMMA at lower ion dose. At higher ion dose the local destruction of polymeric structure follows to broadening of lifetime distribution (hole size distribution).
NASA Astrophysics Data System (ADS)
Halder, Nilanjan; Misra, Kamakhya Prakash
2016-05-01
Using titanium isopropoxide as the precursor, Titanium dioxide (TiO2) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO2 samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increase with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO2 nano powder samples.
Isolating magnetic moments from individual grains within a magnetic assemblage
NASA Astrophysics Data System (ADS)
Béguin, A.; Fabian, K.; Jansen, C.; Lascu, I.; Harrison, R.; Barnhoorn, A.; de Groot, L. V.
2017-12-01
Methods to derive paleodirections or paleointensities from rocks currently rely on measurements of bulk samples (typically 10 cc). The process of recording and storing magnetizations as function of temperature, however, differs for grains of various sizes and chemical compositions. Most rocks, by their mere nature, consist of assemblages of grains varying in size, shape, and chemistry. Unraveling the behavior of individual grains is a holy grail in fundamental rock magnetism. Recently, we showed that it is possible to obtain plausible magnetic moments for individual grains in a synthetic sample by a micromagnetic tomography (MMT) technique. We use a least-squares inversion to obtain these magnetic moments based on the physical locations and dimensions of the grains obtained from a MicroCT scanner and a magnetic flux density map of the surface of the sample. The sample used for this proof of concept, however, was optimized for success: it had a low dispersion of the grains, and the grains were large enough so they were easily detected by the MicroCT scanner. Natural lavas are much more complex than the synthetic sample analyzed so far: the dispersion of the magnetic markers is one order of magnitude higher, the grains differ more in composition and size, and many small (submicron) magnetic markers may be present that go undetected by the MicroCT scanner. Here we present the first results derived from a natural volcanic sample from the 1907-flow at Hawaii. To analyze the magnetic flux at the surface of the sample at room temperature, we used the Magnetic Tunneling Junction (MTJ) technique. We were able to successfully obtain MicroCT and MTJ scans from the sample and isolate plausible magnetic moments for individual grains in the top 70 µm of the sample. We discuss the potential of the MMT technique applied to natural samples and compare the MTJ and SSM methods in terms of work flow and quality of the results.
NASA Astrophysics Data System (ADS)
Foka, Kewele E.; Dejene, Birhanu F.; Koao, Lehlohonolo F.; Swart, Hendrik C.
2018-04-01
A self-activated yellow emitting Zn2V2O7 was synthesized by combustion method. The influence of the processing parameters such as synthesis temperature and dopants concentration on the structure, morphology and luminescence properties was investigated. The X-ray diffraction (XRD) analysis confirmed that the samples have a tetragonal structure and no significant structural change was observed in varying both the synthesis temperature and the dopants concentration. The estimated average crystallite size was 78 nm for the undoped samples synthesized at different temperatures and 77 nm for the doped samples. Scanning electron microscope (SEM) images showed agglomerated hexagonal-shaped particles with straight edges at low temperatures and the shape of the particles changed to cylindrical structures at moderate temperatures. At higher temperatures, the morphology changed completely. However, the morphologies of the doped samples looked alike. The photoluminescence (PL) of the product exhibited broad emission bands ranging from 400 to 800 nm. The best luminescence intensity was observed for the undoped Zn2V2O7 samples and those synthesized at 600 ℃ . Any further increase in synthesis temperature, type and concentration of dopants led to a decrease in the luminescence intensity. The broad band emission peak of Zn2V2O7 consisted of two broad bands corresponding to emissions from the Em1 (3T2→1A1) and Em2 (3T1→1A1) transitions.
Quantifying Morphological Features of α-U3O8 with Image Analysis for Nuclear Forensics.
Olsen, Adam M; Richards, Bryony; Schwerdt, Ian; Heffernan, Sean; Lusk, Robert; Smith, Braxton; Jurrus, Elizabeth; Ruggiero, Christy; McDonald, Luther W
2017-03-07
Morphological changes in U 3 O 8 based on calcination temperature have been quantified enabling a morphological feature to serve as a signature of processing history in nuclear forensics. Five separate calcination temperatures were used to synthesize α-U 3 O 8 , and each sample was characterized using powder X-ray diffraction (p-XRD) and scanning electron microscopy (SEM). The p-XRD spectra were used to evaluate the purity of the synthesized U-oxide; the morphological analysis for materials (MAMA) software was utilized to quantitatively characterize the particle shape and size as indicated by the SEM images. Analysis comparing the particle attributes, such as particle area at each of the temperatures, was completed using the Kolmogorov-Smirnov two sample test (K-S test). These results illustrate a distinct statistical difference between each calcination temperature. To provide a framework for forensic analysis of an unknown sample, the sample distributions at each temperature were compared to randomly selected distributions (100, 250, 500, and 750 particles) from each synthesized temperature to determine if they were statistically different. It was found that 750 particles were required to differentiate between all of the synthesized temperatures with a confidence interval of 99.0%. Results from this study provide the first quantitative morphological study of U-oxides, and reveals the potential strength of morphological particle analysis in nuclear forensics by providing a framework for a more rapid characterization of interdicted uranium oxide samples.
Wang, Meng; Wang, Ting; Song, Shenhua; Ma, Qing; Liu, Renchen
2017-01-01
Based on precursor powders with a size of 200–300 nm prepared by the low-temperature solid reaction method, phase-pure YFeO3 ceramics are fabricated using spark plasma sintering (SPS) at different temperatures. X-ray diffraction (XRD) and scanning electron microscopy (SEM) reveal that the high-purity YFeO3 ceramics can be prepared using SPS, while the results from X-ray photoelectron spectroscopy (XPS) show that the concentration of oxygen vacancies resulting from transformation from Fe3+ to Fe2+ is low. The relative density of the 1000 °C-sintered sample is as high as 97.7%, which is much higher than those of the samples sintered at other temperatures. The present dielectric and magnetic properties are much better than those of the samples fabricated by conventional methods. These findings indicate that the YFeO3 ceramics prepared by the low temperature solid reaction and SPS methods possess excellent dielectric and magnetic properties, making them suitable for potential applications involving magnetic storage. PMID:28772626
Padalino, Lucia; Caliandro, Rocco; Chita, Giuseppe; Conte, Amalia; Del Nobile, Matteo Alessandro
2016-11-20
The influence of drying temperature on the starch crystallites and its impact on durum wheat pasta sensory properties is addressed in this work. In particular, spaghetti were produced by means of a pilot plant using 5 different drying temperature profiles. The sensory properties, as well as the cooking quality of pasta were assessed. X-ray powder diffraction was used for investigating changes in the crystallinity content of the samples. Starch crystallinity, size and density of the starch crystallites were determined from the analysis of the diffraction profiles. As expected, spaghetti sensory properties improved as the drying temperatures increased. In particular, attributes as resistance to break for uncooked samples and firmness, elasticity, bulkiness and stickiness for cooked samples, all benefit from drying temperature increase. The spaghetti cooking quality was also positively affected by the drying temperature increase. Diffraction analysis suggested that the improvement of sensory properties and cooking quality of pasta were directly related to the increase in density of both physical crosslink of starch granules and chemical crosslink of protein matrix. Copyright © 2016 Elsevier Ltd. All rights reserved.
Wei, Xiaomei; Yan, Linmiao; Zhao, Chengjian; Zhang, Yueyun; Xu, Yongli; Cai, Bo; Jiang, Ni; Huang, Yong
2018-05-01
Patterns of geographic variation in body size are predicted to evolve as adaptations to local environmental gradients. However, many of these clinal patterns in body size, such as Bergmann's rule, are controversial and require further investigation into ectotherms such as reptiles on a regional scale. To examine the environmental variables (temperature, precipitation, topography and primary productivity) that shaped patterns of geographic variation in body size in the reptile Calotes versicolor , we sampled 180 adult specimens (91 males and 89 females) at 40 locations across the species range in China. The MANOVA results suggest significant sexual size dimorphism in C. versicolor ( F 23,124 = 11.32, p < .001). Our results showed that C. versicolor failed to fit the Bergmann's rule. We found that the most important predictors of variation in body size of C. versicolor differed for males and females, but mechanisms related to heat balance and water availability hypotheses were involved in both sexes. Temperature seasonality, precipitation of the driest month, precipitation seasonality, and precipitation of the driest quarter were the most important predictors of variation in body size in males, whereas mean precipitation of the warmest quarter, mean temperature of the wettest quarter, precipitation seasonality, and precipitation of the wettest month were most important for body size variation in females. The discrepancy between patterns of association between the sexes suggested that different selection pressures may be acting in males and females.
NASA Astrophysics Data System (ADS)
Ngo, Chi-Vinh; Chun, Doo-Man
2017-07-01
Recently, the fabrication of superhydrophobic metallic surfaces by means of pulsed laser texturing has been developed. After laser texturing, samples are typically chemically coated or aged in ambient air for a relatively long time of several weeks to achieve superhydrophobicity. To accelerate the wettability transition from hydrophilicity to superhydrophobicity without the use of additional chemical treatment, a simple annealing post process has been developed. In the present work, grid patterns were first fabricated on stainless steel by a nanosecond pulsed laser, then an additional low-temperature annealing post process at 100 °C was applied. The effect of 100-500 μm step size of the textured grid upon the wettability transition time was also investigated. The proposed post process reduced the transition time from a couple of months to within several hours. All samples showed superhydrophobicity with contact angles greater than 160° and sliding angles smaller than 10° except samples with 500 μm step size, and could be applied in several potential applications such as self-cleaning and control of water adhesion.
NASA Astrophysics Data System (ADS)
Ueji, R.; Tsuchida, N.; Harada, K.; Takaki, K.; Fujii, H.
2015-08-01
The grain size effect on the deformation twinning in a high manganese austenitic steel which is so-called TWIP (twining induced plastic deformation) steel was studied in order to understand how to control deformation twinning. The 31wt%Mn-3%Al-3% Si steel was cold rolled and annealed at various temperatures to obtain fully recrystallized structures with different mean grain sizes. These annealed sheets were examined by room temperature tensile tests at a strain rate of 10-4/s. The coarse grained sample (grain size: 49.6μm) showed many deformation twins and the deformation twinning was preferentially found in the grains in which the tensile axis is parallel near to [111]. On the other hand, the sample with finer grains (1.8 μm) had few grains with twinning even after the tensile deformation. The electron back scattering diffraction (EB SD) measurements clarified the relationship between the anisotropy of deformation twinning and that of inhomogeneous plastic deformation. Based on the EBSD analysis, the mechanism of the suppression of deformation twinning by grain refinement was discussed with the concept of the slip pattern competition between the slip system governed by a grain boundary and that activated by the macroscopic load.
Investigations on neutron irradiated 3D carbon fibre reinforced carbon composite material
NASA Astrophysics Data System (ADS)
Venugopalan, Ramani; Alur, V. D.; Patra, A. K.; Acharya, R.; Srivastava, D.
2018-04-01
As against conventional graphite materials carbon-carbon (C/C) composite materials are now being contemplated as the promising candidate materials for the high temperature and fusion reactor owing to their high thermal conductivity and high thermal resistance, better mechanical/thermal properties and irradiation stability. The current need is for focused research on novel carbon materials for future new generation nuclear reactors. The advantage of carbon-carbon composite is that the microstructure and the properties can be tailor made. The present study encompasses the irradiation of 3D carbon composite prepared by reinforcement using PAN carbon fibers for nuclear application. The carbon fiber reinforced composite was subjected to neutron irradiation in the research reactor DHRUVA. The irradiated samples were characterized by Differential Scanning Calorimetry (DSC), small angle neutron scattering (SANS), XRD and Raman spectroscopy. The DSC scans were taken in argon atmosphere under a linear heating program. The scanning was carried out at temperature range from 30 °C to 700 °C at different heating rates in argon atmosphere along with reference as unirradiated carbon composite. The Wigner energy spectrum of irradiated composite showed two peaks corresponding to 200 °C and 600 °C. The stored energy data for the samples were in the range 110-170 J/g for temperature ranging from 30 °C to 700 °C. The Wigner energy spectrum of irradiated carbon composite did not indicate spontaneous temperature rise during thermal annealing. Small angle neutron scattering (SANS) experiments have been carried out to investigate neutron irradiation induced changes in porosity of the composite samples. SANS data were recorded in the scattering wave vector range of 0.17 nm-1 to 3.5 nm-1. Comparison of SANS profiles of irradiated and unirradiated samples indicates significant change in pore morphology. Pore size distributions of the samples follow power law size distribution with different exponent. Narrowing of SANS profile of the irradiated sample indicates creation of significant number of larger pores due to neutron irradiation.
The size effect to O2- -Ce4+ charge transfer emission and band gap structure of Sr2 CeO4.
Wang, Wenjun; Pan, Yu; Zhang, Wenying; Liu, Xiaoguang; Li, Ling
2018-04-24
Sr 2 CeO 4 phosphors with different crystalline sizes were synthesized by the sol-gel method or the solid-state reaction. Their crystalline size, luminescence intensity of O 2- -Ce 4+ charge transfer and energy gaps were obtained through the characterization by X-ray diffraction, photoluminescence spectra, as well as UV-visible diffuse reflectance measurements. An inverse relationship between photoluminescence (PL) spectra and crystalline size was observed when the heating temperature was from 1000°C to 1300°C. In addition, band energy calculated for all samples showed that a reaction temperature of 1200°C for the solid-state method and 1100°C for sol-gel method gave the largest values, which corresponded with the smallest crystalline size. Correlation between PL intensity and crystalline size showed an inverse relationship. Band structure, density of states and partial density of states of the crystal were calculated to analyze the mechanism using the cambrige sequential total energy package (CASTEP) module integrated with Materials Studio software. Copyright © 2018 John Wiley & Sons, Ltd.
Key to enhance thermoelectric performance by controlling crystal size of strontium titanate
NASA Astrophysics Data System (ADS)
Wang, Jun; Ye, Xinxin; Yaer, Xinba; Wu, Yin; Zhang, Boyu; Miao, Lei
2015-09-01
One-step molten salt synthesis process was introduced to fabricate nano to micrometer sized SrTiO3 powders in which effects of synthesis temperature, oxide-to-flux ratios and raw materials on the generation of SrTiO3 powders were examined. 100 nm or above sized pure SrTiO3 particles were obtained at relatively lower temperature of 900∘C. Micro-sized rhombohedral crystals with a maximum size of approximately 12 μm were obtained from SrCO3 or Sr(NO3)2 strontium source with 1:1 O/S ratio. Controlled crystal size and morphology of Nb-doped SrTiO3 particles are prepared by using this method to confirm the performance of thermoelectric properties. The Seebeck coefficient obtained is significantly high when compared with the reported data, and the high ratio of nano particles in the sample has a positive effect on the increase of Seebeck coefficient too, which is likely due to the energy filtering effect at large numbers of grain boundaries resulting from largely distributed structure.
Size-driven magnetic transitions in La1/3Ca2/3MnO3 nanoparticles
NASA Astrophysics Data System (ADS)
Markovich, V.; Fita, I.; Wisniewski, A.; Mogilyansky, D.; Puzniak, R.; Titelman, L.; Gorodetsky, G.
2010-09-01
Magnetic properties of electron-doped La1/3Ca2/3MnO3 manganite nanoparticles with average particle size ranging from 12 to 42 nm, prepared by the glycine-nitrate method, have been investigated in temperature range 5-300 K and in magnetic fields up to 90 kOe. Reduction in the particle size suppresses antiferromagnetism and decreases the Néel temperature. In contrast to bulk crystals, the charge ordering does not occur in all studied nanoparticles, while a weak ferromagnetism appears above 200 K. Low temperature magnetic hysteresis loops indicate upon exchange bias effect displayed by horizontal and vertical shifts in field cooled processes. The spontaneous and remanent magnetization at low temperature shows a relatively complex variation with particle size. The size-induced structural/magnetic disorder drives the La1/3Ca2/3MnO3 nanoparticles to a pronounced glassy behavior for the smallest 12 nm particles, as evidenced by large difference between zero field cooled and field cooled magnetization, frequency dependent ac-susceptibility, as well as characteristic slowing down in the spin dynamics. Time evolution of magnetization recorded in magnetic fields after field cooling to low temperatures exhibits pronounced relaxation and a very noisy behavior that may be caused by formation of some collective states. Magnetic properties of the nanoparticle samples are compared with those of La0.2Ca0.8MnO3 nanoparticles. These results shed some light on the coupling between charges and spin degrees of freedom in antiferromagnetic manganite nanoparticles.
NASA Astrophysics Data System (ADS)
Ata-Allah, S. S.; Balagurov, A. M.; Hashhash, A.; Bobrikov, I. A.; Hamdy, Sh.
2016-01-01
The parent NiFe2O4 and Zn/Ga substituted spinel ferrite powders have been prepared by solid state reaction technique. As a typical example, the Ni0.7Zn0.3Fe1.5Ga0.5O4 sample has been prepared by sol-gel auto combustion method with the nano-scale crystallites size. X-ray and Mössbauer studies were carried out for the prepared samples. Structure and microstructure properties were investigated using the time-of-flight HRFD instrument at the IBR-2 pulsed reactor, at a temperatures range 15-473 K. The Rietveld refinement of the neutron diffraction data revealed that all samples possess cubic symmetry corresponding to the space group Fd3m. Cations distribution show that Ni2+ is a complete inverse spinel ion, while Ga3+ equally distributed between the two A and B-sublattices. The level of microstrains in bulk samples was estimated as very small while the size of coherently scattered domains is quite large. For nano-structured sample the domain size is around 120 Å.
Electrical conductivity enhancement in heterogeneously doped scandia-stabilized zirconia
NASA Astrophysics Data System (ADS)
Varanasi, Chakrapani; Juneja, Chetan; Chen, Christina; Kumar, Binod
Composites of 6 mol% scandia-stabilized zirconia materials (6ScSZ) and nanosize Al 2O 3 powder (0-30 wt.%) were prepared and characterized for electrical conductivity by the ac impedance method at various temperatures ranging from 300 to 950 °C. All the composites characterized showed improved conductivity at higher temperatures compared to the undoped ScSZ. An average conductivity of 0.12 S cm -1 was measured at 850 °C for 6ScSZ + 30 wt.% Al 2O 3 composite samples, an increase in conductivity up to 20% compared to the undoped 6ScSZ specimen at this temperature. Microstructural evaluation using scanning electron microscopy revealed that the ScSZ grain size was relatively unchanged up to 10 wt.% of Al 2O 3 additions. However, the grain size was reduced in samples with higher (20 and 30 wt.%) additions of Al 2O 3. Small grain size, reduced quantity of the 6ScSZ material (only 70%), and improved conductivity makes these ScSZ + 30 wt.% Al 2O 3 composites very attractive as electrolyte materials in view of their collective mechanical and electrical properties and cost requirements. The observed increase in conductivity values with the additions of an insulating Al 2O 3 phase is explained in light of the space charge regions at the 6ScSZ-Al 2O 3 grain boundaries.
The Superheat Phenomenon in the Combustion of Magnesium Particles
NASA Technical Reports Server (NTRS)
Shafirovich, E. IA.; Goldshleger, U. I.
1992-01-01
Magnesium is known to be a likely fuel for engines that could work in the CO2 atmospheres of Mars and Venus. The present paper reports temperature measurements of magnesium samples during combustion in CO2. The burning sample temperature increases with the decrease in the initial size. The temperature of the 1-mm samples is 300-400 K higher than the boiling point of magnesium. The stability of the superheated drop is explained by the presence of a porous shell on the surface. An attempt has been made to describe vaporization on the superheated drop by the Knudsen-Langmuir equation. During combustion at high-pressure fragment ejection of the flame is observed in high-speed motion pictures. This phenomenon is shown to be connected with the drop superheat. The repeated fracture of the outer shell formed in the flame ensures the complete burnout of metal particles at high pressure.
Measurement of the thermal expansion of melt-textured YBCO using optical fibre grating sensors
NASA Astrophysics Data System (ADS)
Zeisberger, M.; Latka, I.; Ecke, W.; Habisreuther, T.; Litzkendorf, D.; Gawalek, W.
2005-02-01
In this paper we present measurements of the thermal expansion of melt-textured YBaCuO in the temperature range 30-300 K by means of optical fibre sensors. The sample, which had a size of 38 × 38 × 18 mm3, was prepared by our standard melt-texturing process using SmBaCuO seeds. One fibre containing three Bragg gratings which act as strain sensors was glued to the sample surface with two sensors parallel to the ab-plane and one sensor parallel to the c-axis. The sample was cooled down to a minimum temperature of 30 K in a vacuum chamber using a closed cycle refrigerator. In the temperature range we used, the thermal expansion coefficients are in the range of (3-9) × 10-6 K-1 (ab-direction) and (5-13) × 10-6 K-1 (c-direction).
The Effect of Sintering Temperature on Linear and Nonlinear Optical Properties of YAG Nanoceramics
NASA Astrophysics Data System (ADS)
Gayvoronsky, V. Ya.; Popov, A. S.; Brodyn, M. S.; Uklein, A. V.; Multian, V. V.; Shul'zhenko, O. O.
Recent improvements in powder synthesis and ceramics sintering made it possible to fabricate high-quality optical materials. The work is devoted to the structural and optical characterization of the ({Y_3}{Al_5}{O_{12}}, YAG) ceramics prepared by high-pressure low-temperature technique. The structural properties of the studied ceramic samples was obtained by X-ray diffraction. The studies of the total and in-line transmittance as well as optical scattering indicatrices were performed in visible and NIR ranges. The scatterer size ˜200 nm was estimated by Rayleigh-Gans-Debye model. It was shown that the studied samples demonstrate high transparency at 1064 nm. The nonlinear optical characterization of the samples was done by the self-action of the picosecond laser pulses at 1064 nm. The measured nonlinear optical response (χ^(3)) ˜ 10^{-11} esu) showed significant dependence on the sintering temperature variation.
NASA Astrophysics Data System (ADS)
Tewari, S.; Ghosh, A.; Bhattacharjee, A.
2016-11-01
Sintered pellets of zinc oxide (ZnO), both undoped and Al-doped are prepared through a chemical process. Dopant concentration of Aluminium in ZnO [Al/Zn in weight percentage (wt%)] is varied from 0 to 3 wt%. After synthesis structural characterisation of the samples are performed with XRD and SEM-EDAX which confirm that all the samples are of ZnO having polycrystalline nature with particle size from 108.6 to 116 nm. Frequency dependent properties like a.c. conductivity, capacitance, impedance and phase angle are measured in the frequency range 10 Hz to 100 kHz as a function of temperature (in the range 25-150 °C). Nature of a.c. conductivity in these samples indicates hopping type of conduction arising from localised defect states. The frequency and temperature dependent properties under study are found to be as per correlated barrier hoping model. Dielectric and impedance properties studied in the samples indicate distributed relaxation, showing decrease of relaxation time with temperature.
ε- and β-LiVOPO4: Phase Transformation and Electrochemistry.
Zhou, Hui; Shi, Yong; Xin, Fengxia; Omenya, Fredrick; Whittingham, M Stanley
2017-08-30
ε- and β-LiVOPO 4 were synthesized from the same precursor at different temperatures in an air atmosphere. ε-LiVOPO 4 is obtained at 400 and 700 °C. The 700 °C sample has better purity and crystallinity, but the 400 °C sample has a little better electrochemical performance due to its smaller particle size and the conducting carbon residue in the sample. β-LiVOPO 4 is formed between the above two temperatures, which gives slightly lower capacity than that of the ε-LiVOPO 4 sample, indicating higher kinetics of the lithium reaction for the ε phase than those of the β one. The phase transformation from ε to β then back reversibly to ε was also observed by ex situ X-ray diffraction. This thermal study verifies that ε-LiVOPO 4 is the more stable phase for LiVOPO 4 ; however, reaction kinetics control the phases formed at lower temperatures.
NASA Astrophysics Data System (ADS)
Vidya, S.; Solomon, Sam; Thomas, J. K.
2013-01-01
Nanocrystalline scheelite CaWO4, a promising material for low-temperature co-fired ceramic (LTCC) applications, has been successfully synthesized through a single-step autoignition combustion route. Structural analysis of the sample was performed by powder x-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and Raman spectroscopy. The XRD analysis revealed that the as-prepared sample was single phase with scheelite tetragonal structure. The basic optical properties and optical constants of the CaWO4 nanopowder were studied using ultraviolet (UV)-visible absorption spectroscopy, which showed that the material was a wide-bandgap semiconductor with bandgap of 4.7 eV at room temperature. The sample showed poor transmittance in the ultraviolet region but maximum transmission in the visible/near-infrared regions. The photoluminescence spectra recorded at different temperatures showed intense emission in the green region. The particle size estimated from transmission electron microscopy was 23 nm. The feasibility of CaWO4 for LTCC applications was studied from its sintering behavior. The sample was sintered at a relatively low temperature of 810°C to high density, without using any sintering aid. The surface morphology of the sintered sample was analyzed by scanning electron microscopy. The dielectric constant and loss factor of the sample measured at 5 MHz were found to be 10.50 and 1.56 × 10-3 at room temperature. The temperature coefficient of the dielectric constant was -88.71 ppm/°C. The experimental results obtained in this work demonstrate the potential of nano-CaWO4 as a low-temperature co-fired ceramic as well as an excellent luminescent material.
An Efficient, Robust, and Inexpensive Grinding Device for Herbal Samples like Cinchona Bark
Hansen, Steen Honoré; Holmfred, Else; Cornett, Claus; Maldonado, Carla; Rønsted, Nina
2015-01-01
An effective, robust, and inexpensive grinding device for the grinding of herb samples like bark and roots was developed by rebuilding a commercially available coffee grinder. The grinder was constructed to be able to provide various particle sizes, to be easy to clean, and to have a minimum of dead volume. The recovery of the sample when grinding as little as 50 mg of crude Cinchona bark was about 60%. Grinding is performed in seconds with no rise in temperature, and the grinder is easily disassembled to be cleaned. The influence of the particle size of the obtained powders on the recovery of analytes in extracts of Cinchona bark was investigated using HPLC. PMID:26839823
In situ study of in-beam cobalt suicide growth in silicon
NASA Astrophysics Data System (ADS)
Ruault, M.-O.; Fortuna, F.; Bernas, H.; Kaitasov, O.
1994-02-01
The control of buried suicide layer interfaces requires a systematic study of their formation conditions (implantation temperature, sample orientation, post-annealing conditions). At stoichiometric concentration, the layer roughness stems from the formation and overlap of B-type precipitates during implanted sample annealing. However, at such high concentrations several parameters interfere during suicide layer formation, particularly diffusion-limited precipitate growth and precipitate coalescence and Ostwald ripening. In order to analyze these factors separately, we have performed an in situ TEM study of the initial stages of CoSi 2 precipitate formation and growth in Si during 50 keV Co implantation to fluences between 10 15 and 1.5 × 10 16 Cocm -2, at temperatures between 350 and 650°C. At 350°C, the threshold fluence for suicide precipitate observation was 2 × 10 15 Cocm -2, and the size of the precipitates remained constant (about 4 nm) up to a fluence of 1.5 × 10 16 Cocm -2. At higher implantation temperatures, the average growth rate at 650°C is four times higher than at 500°C until the average size of the precipitates reaches ~ 8 nm. Then the growth rate is surprisingly independent of the implantation temperature. The results are discussed in the light of a recently developed precipitation kinetic analysis.
Is telomere length a molecular marker of past thermal stress in wild fish?
Debes, Paul V; Visse, Marko; Panda, Bineet; Ilmonen, Petteri; Vasemägi, Anti
2016-11-01
Telomeres protect eukaryotic chromosomes; variation in telomere length has been linked (primarily in homoeothermic animals) to variation in stress, cellular ageing and disease risk. Moreover, telomeres have been suggested to function as biomarker for quantifying past environmental stress, but studies in wild animals remain rare. Environmental stress, such as extreme environmental temperatures in poikilothermic animals, may result in oxidative stress that accelerates telomere attrition. However, growth, which may depend on temperature, can also contribute to telomere attrition. To test for associations between multitissue telomere length and past water temperature while accounting for the previous individual growth, we used quantitative PCR to analyse samples from 112 young-of-the-year brown trout from 10 natural rivers with average water temperature differences of up to 6°C (and an absolute maximum of 23°C). We found negative associations between relative telomere length (RTL) and both average river temperature and individual body size. We found no indication of RTL-temperature association differences among six tissues, but we did find indications for differences among the tissues for associations between RTL and body size; size trends, albeit nonsignificant in their differences, were strongest in muscle and weakest in fin. Although causal relationships among temperature, growth, oxidative stress, and cross-sectional telomere length remain largely unknown, our results indicate that telomere-length variation in a poikilothermic wild animal is associated with both past temperature and growth. © 2016 The Authors. Molecular Ecology Published by John Wiley & Sons Ltd.
Application of spatially gridded temperature and land cover data sets for urban heat island analysis
Gallo, Kevin; Xian, George Z.
2014-01-01
Two gridded data sets that included (1) daily mean temperatures from 2006 through 2011 and (2) satellite-derived impervious surface area, were combined for a spatial analysis of the urban heat-island effect within the Dallas-Ft. Worth Texas region. The primary advantage of using these combined datasets included the capability to designate each 1 × 1 km grid cell of available temperature data as urban or rural based on the level of impervious surface area within the grid cell. Generally, the observed differences in urban and rural temperature increased as the impervious surface area thresholds used to define an urban grid cell were increased. This result, however, was also dependent on the size of the sample area included in the analysis. As the spatial extent of the sample area increased and included a greater number of rural defined grid cells, the observed urban and rural differences in temperature also increased. A cursory comparison of the spatially gridded temperature observations with observations from climate stations suggest that the number and location of stations included in an urban heat island analysis requires consideration to assure representative samples of each (urban and rural) environment are included in the analysis.
Bulk and nanocrystalline electron doped Gd0.15Ca0.85MnO3: Synthesis and magnetic characterization
NASA Astrophysics Data System (ADS)
Dhal, Lakshman; Chattarpal; Nirmala, R.; Santhosh, P. N.; Kumary, T. Geetha; Nigam, A. K.
2014-09-01
Polycrystalline Gd0.15Ca0.85MnO3 sample was prepared by solid state reaction method and nanocrystalline samples of different grain sizes of the same were prepared by sol-gel method. Phase purity and composition were verified by room temperature X-ray diffraction and SEM-EDAX analysis. Magnetization data of bulk Gd0.15Ca0.85MnO3 in 5 kOe field shows a peak at 119 K (TN) suggesting an antiferromagnetic transition. Nanocrystalline Gd0.15Ca0.85MnO3 sample ( 54 nm size) also shows a cusp at 107 K and a broad thermal hysteresis between field cooled cooling (FCC) and field cooled warming (FCW) data around this temperature. This thermal hysteresis suggests possible crystal structural transition. Field variation of magnetization of bulk Gd0.15Ca0.85MnO3 at 5 K shows a tendency to saturate, but yields a magnetic moment value of only 1.12 μB/f.u. in 70 kOe. The value of magnetization of nanocrystalline sample at 5 K in 70 kOe field is slightly larger and is 1.38 μB/f.u. which is probably due to the surface moments of the nanoparticle samples. Both the samples show Curie-Weiss-like behaviour in their paramagnetic state.
Body temperature - a marker of infarct size in the era of early reperfusion.
Ben-Dor, Itsik; Haim, Moti; Rechavia, Eldad; Murininkas, Daniel; Nahon, Merav; Harell, Daniella; Porter, Avital; Iakobishvili, Zaza; Scapa, Erez; Battler, Alexander; Hasdai, David
2005-01-01
We measured body temperature in 40 consecutive patients treated for a first ST elevation acute myocardial infarction (AMI) with primary percutaneous coronary interventions. Left ventricular function was assessed by echocardiography, and blood samples were drawn for highly sensitive C-reactive protein (hs-CRP), white blood cell (WBC) count, fibrinogen, creatine kinase (CK), and cardiac troponin I levels (cTnI). The median (25th, 75th quartiles) peak 24-hour temperature was 37.4 degrees C (36.9 degrees C, 37.6 degrees C). Variables significantly associated with peak 24-hour temperature were CK (p = 0.01, r = 0.42), wall motion index (p = 0.01, r = 0.41), hs-CRP (p = 0.01, r = 0.41), and cTnI (p = 0.03, r = 0.35). There was no significant correlation between peak 24-hour temperature and WBC count (p = 0.39, r = 0.14) and fibrinogen (p = 0.12, r = 0.21). Thus, peak 24-hour body temperature after ST elevation AMI probably reflects infarct size rather than a nonspecific inflammatory response. Copyright 2005 S. Karger AG, Basel.
NASA Astrophysics Data System (ADS)
Li, Wanli; Vicente, C. L.; Xia, J. S.; Pan, W.; Tsui, D. C.; Pfeiffer, L. N.; West, K. W.
2009-05-01
The quantum Hall-plateau transition was studied at temperatures down to 1 mK in a random alloy disordered high mobility two-dimensional electron gas. A perfect power-law scaling with κ=0.42 was observed from 1.2 K down to 12 mK. This perfect scaling terminates sharply at a saturation temperature of Ts˜10mK. The saturation is identified as a finite-size effect when the quantum phase coherence length (Lϕ∝T-p/2) reaches the sample size (W) of millimeter scale. From a size dependent study, Ts∝W-1 was observed and p=2 was obtained. The exponent of the localization length, determined directly from the measured κ and p, is ν=2.38, and the dynamic critical exponent z=1.
Expression of Superparamagnetic Particles on FORC Diagrams
NASA Astrophysics Data System (ADS)
Hirt, A. M.; Kumari, M.; Crippa, F.; Petri-Fink, A.
2015-12-01
Identification of superparamagnetic (SP) particles in natural materials provides information on processes that lead to the new formation or dissolution of iron oxides. SP particles express themselves on first-order reversal curve (FORC) diagrams as a distribution centered near the origin of the diagram. Pike et al. (2001, GJI, 145, 721) demonstrated that thermal relaxation produces an upward shift in the FORC distribution, and attributed this to a pause encountered at each reversal field. In this study we examine the relationship between this upward shift and particles size on two sets of synthetic iron oxide nanoparticles. One set of coated magnetite particles have well-constrained particles size with 9, 16 and 20 nm as their diameter. A second set from the FeraSpin™ Series, consisting of FeraSpinXS, M and XL, were evaluated. Rock magnetic experiments indicate that the first set of samples is exclusively magnetite, whereas the FeraSpin samples contain predominantly magnetite with some degree of oxidation. Samples from both sets show that the upward shift of the FORC distribution at the origin increases with decreasing particle size. The amount of shift in the FeraSpin series is less when compared to the samples from the first set. This is attributed to the effect of interaction that counteracts the effect of thermal relaxation behavior of the SP particles. The FeraSpin series also shows a broader FORC distribution on the vertical axis that appears to be related to non-saturation of the hysteresis curve at maximum applied field. This non-saturation behavior can be due to spins of very fine particles or oxidation to hematite. AC susceptibility at low temperature indicates that particle interaction may affect the effective magnetic particle size. Our results suggest that the FORC distribution in pure SP particle systems provides information on the particle size distribution or oxidation, which can be further evaluated with low temperature techniques.
A. Broido; Hsiukang Yow
1977-01-01
Even before weight loss in the low-temperature pyrolysis of cellulose becomes significant, the average degree of polymerization of the partially pyrolyzed samples drops sharply. The gel permeation chromatograms of nitrated derivatives of the samples can be described in terms of a small number of mixed size populationsâeach component fitted within reasonable limits by a...
DOE Office of Scientific and Technical Information (OSTI.GOV)
Sudheesh, V. D.; Vinesh, A.; Lakshmi, N.
Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2}O{sub 4} has been prepared by self combustion method and studied using X-ray diffraction, Moessbauer spectroscopy and DC magnetization techniques. X-ray diffractogram shows highly crystalline nano sized sample with no impurity phases. The room temperature Moessbauer and magnetization measurements show the co-existence of superparamagnetic and ferrimagnetic particles in the sample. The presence of inter particle interaction is confirmed from the {delta}M(H) curve at 20K. The dependence of magnetic moment below blocking temperature in the field cooling curve indicates that the inter particle interaction is weak in the as prepared sample.
THE OCCURRENCE RATE OF SMALL PLANETS AROUND SMALL STARS
DOE Office of Scientific and Technical Information (OSTI.GOV)
Dressing, Courtney D.; Charbonneau, David, E-mail: cdressing@cfa.harvard.edu
We use the optical and near-infrared photometry from the Kepler Input Catalog to provide improved estimates of the stellar characteristics of the smallest stars in the Kepler target list. We find 3897 dwarfs with temperatures below 4000 K, including 64 planet candidate host stars orbited by 95 transiting planet candidates. We refit the transit events in the Kepler light curves for these planet candidates and combine the revised planet/star radius ratios with our improved stellar radii to revise the radii of the planet candidates orbiting the cool target stars. We then compare the number of observed planet candidates to themore » number of stars around which such planets could have been detected in order to estimate the planet occurrence rate around cool stars. We find that the occurrence rate of 0.5-4 R{sub Circled-Plus} planets with orbital periods shorter than 50 days is 0.90{sup +0.04}{sub -0.03} planets per star. The occurrence rate of Earth-size (0.5-1.4 R{sub Circled-Plus }) planets is constant across the temperature range of our sample at 0.51{sub -0.05}{sup +0.06} Earth-size planets per star, but the occurrence of 1.4-4 R{sub Circled-Plus} planets decreases significantly at cooler temperatures. Our sample includes two Earth-size planet candidates in the habitable zone, allowing us to estimate that the mean number of Earth-size planets in the habitable zone is 0.15{sup +0.13}{sub -0.06} planets per cool star. Our 95% confidence lower limit on the occurrence rate of Earth-size planets in the habitable zones of cool stars is 0.04 planets per star. With 95% confidence, the nearest transiting Earth-size planet in the habitable zone of a cool star is within 21 pc. Moreover, the nearest non-transiting planet in the habitable zone is within 5 pc with 95% confidence.« less
Fabrication of setup for high temperature thermal conductivity measurement.
Patel, Ashutosh; Pandey, Sudhir K
2017-01-01
In this work, we report the fabrication of an experimental setup for high temperature thermal conductivity (κ) measurement. It can characterize samples with various dimensions and shapes. Steady state based axial heat flow technique is used for κ measurement. Heat loss is measured using parallel thermal conductance technique. Simple design, lightweight, and small size sample holder is developed by using a thin heater and limited components. Low heat loss value is achieved by using very low thermal conductive insulator block with small cross-sectional area. Power delivered to the heater is measured accurately by using 4-wire technique and for this, the heater is developed with 4 wires. This setup is validated by using Bi 0.36 Sb 1.45 Te 3 , polycrystalline bismuth, gadolinium, and alumina samples. The data obtained for these samples are found to be in good agreement with the reported data. The maximum deviation of 6% in the value κ is observed. This maximum deviation is observed with the gadolinium sample. We also report the thermal conductivity of polycrystalline tellurium from 320 K to 550 K and the nonmonotonous behavior of κ with temperature is observed.
The impedance spectroscopy analysis of complex perovskite Sr2YbSbO6
NASA Astrophysics Data System (ADS)
Barua, A.; Maity, S.; Mondal, R.; Kumar, S.
2018-04-01
Herein, we have reported the dielectric properties of single phase monoclinic double perovskite oxide of Sr2YbSbO6 having lattice parameter a=5.79 Å, b=5.79 Å, c=8.19 Å and β = 90.136° with grain size ranging between 0.5 to 2.4 µm. The sample has been synthesized by solid state ceramic method. We have performed the impedence spectroscopic study of the sample in the frequency range of 40 Hz to 5 MHz at various temperatures. The relaxation in the sample is polydispersive in nature and obeys the Cole-Cole model. The values of dielectric permittivity and loss tangent at room temperature are 117.94 and 0.18 respectively. The temperature variation of dc conductivity follows the Arrhenius Law with activation energy 0.2 eV and the conduction mechanism of the sample is governed by p-type polaron hopping. Due to its high dielectric permittivity and low loss tangent the sample can be fruitfully utilized for the fabrication of radio frequency devices.
Invited paper: Dielectric properties of CaCu3Ti4O12 polycrystalline ceramics
NASA Astrophysics Data System (ADS)
Lee, Sung Yun; Hong, Youn Woo; Yoo, Sang Im
2011-12-01
We investigated the relationship between the microstructures and dielectric properties of various CaCu3Ti4O12 (CCTO) polycrystalline ceramics sintered in air. An abrupt increase in the dielectric constant ( ɛ r) from ˜3,000 to ˜170,000 at 1 kHz occurred with increasing the sintering temperature from 980 to 1000°C for 12 h, respectively, which was accompanied by a very large increase in the average grain size from 5 to 300 µm, respectively, due to an abnormal grain growth. With further increasing the sintering temperature, the ɛ r value at 1 kHz was slightly decreased to ˜150,000 at 1020°C with no variation in the average grain size, significantly decreased to ˜77,000 at 1040°C with a large decrease in the average grain size (˜150 µm), and then maintained the values of ˜76,000 and ˜69,000 at 1060 and 1080°C, respectively, without noticeable variation in the average grain size. While no abnormal grain growth occurred in the CCTO samples sintered at 980°C for the holding time to 24 h and thus their ɛ r values showed relatively lower ɛ r values (< ˜4,000 at 1 kHz), the abnormal grain growth occurred in the samples after a certain holding time at a given sintering temperature of higher than 1000°C and thus their ɛ r values abruptly increased. Analyses by the complex impedance ( Z*) and modulus ( M*) spectroscopy revealed that the ɛ r values of the CCTO samples were dominantly affected by the electrical properties of grain boundary so that high ɛ r values over 10,000 at 1 kHz were attributable to the high capacitance ( C) of grain boundary, which is in good agreement with grain boundary internal barrier layer capacitor (IBLC) model.
NASA Astrophysics Data System (ADS)
Lubenets, S. V.; Rusakova, A. V.; Fomenko, L. S.; Moskalenko, V. A.
2018-01-01
The anisotropy of microhardness of pure α-Ti single crystals, indentation size effect in single-crystal, course grained (CG) pure and nanocrystalline (NC) VT1-0 titanium, as well as the temperature dependences of the microhardness of single-crystal and CG Ti in the temperature range 77-300 K were studied. The minimum value of hardness was obtained when indenting into the basal plane (0001). The indentation size effect (ISE) was clearly observed in the indentation of soft high-purity single-crystal iodide titanium while it was the least pronounced in a sample of nanocrystalline VT1-0 titanium. It has been demonstrated that the ISE can be described within the model of geometrically necessary dislocations (GND), which follows from the theory of strain gradient plasticity. The true hardness and others parameters of the GND model were determined for all materials. The temperature dependence of the microhardness is in agreement with the idea of the governing role of Peierls relief in the dislocation thermally-activated plastic deformation of pure titanium as has been earlier established and justified in macroscopic tensile investigations at low temperatures. The activation energy and activation volume of dislocation motion in the strained region under the indenter were estimated.
Global Sensitivity Analysis with Small Sample Sizes: Ordinary Least Squares Approach
DOE Office of Scientific and Technical Information (OSTI.GOV)
Davis, Michael J.; Liu, Wei; Sivaramakrishnan, Raghu
2016-12-21
A new version of global sensitivity analysis is developed in this paper. This new version coupled with tools from statistics, machine learning, and optimization can devise small sample sizes that allow for the accurate ordering of sensitivity coefficients for the first 10-30 most sensitive chemical reactions in complex chemical-kinetic mechanisms, and is particularly useful for studying the chemistry in realistic devices. A key part of the paper is calibration of these small samples. Because these small sample sizes are developed for use in realistic combustion devices, the calibration is done over the ranges of conditions in such devices, with amore » test case being the operating conditions of a compression ignition engine studied earlier. Compression ignition engines operate under low-temperature combustion conditions with quite complicated chemistry making this calibration difficult, leading to the possibility of false positives and false negatives in the ordering of the reactions. So an important aspect of the paper is showing how to handle the trade-off between false positives and false negatives using ideas from the multiobjective optimization literature. The combination of the new global sensitivity method and the calibration are sample sizes a factor of approximately 10 times smaller than were available with our previous algorithm.« less
NASA Astrophysics Data System (ADS)
Nopwinyuwong, Atchareeya; Kitaoka, Takuya; Boonsupthip, Waraporn; Pechyen, Chiravoot; Suppakul, Panuwat
2014-09-01
Polydiacetylene (PDA)/silica nanocomposites were synthesized by self-assembly method using polymerizable amphiphilic diacetylene monomers, 10,12-pentacosadiynoic acid (PCDA). Addition of cationic surfactants (PDADMAC and CTAB) to PDA/SiO2 nanocomposites induced higher intermolecular force which affected their size, shape and color transition. Pure PDA, PDA/SiO2, PDA/SiO2/PDADMAC and PDA/SiO2/CTAB were investigated by particle size analysis, TEM, SEM, UV-vis spectroscopy and FT-IR. It was found that the PDA/SiO2 nanocomposites exhibited slightly larger particle sizes than those of other samples. The PDA/SiO2 nanocomposites with a core-shell structure were almost regarded as spherical-shaped particles. Cationic surfactants, especially CTAB, presumably affected the particle size and shape of PDA/SiO2 nanocomposites due to the disruption of hydrogen bonding between PDA head group and ammonium group. The colorimetric response of both PDA/SiO2/surfactant and surfactant-free PDA/SiO2 aqueous solutions directly changed in relation to time and temperature; thus they were expected to be applied as a new polymer-based time-temperature indicator (TTI).
NASA Astrophysics Data System (ADS)
Kennett, Shane C.
Three low-carbon ASTM A514 microalloyed steels were used to assess the effects of austenite conditioning on the microstructure and mechanical properties of martensite. A range of prior austenite grain sizes with and without thermomechanical processing were produced in a Gleeble RTM 3500 and direct-quenched. Samples in the as-quenched, low temperature tempered, and high temperature tempered conditions were studied. The microstructure was characterized with scanning electron microscopy, electron backscattered diffraction, transmission electron microscopy, and x-ray diffraction. The uniaxial tensile properties and Charpy V-notch properties were measured and compared with the microstructural features (prior austenite grain size, packet size, block size, lath boundaries, and dislocation density). For the equiaxed prior austenite grain conditions, prior austenite grain size refinement decreases the packet size, decreases the block size, and increases the dislocation density of as-quenched martensite. However, after high temperature tempering the dislocation density decreases with prior austenite grain size refinement. Thermomechanical processing increases the low angle substructure, increases the dislocation density, and decreases the block size of as-quenched martensite. The dislocation density increase and block size refinement is sensitive to the austenite grain size before ausforming. The larger prior austenite grain size conditions have a larger increase in dislocation density, but the small prior austenite grain size conditions have the largest refinement in block size. Additionally, for the large prior austenite grain size conditions, the packet size increases with thermomechanical processing. The strength of martensite is often related to an effective grain size or carbon concentration. For the current work, it was concluded that the strength of martensite is primarily controlled by the dislocation density and dislocation substructure; which is related to a grain size and carbon concentration. In the microyielding regime, the strength and work hardening is related to the motion of unpinned dislocation segments. However, with tensile strain, a dislocation cell structure is developed and the flow strength (greater than 1% offset) is controlled by the dislocation density following a Taylor hardening model, thereby ruling out any grain size effects on the flow strength. Additionally, it is proposed that lath boundaries contribute to strength. It is shown that the strength differences associated with thermomechanically processed steels can be fully accounted for by dislocation density differences and the effect of lath boundaries. The low temperature ductile to brittle transition of martensite is controlled by the martensite block size, packet size, and prior austenite grain size. However, the effect of block size is likely small in comparison. The ductile to brittle transition temperature is best correlated to the inverse square root of the martensite packet size because large crack deflections are typical at packet boundaries.
In situ synchrotron investigation of grain growth behavior of nano-grained UO 2
DOE Office of Scientific and Technical Information (OSTI.GOV)
Miao, Yinbin; Yao, Tiankai; Lian, Jie
Here, we report on the study of grain growth kinetics in nano-grained UO 2 samples. Dense nano-grained UO 2 samples with well-controlled stoichiometry and grain size were fabricated using the spark plasma sintering technique. To determine the grain growth kinetics at elevated temperatures, a synchrotron wide-angle X-ray scattering (WAXS) study was performed in situ to measure the real-time grain size evolution based on the modified Williamson-Hall analysis. The unique grain growth kinetics of nanocrystalline UO 2 at 730 °C and 820 °C were observed and explained by the difference in mobility of various grain boundaries.
In situ synchrotron investigation of grain growth behavior of nano-grained UO 2
Miao, Yinbin; Yao, Tiankai; Lian, Jie; ...
2017-01-09
Here, we report on the study of grain growth kinetics in nano-grained UO 2 samples. Dense nano-grained UO 2 samples with well-controlled stoichiometry and grain size were fabricated using the spark plasma sintering technique. To determine the grain growth kinetics at elevated temperatures, a synchrotron wide-angle X-ray scattering (WAXS) study was performed in situ to measure the real-time grain size evolution based on the modified Williamson-Hall analysis. The unique grain growth kinetics of nanocrystalline UO 2 at 730 °C and 820 °C were observed and explained by the difference in mobility of various grain boundaries.
NASA Astrophysics Data System (ADS)
Kamal, Abu Sayed Md
Wide adoption by the construction industry of Fibre Reinforced Polymer (FRP) rebars - a relatively recent construction material that offers numerous advantages of corrosion resistance, higher strength, lighter weight, etc. over conventional reinforcing materials for concrete, such as steel - is at least partially impeded due to a lack of an effective long term in-service performance prediction model and relatively high initial costs. A reliable service life prediction model for FRP composites in concrete depends on a clear understanding of the transport mechanisms of potentially harmful chemical species into the FRP composites and their subsequent contribution to any potentially active degradation mechanism(s). To identify which mechanisms control the degradation of Glass Fibre Reinforced Polymers (GFRP) in alkaline environments, GFRP rebars were immersed into simulated concrete pore solutions and subjected to accelerated ageing tests (Phase 1). The conditioned samples were analyzed by various electron microscopy (SEM, EDS) and spectroscopic methods (FTIR). Analyses of these tests revealed that fibre-matrix debonding took place in few samples exposed to 75 °C (the highest temperature considered in this study), and tested after one year, despite the fact that the glass fibres and polymer matrix remained essentially intact and that no penetration of alkalis into the GFRP rebars was observed. Hence, this study shows that the Vinyl Ester (VE) polymer matrix used acts as an effective semi-permeable membrane by allowing the penetration of water while blocking alkali ions. The findings showing that most of the damage seems to be confined to the fibre-matrix interphase (or interface), under the considered test conditions, stimulated an investigation on the effects of sizing on the strength retention and water up-take of GFRP rebars in Phase 2 of the testing program. In order to study the effects of sizing on the properties of GFRP rebars, GFRP custom plane sheets with sized and desized glass fibers were produced and exposed to deionized water at 4 °C, 23 °C, and 50 °C. Irrespective of sample types, the tensile strength decreased with temperature while the mass gain and moisture diffusivity increased with temperature. However, the sized samples showed a similar mass gain behavior as the desized ones, at the same exposure environment. This study confirms that sizing in GFRP custom plane sheets contributes not only to the initial strength of the composite by enhancing the adhesion between the glass fibre and a matrix, but also to the strength retention (i.e., durability) when exposed to harsh environments. The experiments of Phase 2 were carried out at 100% relative humidity (RH). However, field service conditions vary with respect to RH and temperature for GFRP composites in concrete. Therefore, a further study was conducted to investigate the effects of RH and temperature on the properties of GFRP rebars in Phase 3. The effects of RH were investigated by exposing GFRP rebars to nine RH environments (9%-100%) while monitoring mass changes during drying and wetting. Moreover, the thermal effects of GFRP rebars on water uptake in deionized water at 4 °C, 23 °C, and 50 °C were studied and compared with those for GFRP custom plane sheets. The effects of RH on drying and wetting for GFRP rebars exhibited a hysteretic behavior. The percent of mass gain at 100% RH showed a significant difference from that in other RH environments. Mass gain and moisture diffusivity were found to increase for both rebars and custom sheets with increasing temperature. A typical Fickian behaviour of water absorption was observed for both types of samples at all exposure conditions, except the GFRP rebars at higher temperatures (starting at 50 °C) which showed non-Fickian behaviour for water absorption. The dependence of the diffusion coefficient on temperature was found to follow the Arrhenius equation. (Abstract shortened by UMI.)
Heather, F J; Childs, D Z; Darnaude, A M; Blanchard, J L
2018-01-01
Accurate information on the growth rates of fish is crucial for fisheries stock assessment and management. Empirical life history parameters (von Bertalanffy growth) are widely fitted to cross-sectional size-at-age data sampled from fish populations. This method often assumes that environmental factors affecting growth remain constant over time. The current study utilized longitudinal life history information contained in otoliths from 412 juveniles and adults of gilthead seabream, Sparus aurata, a commercially important species fished and farmed throughout the Mediterranean. Historical annual growth rates over 11 consecutive years (2002-2012) in the Gulf of Lions (NW Mediterranean) were reconstructed to investigate the effect of temperature variations on the annual growth of this fish. S. aurata growth was modelled linearly as the relationship between otolith size at year t against otolith size at the previous year t-1. The effect of temperature on growth was modelled with linear mixed effects models and a simplified linear model to be implemented in a cohort Integral Projection Model (cIPM). The cIPM was used to project S. aurata growth, year to year, under different temperature scenarios. Our results determined current increasing summer temperatures to have a negative effect on S. aurata annual growth in the Gulf of Lions. They suggest that global warming already has and will further have a significant impact on S. aurata size-at-age, with important implications for age-structured stock assessments and reference points used in fisheries.
Zhang, Xiao-Lei; Zhang, Jie; Fan, Tuo; Ren, Wen-Jie; Lai, Chun-Hong
2014-09-01
In order to make surface-enhanced Raman scattering (SERS) substrates contained more "hot spots" in a three-dimensional (3D) focal volume, and can be adsorbed more probe molecules and metal nanoparticles, to obtain stronger Raman spectral signal, a new structure based on vertically aligned carbon nanotubes (CNTs) coated by Ag nanoparticles for surface Raman enhancement is presented. The vertically aligned CNTs are synthesized by chemical vapor deposition (CVD). A silver film is first deposited on the vertically aligned CNTs by magnetron sputtering. The samples are then annealed at different temperature to cause the different size silver nanoparticles to coat on the surface and sidewalls of vertically aligned CNTs. The result of scanning electron microscopy(SEM) shows that Ag nanoparticles are attached onto the sidewalls and tips of the vertically aligned CNTs, as the annealing temperature is different , pitch size, morphology and space between the silver nanoparticles is vary. Rhodamine 6G is served as the probe analyte. Raman spectrum measurement indicates that: the higher the concentration of R6G, the stronger the Raman intensity, but R6G concentration increase with the enhanced Raman intensity varies nonlinearly; when annealing temperature is 450 °C, the average size of silver nanoparticles is about 100 to 120 nm, while annealing temperature is 400 °C, the average size is about 70 nm, and the Raman intensity of 450 °C is superior to the annealing temperature that of 400 °C and 350 °C.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Simpraditpan, Athapon; Wirunmongkol, Thanakorn; Pavasupree, Sorapong, E-mail: sorapongp@yahoo.com
2013-09-01
Graphical abstract: - Highlights: • Nanofibers were prepared from low-cost ilmenite mineral via simple hydrothermal. • High photocatalyst nanofibers were prepared via post heat treatment method. • The nanofibers calcined at 100–700 °C for 2 h maintained nanofiber structure. • The calcined nanofibers at 400 °C showed the highest photocatalytic activity. - Abstract: Titanate nanofibers were synthesized via the hydrothermal method (120 °C for 72 h) using natural ilmenite mineral (FeTiO{sub 3}) as the starting material. The samples were characterized by X-ray diffraction (XRD), X-ray fluorescent (XRF), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and Brunauer–Emmett–Teller (BET) for specificmore » surface area. The nanofibers were 20–90 nm in diameter and 2–7 μm in length. The as-synthesized nanofibers calcined at 300–400 °C showed TiO{sub 2} (B) whereas the nanofibers calcined at 500 °C revealed a mixture of two phases of TiO{sub 2} (B) and anatase. The nanofibers calcined at high temperature of 600–1000 °C showed a mixture of tri-crystalline of anatase, rutile, and Fe{sub 2}O{sub 3}. The rutile phase increased with increasing calcination temperature. The nanofibers calcined at 300–700 °C maintained their structure while the morphology of the nanofibers calcined at 800–1000 °C transformed into submicron rod-like structure. This increase of calcination temperature led to the phase transformation from thermodynamically metastable anatase to the most stable form of rutile phase. The crystallite size of prepared samples increased with increasing calcination temperature. Interestingly, with increasing calcination temperature, the absorption edge of the prepared samples shows an obvious shift to visible light region due to the change of crystallite phase and increased crystallite size. Therefore, the band gap energy of the prepared samples became narrower with increasing calcination temperature. Furthermore, the photocatalytic activity of the nanofibers calcined at 400 °C for 2 h was found to be not merely higher than those of the commercially available TiO{sub 2} nanoparticles powders (P-25, JRC-01, and JRC-03) but also the highest of all the samples in this study.« less
Anisotropic dielectric properties of two-dimensional matrix in pseudo-spin ferroelectric system
NASA Astrophysics Data System (ADS)
Kim, Se-Hun
2016-10-01
The anisotropic dielectric properties of a two-dimensional (2D) ferroelectric system were studied using the statistical calculation of the pseudo-spin Ising Hamiltonian model. It is necessary to delay the time for measurements of the observable and the independence of the new spin configuration under Monte Carlo sampling, in which the thermal equilibrium state depends on the temperature and size of the system. The autocorrelation time constants of the normalized relaxation function were determined by taking temperature and 2D lattice size into account. We discuss the dielectric constants of a two-dimensional ferroelectric system by using the Metropolis method in view of the Slater-Takagi defect energies.
Localized diffusive motion on two different time scales in solid alkane nanoparticles
NASA Astrophysics Data System (ADS)
Wang, S.-K.; Mamontov, E.; Bai, M.; Hansen, F. Y.; Taub, H.; Copley, J. R. D.; García Sakai, V.; Gasparovic, G.; Jenkins, T.; Tyagi, M.; Herwig, K. W.; Neumann, D. A.; Montfrooij, W.; Volkmann, U. G.
2010-09-01
High-energy-resolution quasielastic neutron scattering on three complementary spectrometers has been used to investigate molecular diffusive motion in solid nano- to bulk-sized particles of the alkane n-C32H66. The crystalline-to-plastic and plastic-to-fluid phase transition temperatures are observed to decrease as the particle size decreases. In all samples, localized molecular diffusive motion in the plastic phase occurs on two different time scales: a "fast" motion corresponding to uniaxial rotation about the long molecular axis; and a "slow" motion attributed to conformational changes of the molecule. Contrary to the conventional interpretation in bulk alkanes, the fast uniaxial rotation begins in the low-temperature crystalline phase.
NASA Astrophysics Data System (ADS)
Shekar, Yamini
This research investigates the nano-scale pore structure of cementitious mortars undergoing delayed ettringite formation (DEF) using small angle x-ray scattering (SAXS). DEF has been known to cause expansion and cracking during later ages (around 4000 days) in concrete that has been heat cured at temperatures of 70°C or above. Though DEF normally occurs in heat cured concrete, mass cured concrete can also experience DEF. Large crystalline pressures result in smaller pore sizes. The objectives of this research are: (1) to investigate why some samples expand early than later expansion, (2) to evaluate the effects of curing conditions and pore size distributions at high temperatures, and (3) to assess the evolution of the pore size distributions over time. The most important outcome of the research is the pore sizes obtained from SAXS were used in the development of a 3-stage model. From the data obtained, the pore sizes increase in stage 1 due to initial ettringite formation and in turn filling up the smallest pores. Once the critical pore size threshold is reached (around 20nm) stage 2 is formed due to cracking which tends to decrease in the pore sizes. Finally, in stage 3, the cracking continues, therefore increasing in the pore size.
Size-controlled synthesis of nanocrystalline CdSe thin films by inert gas condensation
NASA Astrophysics Data System (ADS)
Sharma, Jeewan; Singh, Randhir; Kumar, Akshay; Singh, Tejbir; Agrawal, Paras; Thakur, Anup
2018-02-01
Size, shape and structure are considered to have significant influence on various properties of semiconducting nanomaterials. Different properties of these materials can be tailored by controlling the size. Size-controlled CdSe crystallites ranging from ˜ 04 to 95 nm were deposited by inert gas-condensation technique (IGC). In IGC method, by controlling the inert gas pressure in the condensation chamber and the substrate temperature or both, it was possible to produce nanoparticles with desired size. Structure and crystallite size of CdSe thin films were determined from Hall-Williamson method using X-ray diffraction data. The composition of CdSe samples was estimated by X-ray microanalysis. It was confirmed that CdSe thin film with different nanometer range crystallite sizes were synthesized with this technique, depending upon the synthesis conditions. The phase of deposited CdSe thin films also depend upon deposition conditions and cubic to hexagonal phase transition was observed with increase in substrate temperature. The effect of crystallite size on optical and electrical properties of these films was also studied. The crystallite size affects the optical band gap, electrical conductivity and mobility activation of nanocrystalline CdSe thin films. Mobility activation study suggested that there is a quasi-continuous linear distribution of three different trap levels below the conduction band.
NASA Astrophysics Data System (ADS)
Hrutkay, Kyle
Haynes 230 and Inconel 617 are austenitic nickel based superalloys, which are candidate structural materials for next generation high temperature nuclear reactors. High temperature deformation behavior of Haynes 230 and Inconel 617 have been investigated at the microstructural level in order to gain a better understanding of mechanical properties. Tensile tests were performed at strain rates ranging from 10-3-10-5 s -1 at room temperature, 600 °C, 800 °C and 950 °C. Subsequent microstructural analysis, including Scanning Electron Microscopy, Transmission Electron Microscopy, Energy-Dispersive X-ray Spectroscopy, and X-Ray Diffraction were used to relate the microstructural evolution at high temperatures to that of room temperature samples. Grain sizes and precipitate morphologies were used to determine high temperature behavior and fracture mechanics. Serrated flow was observed at intermediate and high temperatures as a result of discontinuous slip and dynamic recrystallization. The amplitude of serration increased with a decrease in the strain rate and increase in the temperature. Dynamic strain ageing was responsible for serrations at intermediate temperatures by means of a locking and unlocking phenomenon between dislocations and solute atoms. Dynamic recrystallization nucleated by grain and twin bulging resulting in a refinement of grain size. Existing models found in the literature were discussed to explain both of these phenomena.
Surface properties of heat-induced soluble soy protein aggregates of different molecular masses.
Guo, Fengxian; Xiong, Youling L; Qin, Fang; Jian, Huajun; Huang, Xiaolin; Chen, Jie
2015-02-01
Suspensions (2% and 5%, w/v) of soy protein isolate (SPI) were heated at 80, 90, or 100 °C for different time periods to produce soluble aggregates of different molecular sizes to investigate the relationship between particle size and surface properties (emulsions and foams). Soluble aggregates generated in these model systems were characterized by gel permeation chromatography and sodium dodecyl sulfate-polyacrylamide gel electrophoresis. Heat treatment increased surface hydrophobicity, induced SPI aggregation via hydrophobic interaction and disulfide bonds, and formed soluble aggregates of different sizes. Heating of 5% SPI always promoted large-size aggregate (LA; >1000 kDa) formation irrespective of temperature, whereas the aggregate size distribution in 2% SPI was temperature dependent: the LA fraction progressively rose with temperature (80→90→100 °C), corresponding to the attenuation of medium-size aggregates (MA; 670 to 1000 kDa) initially abundant at 80 °C. Heated SPI with abundant LA (>50%) promoted foam stability. LA also exhibited excellent emulsifying activity and stabilized emulsions by promoting the formation of small oil droplets covered with a thick interfacial protein layer. However, despite a similar influence on emulsion stability, MA enhanced foaming capacity but were less capable of stabilizing emulsions than LA. The functionality variation between heated SPI samples is clearly related to the distribution of aggregates that differ in molecular size and surface activity. The findings may encourage further research to develop functional SPI aggregates for various commercial applications. © 2015 Institute of Food Technologists®
Study of the glow curve structure of the minerals separated from black pepper (Piper nigrum L.)
NASA Astrophysics Data System (ADS)
Guzmán, S.; Ruiz Gurrola, B.; Cruz-Zaragoza, E.; Tufiño, A.; Furetta, C.; Favalli, A.; Brown, F.
2011-04-01
The inorganic mineral fraction extracted from black pepper (Piper nigrum L.) has been analysed using a thermoluminescence (TL) method, investigating the glow curve structure, including an evaluation of the kinetic parameters. Different grain sizes, i.e. 10, 74, and 149 μm, were selected from commercial black pepper. The X-ray diffraction of the inorganic fraction shows that quartz is the main mineral present in it. The samples were exposed to 1-25 kGy doses by gamma rays of 60Co in order to analyse the thermally stimulated luminescence response as a function of the delivered dose. The glow curves show a complex structure for different grain sizes of the pepper mineral samples. The fading of the TL signal at room temperature was obtained after irradiation, and it was observed that the maximum peaks of the glow curves shift towards higher values of the temperature when the elapsed time from irradiation increases. It seems that the fading characteristic may be related to a continuous trap distribution responsible for the complex structure of the glow curve. Similar glow curves structure behaviour was found under ultraviolet irradiation of the samples. The activation energy and the frequency factor were determined from the glow curves of different grain sizes using a deconvolution programme because of the evident complexity of the structure.
Recrystallization and grain growth phenomena in a particle-reinforced aluminum composite
NASA Astrophysics Data System (ADS)
van Aken, D. C.; Krajewski, P. E.; Vyletel, G. M.; Allison, J. E.; Jones, J. W.
1995-06-01
Recrystallization and grain growth in a 2219/TiC/15p composite were investigated as functions of the amount of deformation and deformation temperature. Both cold and hot deformed samples were annealed at the normal solution treatment temperature of 535 °C. It was shown that large recrystallized grain diameters, relative to the interparticle spacing, could be produced in a narrow range of deformation for samples cold-worked and those hot-worked below 450 °C. For cold-worked samples, between 4 to 6 pct deformation, the recrystallized grain diameters varied from 530 to 66 μm as the amount of deformation increased. Subsequent grain growth was not observed in these recrystallized materials and noncompact grain shapes were observed. For deformations greater than 15 pct, recrystallized grain diameters less than the interparticle spacing were observed and subsequent grain growth produced a pinned grain diameter of 27 μm. The pinned grain diameter agreed well with an empirical model based on three dimensional (3-D) Monte Carlo simulations of grain growth and particle pinning in a two-phase material. Tensile properties were determined as a function of grain size, and it was shown that grain size had a weak influence on yield strength. A maximum in the yield strength was observed at a grain size larger than the normal grain growth and particle-pinned diameter.
Liu, Shuxin; Wang, Haibin; Yin, Hengbo; Wang, Hong; He, Jichuan
2014-03-01
The carbon coated LiFePO4 (LiFePO4/C) nanocomposites materials were successfully synthesized by sol-gel method. The microstructure and morphology of LiFePO4/C nanocomposites were characterized by X-ray diffraction, Raman spectroscopy and scanning electron microscopy. The results showed that the carbon layers decomposed by different dispersant and carbon source had different graphitization degree, and the sugar could decompose to form more graphite-like structure carbon. The carbon source and heat-treatment temperature had some effect on the particle size and morphology, the sample LFP-S700 synthesized by adding sugar as carbon source at 700 degrees C had smaller particle size, uniform size distribution and spherical shape. The electrochemical behavior of LiFePO4/C nanocomposites was analyzed using galvanostatic measurements and cyclic voltammetry (CV). The results showed that the sample LFP-S700 had higher discharge specific capacities, higher apparent lithium ion diffusion coefficient and lower charge transfer resistance. The excellent electrochemical performance of sample LFP-S700 could be attributed to its high graphitization degree of carbon, smaller particle size and uniform size distribution.
NASA Astrophysics Data System (ADS)
Pohl, Leos; Britt, Daniel
2017-10-01
Some sub-types of carbonaceous chondrites contain a significant amount of hydrated minerals which produce specific absorption lines, typically due to the presence of hydroxyls. However, if these asteroids have come close enough to the Sun during their history, the high temperatures might have resulted in mineral decomposition and consequent loss of hydroxyl (or water) molecules in the surface layer and even to certain depths. Determination of the hydration state of phyllosilicates typically found on asteroids as well as the relative quantities of hydrated to desiccated phyllosilicates relies on experimental data - the temperature and rate of dehydration. Both dehydration temperature and rate depend on pressure. The rate also depends on the temperature. Experimentally determined phase curves for serpentine, that show for example decomposition of antigorite to forsterite and enstatite or talc and water, exist for GPa pressure levels. For antigorite, these temperatures span the range 500-750°C for pressures between 0.1 GPa and 8 GPa. However, these data are not suitable for vacuum environment found on asteroids; further, at lower pressures, the available data suggest a monotonically decreasing dehydration temperature with decreasing pressure. Also, the available data suggest dependence of both dehydration temperature and rate on the grain size distribution of the mineral. We have determined the temperature and rate of dehydration of the serpentine polymorphs antigorite, lizardite, cronstedtite, under high vacuum conditions and for various grain size distributions. The grain size distributions have been determined by particle analyzer and each sample source was also analyzed using X-Ray Diffraction.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ashtar, M.; Munir, A.; Anis-ur-Rehman, M.
2016-07-15
Graphical abstract: Variation of AC conductivity (σ{sub AC}) as a function of natural log of angular frequency (lnω) for Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2-x}Cr{sub x}O{sub 4} nanoferrites at room temperature. - Highlights: • Cr doped mixed Ni-Zn ferrites were successfully synthesized by a newly developed WOWS sol gel technique. • The specific surface area and specific surface area to volume ratio increased with decrease in particle size. • The resonance peaks appeared in dielectric loss graphs, shifting towards low frequency with the increase in Cr concentration. • The prepared samples have the lowest values of the dielectric constant. • The dielectricmore » constant were observed to be inversely proportional to square root of the AC resistivity. - Abstract: Cr{sup +3} doped Ni-Zn nanoferrite samples with composition Ni{sub 0.5}Zn{sub 0.5}Fe{sub 2-x}Cr{sub x}O{sub 4}(x = 0.1, 0.2, 0.3, 0.4) were synthesized With Out Water and Surfactant (WOWS) sol-gel technique. The structural, morphological and dielectric properties of the samples were investigated. The lattice constant, crystallite size, theoretical density and porosity of each sample were obtained from X-ray diffraction (XRD) data. The specific surface area and specific surface area to volume ratio increased with the decrease in the size of Cr{sup +3} doped Ni-Zn ferrite nanoparticles, as the concentration of Cr{sup +3} increased. The SEM analysis revealed that the particles were of nano size and of spherical shape. The dielectric parameters such as dielectric constant (ε′) and dielectric loss (tanδ) of all the samples as a function of frequency at room temperature were measured. The AC conductivity (σ{sub AC}) was determined from the dielectric parameters, which showed increasing trend with the rise in frequency.« less
Structural, magnetic and optical properties of ZnO nanostructures converted from ZnS nanoparticles
DOE Office of Scientific and Technical Information (OSTI.GOV)
Patel, Prayas Chandra; Ghosh, Surajit; Srivastava, P.C., E-mail: pcsrivastava50@gmail.com
Graphical abstract: The phase conversion of ZnS to highly crystalline hexagonal ZnO was done by heat treatment. - Highlights: • Phase change of cubic ZnS to hexagonal ZnO via heat treatment. • Band gap was found to decrease with increasing calcinations temperature. • ZnO samples have higher magnetic moment than ZnS. • Blocking Temperature of the samples is well above room temperature. • Maximum negative%MR with saturation value ∼38% was found for sample calcined at 600° C. - Abstract: The present work concentrates on the synthesis of cubic ZnS and hexagonal ZnO semiconducting nanoparticle from same precursor via co-precipitation method.more » The phase conversion of ZnS to highly crystalline hexagonal ZnO was done by heat treatment. From the analysis of influence of calcination temperature on the structural, optical and vibrational properties of the samples, an optimum temperature was found for the total conversion of ZnS nanoparticles to ZnO. Role of quantum confinement due to finite size is evident from the blue shift of the fundamental absorption in UV–vis spectra only in the ZnS nanoparticles. The semiconducting nature of the prepared samples is confirmed from the UV–vis, PL study and transport study. From the magnetic and transport studies, pure ZnO phase was found to be more prone to magnetic field.« less
NASA Astrophysics Data System (ADS)
Kumar, Amit; Meenakshi, Mahto, Rabindra Nath
2018-04-01
We have investigated magnetization properties of the sol-gel prepared SrCo0.95Mn0.05O3 (SCMO) sample with respect to change in structural symmetry. The X-ray diffraction patterns show the crystal structure changes from nH-hexagonal, showing trigonal symmetry (SCMO1), to 2H-hexagonal phase (SCMO2). The trigonal crystal symmetry was obtained at lower annealing temperature (less than 1100 °C), however, the 2H-hexagonal symmetry was obtained at higher annealing temperature. The crystallite size calculated using Debye Scherer formula is found to be ˜ 46 nm and ˜ 33 nm for SCMO1 and SCMO2 samples respectively. The temperature dependence zero field cooled (MZFC) and field cooled (MFC) magnetization curves measured under the applied magnetic field of 500 Oe show magnetic reversibility for the SCMO1 sample. However, MZFC and MFC curves in hexagonal phase show magnetic irreversibility with onset temperature, Tirr ˜ 150 K, exhibits weak ferromagnetic ordering. The temperature variation of magnetization in paramagnetic region was analyzed by following Curie-Weiss law fitting. The χ-1(T) curve shows complete linear behavior with single slope for SCMO1 sample, whereas, the SCMO2 curve exhibit the linear behavior with two distinct slopes. Interestingly the sample in hexagonal phase shows small hysteresis loop at 2 K and 100 K respectively.
NASA Astrophysics Data System (ADS)
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.
3D printed glass: surface finish and bulk properties as a function of the printing process
NASA Astrophysics Data System (ADS)
Klein, Susanne; Avery, Michael P.; Richardson, Robert; Bartlett, Paul; Frei, Regina; Simske, Steven
2015-03-01
It is impossible to print glass directly from a melt, layer by layer. Glass is not only very sensitive to temperature gradients between different layers but also to the cooling process. To achieve a glass state the melt, has to be cooled rapidly to avoid crystallization of the material and then annealed to remove cooling induced stress. In 3D-printing of glass the objects are shaped at room temperature and then fired. The material properties of the final objects are crucially dependent on the frit size of the glass powder used during shaping, the chemical formula of the binder and the firing procedure. For frit sizes below 250 μm, we seem to find a constant volume of pores of less than 5%. Decreasing frit size leads to an increase in the number of pores which then leads to an increase of opacity. The two different binders, 2- hydroxyethyl cellulose and carboxymethylcellulose sodium salt, generate very different porosities. The porosity of samples with 2-hydroxyethyl cellulose is similar to frit-only samples, whereas carboxymethylcellulose sodium salt creates a glass foam. The surface finish is determined by the material the glass comes into contact with during firing.
NASA Astrophysics Data System (ADS)
Papantonakis, Michael R.; Nguyen, Viet K.; Furstenberg, Robert; White, Caitlyn; Shuey, Melissa; Kendziora, Christopher A.; McGill, R. Andrew
2017-05-01
Knowledge of the persistence of trace explosives materials is critical to aid the security community in designing detection methods and equipment. The physical and environmental factors affecting the lifetimes of particles include temperature, airflow, interparticle distance, adlayers, humidity, particle field size and vapor pressure. We are working towards a complete particle persistence model that captures the relative importance of these effects to allow the user, with known environmental conditions, to predict particle lifetimes for explosives or other chemicals. In this work, particles of explosives are sieved onto smooth glass substrates using particle sizes and loadings relevant to those deposited by fingerprint deposition. The coupon is introduced into a custom flow cell and monitored under controlled airflow, humidity and temperature. Photomicroscopy images of the sample taken at fixed time intervals are analyzed to monitor particle sublimation and characterized as a size-independent radial sublimation velocity for each particle in the ensemble. In this paper we build on previous work by comparing the relationship between sublimation of different materials and their vapor pressures. We also describe the influence of a sebum adlayer on particle sublimation, allowing us to better model `real world' samples.
Paula Menéndez, Lumila
2018-02-01
The aim of this study is to analyze the association between cranial variation and climate in order to discuss their role during the diversification of southern South American populations. Therefore, the specific objectives are: (1) to explore the spatial pattern of cranial variation with regard to the climatic diversity of the region, and (2) to evaluate the differential impact that the climatic factors may have had on the shape and size of the diverse cranial structures studied. The variation in shape and size of 361 crania was studied, registering 62 3D landmarks that capture shape and size variation in the face, cranial vault, and base. Mean, minimum, and maximum annual temperature, as well as mean annual precipitation, but also diet and altitude, were matched for each population sample. A PCA, as well as spatial statistical techniques, including kriging, regression, and multimodel inference were employed. The facial skeleton size presents a latitudinal pattern which is partially associated with temperature diversity. Both diet and altitude are the variables that mainly explain the skull shape variation, although mean annual temperature also plays a role. The association between climate factors and cranial variation is low to moderate, mean annual temperature explains almost 40% of the entire skull, facial skeleton and cranial vault shape variation, while annual precipitation and minimum annual temperature only contribute to the morphological variation when considered together with maximum annual temperature. The cranial base is the structure less associated with climate diversity. These results suggest that climate factors may have had a partial impact on the facial and vault shape, and therefore contributed moderately to the diversification of southern South American populations, while diet and altitude might have had a stronger impact. Therefore, cranial variation at the southern cone has been shaped both by random and nonrandom factors. Particularly, the influence of climate on skull shape has probably been the result of directional selection. This study supports that, although cranial vault is the cranial structure more associated to mean annual temperature, the impact of climate signature on morphology decreases when populations from extreme cold environments are excluded from the analysis. Additionally, it shows that the extent of the geographical scales analyzed, as well as differential sampling may lead to different results regarding the role of ecological factors and evolutionary processes on cranial morphology. © 2017 Wiley Periodicals, Inc.
NASA Astrophysics Data System (ADS)
Jux, Maximilian; Finke, Benedikt; Mahrholz, Thorsten; Sinapius, Michael; Kwade, Arno; Schilde, Carsten
2017-04-01
Several epoxy Al(OH)O (boehmite) dispersions in an epoxy resin are produced in a kneader to study the mechanistic correlation between the nanoparticle size and mechanical properties of the prepared nanocomposites. The agglomerate size is set by a targeted variation in solid content and temperature during dispersion, resulting in a different level of stress intensity and thus a different final agglomerate size during the process. The suspension viscosity was used for the estimation of stress energy in laminar shear flow. Agglomerate size measurements are executed via dynamic light scattering to ensure the quality of the produced dispersions. Furthermore, various nanocomposite samples are prepared for three-point bending, tension, and fracture toughness tests. The screening of the size effect is executed with at least seven samples per agglomerate size and test method. The variation of solid content is found to be a reliable method to adjust the agglomerate size between 138-354 nm during dispersion. The size effect on the Young's modulus and the critical stress intensity is only marginal. Nevertheless, there is a statistically relevant trend showing a linear increase with a decrease in agglomerate size. In contrast, the size effect is more dominant to the sample's strain and stress at failure. Unlike microscaled agglomerates or particles, which lead to embrittlement of the composite material, nanoscaled agglomerates or particles cause the composite elongation to be nearly of the same level as the base material. The observed effect is valid for agglomerate sizes between 138-354 nm and a particle mass fraction of 10 wt%.
Dielectric properties of Ti4+ substituted BaFe12O19 nanoparticles
NASA Astrophysics Data System (ADS)
Ghoneim, A. I.; Amer, M. A.; Meaz, T. M.; Attalah, S. S.
2017-02-01
Series of nanocrystalline BaTixFe12-(4/3)xO19 hexagonal ferrites, 0≤x≤1, was prepared using the chemical co-precipitation method. As-prepared samples were heated at 1200 °C for 20 h and slowly cooled to room temperature (RT). XRD studies proved that the samples have single phase M-type hexagonal nanostructure, where their grain size lies in the range of 42.4 - 61.3 nm. Their dielectric properties were studied against temperature (T) and frequency (F). DC conductivity showed increase against T, whereas AC conductivity showed increase with increasing both T and F. This proved the semiconducting behavior of the samples. Activation energies were found to lie in the range of 0.054-0.169 eV for temperature range of RT 373 K and of 0.114-0.274 eV for higher temperatures up to 473 K. Variation of the dielectric constant and AC conductivity against F revealed dispersion in all these hexagonal nanostructures, which was assigned to Maxwell-Wagner type of interfacial polarization. Variation of the dielectric loss tangent against F showed a relaxation spectrum for all samples, whereas the dielectric constant and loss tangent showed an increasing trend against T. The relative magnetic permeability μr showed an increasing trend with temperature.
Al2O3/ZrO2/Y3Al5O12 Composites: A High-Temperature Mechanical Characterization
Palmero, Paola; Pulci, Giovanni; Marra, Francesco; Valente, Teodoro; Montanaro, Laura
2015-01-01
An Al2O3/5 vol%·ZrO2/5 vol%·Y3Al5O12 (YAG) tri-phase composite was manufactured by surface modification of an alumina powder with inorganic precursors of the second phases. The bulk materials were produced by die-pressing and pressureless sintering at 1500 °C, obtaining fully dense, homogenous samples, with ultra-fine ZrO2 and YAG grains dispersed in a sub-micronic alumina matrix. The high temperature mechanical properties were investigated by four-point bending tests up to 1500 °C, and the grain size stability was assessed by observing the microstructural evolution of the samples heat treated up to 1700 °C. Dynamic indentation measures were performed on as-sintered and heat-treated Al2O3/ZrO2/YAG samples in order to evaluate the micro-hardness and elastic modulus as a function of re-heating temperature. The high temperature bending tests highlighted a transition from brittle to plastic behavior comprised between 1350 and 1400 °C and a considerable flexural strength reduction at temperatures higher than 1400 °C; moreover, the microstructural investigations carried out on the re-heated samples showed a very limited grain growth up to 1650 °C. PMID:28787961
Beam Heating of Samples: Modeling and Verification. Part 2
NASA Technical Reports Server (NTRS)
Kazmierczak, Michael; Gopalakrishnan, Pradeep; Kumar, Raghav; Banerjee Rupak; Snell, Edward; Bellamy, Henry; Rosenbaum, Gerd; vanderWoerd, Mark
2006-01-01
Energy absorbed from the X-ray beam by the sample requires cooling by forced convection (i.e. cryostream) to minimize temperature increase and the damage caused to the sample by the X-ray heating. In this presentation we will first review the current theoretical models and recent studies in the literature, which predict the sample temperature rise for a given set of beam parameters. It should be noted that a common weakness of these previous studies is that none of them provide actual experimental confirmation. This situation is now remedied in our investigation where the problem of x-ray sample heating is taken up once more. We have theoretically investigated, and at the same time, in addition to the numerical computations, performed experiments to validate the predictions. We have modeled, analyzed and experimentally tested the temperature rise of a 1 mm diameter glass sphere (sample surrogate) exposed to an intense synchrotron X-ray beam, while it is being cooled in a uniform flow of nitrogen gas. The heat transfer, including external convection and internal heat conduction was theoretically modeled using CFD to predict the temperature variation in the sphere during cooling and while it was subjected to an undulator (ID sector 19) X-ray beam at the APS. The surface temperature of the sphere during the X-ray beam heating was measured using the infrared camera measurement technique described in a previous talk. The temperatures from the numerical predictions and experimental measurements are compared and discussed. Additional results are reported for the two different sphere sizes and for two different supporting pin orientations.
NASA Astrophysics Data System (ADS)
Hassen, Harzali; Adel, Megriche; Arbi, Mgaidi
2018-03-01
Ultrasound-assisted co-precipitation has been used to prepare nano-sized Ni0.4Cu0.2Zn0.4Fe2O4 ferrite. Continuous (C-US) and pulsed (P-US) ultrasound modes are used at constant frequency = 20 kHz, reaction time = 2 h and pulse durations of 10 s on and 10 s off. All experiments were conducted at two temperatures 90 and 100°C. Samples were characterized by X-ray diffraction (XRD), Fourier transform spectroscopy (FT-IR), N2 adsorption isotherms at 77 k analysis (BET), transmission electron microscopy (TEM) and vibrating sample magnetometry (VSM) techniques. A nanocrystalline single-phase with particle size in the range 12-18 nm is obtained in both modes: continuous and pulsed ultrasound mode. FT-IR measurements show two absorption bands assigned to the tetrahedral and octahedral vibrations (ν1 and ν2) characteristics of cubic spinel ferrite. The specific surface area (S BET) is in the range of 110-140 m2 g-1 and an average pore size between 5.5 and 6.5 nm. The lowest values are obtained in pulsed mode. Finally, this work shows that the magnetic properties are affected by the ultrasound conditions, without affecting the particle shape. The saturation magnetization (Ms) values obtained for all samples are comparable. In P-US mode, the saturation magnetization (Ms) increases as temperature increases. Moreover, P-US mode opens a new avenue for synthesis of NiCuZn ferrites.
Infrared dynamics of cold atoms on hot graphene membranes
NASA Astrophysics Data System (ADS)
Sengupta, Sanghita; Kotov, Valeri N.; Clougherty, Dennis P.
2016-06-01
We study the infrared dynamics of low-energy atoms interacting with a sample of suspended graphene at finite temperature. The dynamics exhibits severe infrared divergences order by order in perturbation theory as a result of the singular nature of low-energy flexural phonon emission. Our model can be viewed as a two-channel generalization of the independent boson model with asymmetric atom-phonon coupling. This allows us to take advantage of the exact nonperturbative solution of the independent boson model in the stronger channel while treating the weaker one perturbatively. In the low-energy limit, the exact solution can be viewed as a resummation (exponentiation) of the most divergent diagrams in the perturbative expansion. As a result of this procedure, we obtain the atom's Green function which we use to calculate the atom damping rate, a quantity equal to the quantum sticking rate. A characteristic feature of our results is that the Green's function retains a weak, infrared cutoff dependence that reflects the reduced dimensionality of the problem. As a consequence, we predict a measurable dependence of the sticking rate on graphene sample size. We provide detailed predictions for the sticking rate of atomic hydrogen as a function of temperature and sample size. The resummation yields an enhanced sticking rate relative to the conventional Fermi golden rule result (equivalent to the one-loop atom self-energy), as higher-order processes increase damping at finite temperature.
The Effect of deposition rate on FePt/MgO crystal orientation
NASA Astrophysics Data System (ADS)
Sheikhi, M.; Sebt, S. A.; Khajehnezhad, A.
2018-06-01
FePt granular layers which are made in suitable conditions can have three types of ordering that are crystalline, compositional orders and directional configuration of nanoparticles. Formation of fct structure with L10 compositional ordering requires high temperature. At this temperature, a problem is the size control of the nanoparticles and another problem is control of their crystal orientation. Fabrication method and the use of suitable substrates can help solving these problems. In direct synthesis by sputtering method on the warm substrate the size of FePt nanoparticles in L10 compositional ordered phase can be controlled. We show that crystal orientation of L10-FePt nanoparticles on a thin layer of MgO depends on the rate of deposition. This becomes clear from the results of the XRD analyses of samples. Based on these results in synthesis at room temperature with deposition rate of upper than 1.5 Å/s after annealing, (001) peak is dominated and at rate of lower than 1.0 Å/s just (111) peak is appeared. In direct synthesis with intermediate rate (111) and (110) peaks can be seen. Moreover, the difference of the shape of hysteresis loops of samples in parallel and vertical directions are the witnesses for orientation of samples in presence of MgO layer and the effect of FePt deposition rate on it.
High-throughput screening for combinatorial thin-film library of thermoelectric materials.
Watanabe, Masaki; Kita, Takuji; Fukumura, Tomoteru; Ohtomo, Akira; Ueno, Kazunori; Kawasaki, Masashi
2008-01-01
A high-throughput method has been developed to evaluate the Seebeck coefficient and electrical resistivity of combinatorial thin-film libraries of thermoelectric materials from room temperature to 673 K. Thin-film samples several millimeters in size were deposited on an integrated Al2O3 substrate with embedded lead wires and local heaters for measurement of the thermopower under a controlled temperature gradient. An infrared camera was used for real-time observation of the temperature difference Delta T between two electrical contacts on the sample to obtain the Seebeck coefficient. The Seebeck coefficient and electrical resistivity of constantan thin films were shown to be almost identical to standard data for bulk constantan. High-throughput screening was demonstrated for a thermoelectric Mg-Si-Ge combinatorial library.
Effects of particle size and heating time on thiobarbituric acid (TBA) test of soybean powder.
Lee, Youn-Ju; Yoon, Won-Byong
2013-06-01
Effects of particle size and heating time during TBA test on the thiobarbituric acid reactive substance (TBARS) of soybean (Glycine Max) powder were studied. Effects of processing variables involved in the pulverization of soybean, such as the temperature of soybean powder, the oxygen level in the vessel, and the pulverisation time, were investigated. The temperature of the soybean powder and the oxygen level had no significant influence on the TBARS (p<0.05). The pulverization time and the heating time during TBA test significantly affected the TBARS. Change of TBARS during heating was well described by the fractional conversion first order kinetics model. A diffusion model was introduced to quantify the effect of particle size on TBARS. The major finding of this study was that the TBA test to estimate the level of the lipid oxidation directly from powders should consider the heating time and the mean particle sizes of the sample. Copyright © 2012 Elsevier Ltd. All rights reserved.
The Effects of Atmosphere on the Sintering of Ultrafine-Grained Tungsten with Ti
NASA Astrophysics Data System (ADS)
Ren, Chai; Koopman, Mark; Fang, Z. Zak; Zhang, Huan
2016-11-01
Tungsten (W) is a brittle material at room temperature making it very difficult to fabricate. Although the lack of ductility remains a difficult challenge, nano-sized and ultrafine-grained (UFG) structures offer the potential to overcome tungsten's room-temperature brittleness. One way to manufacture UFG W is to compact and sinter nano-sized W powder. It is challenging, however, to control grain growth during sintering. As one method to inhibit grain growth, the effect of Ti-based additives on the densification and grain growth of nano-W powders was investigated in this study. Addition of 1% Ti into tungsten led to more than a 63% decrease in average grain size of sintered samples at comparable density levels. It was found that sintering in Ar yielded a finer grain size than sintering in H2 at similar densities. The active diffusion mechanisms during sintering were different for W-1% Ti nano powders sintered in Ar and H2.
Influence of Sintering Temperature on Hardness and Wear Properties of TiN Nano Reinforced SAF 2205
NASA Astrophysics Data System (ADS)
Oke, S. R.; Ige, O. O.; E Falodun, O.; Obadele, B. A.; Mphalele, M. R.; Olubambi, P. A.
2017-12-01
Conventional duplex stainless steel degrade in wear and mechanical properties at high temperature. Attempts have been made by researchers to solve this problems leading to the dispersion of second phase particles into duplex matrix. Powder metallurgy methods have been used to fabricate dispersion strengthened steels with a challenge of obtaining fully dense composite and grain growth. This could be resolved by appropriate selection of sintering parameters especially temperature. In this research, spark plasma sintering was utilized to fabricate nanostructured duplex stainless steel grade SAF 2205 with 5 wt.% nano TiN addition at different temperatures ranging from 1000 °C to 1200 °C. The effect of sintering temperature on the microstructure, density, hardness and wear of the samples was investigated. The results showed that the densities and grain sizes of the sintered nanocomposites increased with increasing the sintering temperature. The microstructures reveal ferrite and austenite grains with fine precipitates within the ferrite grains. The study of the hardness and wear behaviors, of the samples indicated that the optimum properties were obtained for the sintering temperature of 1150 °C.
2008-01-01
oriented grain-boundaries. In this work we show considerable evidence for such weak-coupling by study of the dependence of magnetization in bulk and...powdered samples. Bulk sample magnetization curves show very little hysteresis while remanent magnetization shows almost no sample size dependence...K Fig. 2 (Color online) Magnetization hysteresis loops at 5 and 20 K for the bulk LaO0.89F0.11FeAs. Inset shows the temperature dependence of
NASA Astrophysics Data System (ADS)
Zhang, X.; Roman, M.; Kimmel, D.; McGilliard, C.; Boicourt, W.
2006-05-01
High-resolution, axial sampling surveys were conducted in Chesapeake Bay during April, July, and October from 1996 to 2000 using a towed sampling device equipped with sensors for depth, temperature, conductivity, oxygen, fluorescence, and an optical plankton counter (OPC). The results suggest that the axial distribution and variability of hydrographic and biological parameters in Chesapeake Bay were primarily influenced by the source and magnitude of freshwater input. Bay-wide spatial trends in the water column-averaged values of salinity were linear functions of distance from the main source of freshwater, the Susquehanna River, at the head of the bay. However, spatial trends in the water column-averaged values of temperature, dissolved oxygen, chlorophyll-a and zooplankton biomass were nonlinear along the axis of the bay. Autocorrelation analysis and the residuals of linear and quadratic regressions between each variable and latitude were used to quantify the patch sizes for each axial transect. The patch sizes of each variable depended on whether the data were detrended, and the detrending techniques applied. However, the patch size of each variable was generally larger using the original data compared to the detrended data. The patch sizes of salinity were larger than those for dissolved oxygen, chlorophyll-a and zooplankton biomass, suggesting that more localized processes influence the production and consumption of plankton. This high-resolution quantification of the zooplankton spatial variability and patch size can be used for more realistic assessments of the zooplankton forage base for larval fish species.
Joshi, C; Dwivedi, A; Rai, S B
2014-08-14
Infrared-to-visible upconverting rare earths Er(3+)/Yb(3+) co-doped Y2O3 nano-crystalline phosphor samples have been prepared by solution combustion method followed by post-heat treatment at higher temperatures. A slight increase in average crystallite size has been found on calcinations verified by X-ray analysis. Transmission electron microscopy (TEM) confirms the nano-crystalline nature of the as-prepared and calcinated samples. Fourier transform infrared (FTIR) analysis shows the structural changes in as-prepared and calcinated samples. Upconversion and downconversion emission recorded using 976 and 532 nm laser sources clearly demonstrates a better luminescence properties in the calcinated samples as compared to as-prepared sample. Upconversion emission has been quantified in terms of standard chromaticity diagram (CIE) showing a shift in overall upconversion emission of as-prepared and calcinated samples. Temperature sensing behaviour of this material has also been investigated by measurement of fluorescence intensity ratio (FIR) of various signals in green emission in the temperature range of 315 to 555 K under 976 nm laser excitation. Copyright © 2014 Elsevier B.V. All rights reserved.
NASA Astrophysics Data System (ADS)
El-Danaf, Ehab A.; Baig, Muneer; Almajid, Abdulhakim A.; Soliman, Mahmoud S.
2014-08-01
Mechanical Attrition of metallic powders induces severe plastic deformation and consequently reduces the average grain size. Powders of 99.7 Al (45μm particle size), cryomilled for 7 hrs having a crystal size of ~ 20 nm, were consolidated by high frequency induction sintering under a constant pressure of 50 MPa and at two temperatures of 500 and 550 °C for two sintering dwell times of 1 and 3 minutes at a constant heating rate of 400 °C/min. The bright field TEM image and X-ray line broadening technique, for the cryomilled powders, were used to measure-the crystallite size. Simple compression at an initial strain rate of 10-4 s-1 was conducted at room temperature, 373 and 473 K, and the yield strength was documented and correlated with the sintering parameters. The as-received 99.7 Al powders-consolidated using one of the sintering parameters was used as a reference material to compare the mechanical properties. Hardness, density and crystal size of the consolidated sample, that gave the highest yield and fracture strength, were measured.
NASA Astrophysics Data System (ADS)
Murkute, Punam; Ghadi, Hemant; Saha, Shantanu; Chavan, Vinayak; Chakrabarti, Subhananda
2018-03-01
High band gap (3.34 eV) and large exciton binding energy (60 meV) at room temperature facilitates ZnO as a useful candidate for optoelectronics devices. Presence of zinc interstitial and oxygen vacancies results in n-type ZnO film. Phosphorus implantation was carried out using plasma immersion ion implantation technique (2kV, 900W) for constant duration (50 s) on RF sputtered ZnO thin films (Sample A). For dopant activation, sample A was subjected to Rapid Thermal Annealing (RTA) at 700, 800, 900 and 1000°C for 10 s in Oxygen ambient (Sample B, C, D, E). Low temperature (18 K) photoluminescence measurement demonstrated strong donor bound exciton peak for sample A. Dominant donor to acceptor pair peak (DAP) was observed for sample D at around 3.22 eV with linewidth of 131.3 meV. High resolution x-ray diffraction measurement demonstrated (001) and (002) peaks for sample A. (002) peak with high intensity was observed from all annealed samples. Incorporation of phosphorus in ZnO films leads to peak shift towards higher 2θ angle indicate tensile strain in implanted samples. Scanning electron microscopy images reveals improvement in grain size distribution along with reduction of implantation related defects. Raman spectra measured A1(LO) peak at around 576 cm-1 for sample A. Low intensity E2 (high) peak was observed for sample D indicating formation of (PZn+2VZn) complexes. From room temperature Hall measurement, sample D measured 1.17 x 1018 cm -3 carrier concentration with low resistivity of 0.464 Ω.
NASA Astrophysics Data System (ADS)
Taffin, C.; Grasset, O.; Le Menn, E.; Le Mouélic, S.
2009-12-01
Near IR signatures of water ices are known to depend on temperature and grain size, a property that could be used to constrain the surface characteristics of icy moons1,2,3. Models indicate that the 1.65 µm absorption band depends strongly on temperature2,4,5 and on grain size. Other bands (1.03, 1.27, 1.50 and 2 µm) show a strong dependence with grain size (e.g. (6) for the 1.03 µm band). But the respective influence of temperature and grain size is still not fully understood. In this work, we focus on the 1.50 and 1.55 µm absorption bands. Characteristics of near-IR spectra of pure ice Ih grains have been experimentally investigated using temperature and pressure ranges relevant for icy moons. Nineteen experiments have been conducted both at microscopic (individual grains smaller than 100 mm) and macroscopic (grains ranging from 200 to 800 µm) scales, using a FTIR spectrometer. Position, area and depth of the four main absorption bands in the near-IR domain (1.50, 1.55, 1.65 and 2 µm) have been studied . It will be shown that the positions of the 1.50 µm and the 1.55 µm bands are very good indicators of grain size and of temperature, respectively (Fig.1). The scaling laws established from experimental data can be used to characterize the surface properties of icy moons. Preliminary tests are conducted on extensively studied regions to validate the approach. An application to the Tiger Stripes on Enceladus will be presented. The estimated temperatures are at first order consistent with those obtained by CIRS7, but they still appear slightly higher in average (between 10 and 20 K). Grain size are also bigger than in a previous model8 but the same tendency is observed, i.e., the grain size is larger on the Tiger Stripes than in the surroundings. Ref. : 1-Fink and Larson, Icarus, 1975. 2-Leto et al. Mem. S.A.It. Suppl. 2005. 3-Grundy, Icarus, 1999. 4-Grundy and Schmitt, JGR. 1998. 5-Mastrapa et al. Icarus, 2008. 6-Nolin and Dozier Rem. Sens. Environ. 2000. 7-Abramov and Spencer, Icarus 2009. 8-Jaumann et al. Icarus, 2007. Figure 1: a) Position of the 1.55 µm band versus temperature for ice (black) and frost (red). For each temperature a dispersion of 10 - 20 cm-1 is observed due to the grain size variations from 200 to 800 µm. b) Position of the 1.50 µm band relative to the grain size at microscopic (black) and macroscopic (red) scales. The grain size of macroscopic samples is estimated using the Nolin and Dozier’s method (6).
[Preparation of titanium dioxide particles and properties for flue gas desulfurization].
Luo, Yonggang; Li, Daji; Huang, Zhen
2003-01-01
Under different sintering temperatures(340 degrees C, 440 degrees C, 540 degrees C, 640 degrees C), four TiO2 particles were prepared. The crystal types of all four samples were found to possess anatase structures by XRD. It was obtained by N2 experimental adsorption at low temperature (77K) that their surface areas and average pore size were between 79 and 124 m2/g, 56.8 and 254.8 A respectively. The pore structure of TiO2 particles was characterized by scanning electron microscope (SEM). The tests of adsorption dynamics for FGD and the performance of SO2 removal were investigated in a fixed-bed system for different samples. The results show that SG540 sample which made at 540 degrees C sintering temperature had the most quality among the four samples. It can adsorb SO2 of 38.9 mg for one gram SG540 sample. Different operating conditions for SG540 such as adsorption temperature, SO2 concentration in flue gas and the superficial velocity of flue gas were investigated. TiO2 particles for FGD had more efficiency than other physical sorbents such as active carbon and zeolite. The mechanism for SO2 removal was demonstrated by infrared (IR) spectroscopy and desorption test results to be mainly physical adsorption.
Becker, Jacob; Hald, Peter; Bremholm, Martin; Pedersen, Jan S; Chevallier, Jacques; Iversen, Steen B; Iversen, Bo B
2008-05-01
Nanocrystalline ZrO(2) samples with narrow size distributions and mean particle sizes below 10 nm have been synthesized in a continuous flow reactor in near and supercritical water as well as supercritical isopropyl alcohol using a wide range of temperatures, pressures, concentrations and precursors. The samples were comprehensively characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), and small-angle X-ray scattering (SAXS), and the influence of the synthesis parameters on the particle size, particle size distribution, shape, aggregation and crystallinity was studied. On the basis of the choice of synthesis parameters either monoclinic or tetragonal zirconia phases can be obtained. The results suggest a critical particle size of 5-6 nm for nanocrystalline monoclinic ZrO(2) under the present conditions, which is smaller than estimates reported in the literature. Thus, very small monoclinic ZrO(2) particles can be obtained using a continuous flow reactor. This is an important result with respect to improvement of the catalytic properties of nanocrystalline ZrO(2).
NASA Astrophysics Data System (ADS)
Xu, Weitai; Zhao, Yutao; Sun, Shaochun; Liu, Manping; Ma, Dexin; Liang, Xiangfeng; Wang, Cunlong; Tao, Ran
2018-04-01
The mold shell used for single-crystal turbine blades preparation was modified from conventional process to fiber reinforcement technology. The wall thickness was decreased by 32.3 percent (pct) than the conventional process. Then these two mold shells were used to produce single crystal samples of nickel-base superalloy in a Bridgman furnace. The local temperature curves were recorded in the process. The results show that the modified mold shell can increase the temperature gradient in the mushy zone than the conventional mold shell. The primary and secondary dendrite arm space were reduced by 8 pct and 12 pct, respectively. Moreover, both the area fraction and mean size of the γ‧/γ eutectic were declined, as well as the dendritic segregation tendency. Therefore it contributed to the lower residual eutectic and micro-porosity in the heat-treated microstructure. Further, fracture surface of the samples made by modified mold shell exhibited smaller facets and more uniform dimples in the size and shape.
Experimental evidence for stochastic switching of supercooled phases in NdNiO3 nanostructures
NASA Astrophysics Data System (ADS)
Kumar, Devendra; Rajeev, K. P.; Alonso, J. A.
2018-03-01
A first-order phase transition is a dynamic phenomenon. In a multi-domain system, the presence of multiple domains of coexisting phases averages out the dynamical effects, making it nearly impossible to predict the exact nature of phase transition dynamics. Here, we report the metal-insulator transition in samples of sub-micrometer size NdNiO3 where the effect of averaging is minimized by restricting the number of domains under study. We observe the presence of supercooled metallic phases with supercooling of 40 K or more. The transformation from the supercooled metallic to the insulating state is a stochastic process that happens at different temperatures and times in different experimental runs. The experimental results are understood without incorporating material specific properties, suggesting that the behavior is of universal nature. The size of the sample needed to observe individual switching of supercooled domains, the degree of supercooling, and the time-temperature window of switching are expected to depend on the parameters such as quenched disorder, strain, and magnetic field.
Kinetic studies on the reduction of iron ore nuggets by devolatilization of lean-grade coal
NASA Astrophysics Data System (ADS)
Biswas, Chanchal; Gupta, Prithviraj; De, Arnab; Chaudhuri, Mahua Ghosh; Dey, Rajib
2016-12-01
An isothermal kinetic study of a novel technique for reducing agglomerated iron ore by volatiles released by pyrolysis of lean-grade non-coking coal was carried out at temperature from 1050 to 1200°C for 10-120 min. The reduced samples were characterized by scanning electron microscopy, energy-dispersive X-ray spectroscopy, and chemical analysis. A good degree of metallization and reduction was achieved. Gas diffusion through the solid was identified as the reaction-rate-controlling resistance; however, during the initial period, particularly at lower temperatures, resistance to interfacial chemical reaction was also significant, though not dominant. The apparent rate constant was observed to increase marginally with decreasing size of the particles constituting the nuggets. The apparent activation energy of reduction was estimated to be in the range from 49.640 to 51.220 kJ/mol and was not observed to be affected by the particle size. The sulfur and carbon contents in the reduced samples were also determined.
NASA Astrophysics Data System (ADS)
Chandekar, Kamlesh V.; Kant, K. Mohan
2017-09-01
Superparamagnetic cobalt ferrite (CoFe2O4) spherical nanoparticles and rhomboidal nanoplatelets were synthesized by co-precipitation at 80 °C (S1) and hydrothermal route at 150 °C (S2). X-ray diffraction (XRD) pattern confirms formation of cubic inverse spinel structure of as prepared cobalt ferrite samples (S1 and S2) with average crystallite size of 13 nm and 18.7 nm for S1 and S2 respectively. Transmission electron microscopy (TEM) reveals spherical and rhomboidal shaped with average particle size 16.7 nm (S1) and 19.8 nm (S2). The zero field cooled magnetization MZFCvs. T exhibit a broad maxima at 400 K and 510 K for S1 and S2 respectively. The blocking temperature TB is obtained as 310 K and 341 K for S1 and S2 respectively, by fitting coercive field at different temperatures to T 1 / 2 law. The morphology of S1 and S2 corresponds to shape dependence of continuum approach. The effective demagnetization factors estimated as ΔN1 = 0 and ΔN2 = 0 . 749 for S1 and S2 samples respectively. The uniaxial anisotropy and shape anisotropy observed to be dominant in spherical shaped and rhomboidal shaped CoFe2O4 nanoparticles respectively. The uniaxial anisotropy constant of S1 sample is estimated as 56 (kJ/m3) at TB = 310 K whereas the effective anisotropy constant for S2 sample is 627 (kJ/m3) at TB = 341 K , in which shape anisotropy constant 605 (kJ/m3) dominates over contribution from uniaxial anisotropy constant 22 (kJ/m3) in S2 sample.
NASA Astrophysics Data System (ADS)
Drazin, John Walter
Calcia-, and yttria- doped zirconia powders and samples are essential systems in academia and industry due to their observed bulk polymorphism. Pure zirconia manifests as Baddeleyite, a monoclinic structured mineral with 7-fold coordination. This bulk form of zirconia has little application due to its asymmetry. Therefore dopants are added to the grain in-order to induce phase transitions to either a tetragonal or cubic polymorph with the incorporation of oxygen vacancies due to the dopant charge mis-match with the zirconia matrix. The cubic polymorph has cubic symmetry such that these samples see applications in solid oxide fuel cells (SOFCs) due to the high oxygen vacancy concentrations and high ionic mobility at elevated temperatures. The tetragonal polymorph has slight asymmetry in the c-axis compared to the a-axis such that the tetragonal samples have increased fracture toughness due to an impact induced phase transformation to a cubic structure. These ceramic systems have been extensively studied in academia and used in various industries, but with the advent of nanotechnology one can wonder whether smaller grain samples will see improved characteristics similar to their bulk grain counterparts. However, there is a lack of data and knowledge of these systems in the nano grained region which provides us with an opportunity to advance the theory in these systems. The polymorphism seen in the bulk grains samples is also seen in the nano-grained samples, but at slightly distinct dopant concentrations. The current theory hypothesizes that a surface excess, gamma (J/m 2), can be added to the Gibbs Free energy equation to account for the additional free energy of the nano-grain atoms. However, these surface energies have been difficult to measure and therefore thermodynamic data on these nano-grained samples have been sparse. Therefore, in this work, I will use a well established water adsorption microcalorimetry apparatus to measure the water coverage isotherms while simultaneously collecting the energetic contribution of the adsorbing water vapor. With this data and apparatus, I have derived a 2nd order differential equation that relates the surface energy to the measured quantities such that I collected surfaces energies for over 35 specimens in the calcia-zirconia and yttria-zirconia systems for the first time. From the results, it was found that the monoclinic polymorph had the largest surface energy in the range of 1.9 - 2.1 ( J/m2) while the tetragonal surface energies were roughly 1.4 - 1.6 (J/m2), the cubic surface energies were roughly 0.8 - 1.0 (J/m2), and the amorphous surface energies were the smallest at roughly 0.7 - 0.8 (J/m 2). With the measured surface energy data, collected for the first time, we can create a nano-grain phase diagram similar to a bulk phase diagram that shows the stable polymorph as a function of dopant concentration and grain size using the bulk enthalpy data collected from high temperature oxide melt drop solution calorimetry. The phase diagrams show that pure zirconia will transform into tetragonal and cubic polymorphs from the monoclinic one at 7 and 5 nm respectively which confirms the experimental observations. The results are powerful predictive tools successfully applied in the nCZ and nYZ systems to a high degree of accuracy and adds a new development to conventional bulk phase diagrams. These diagrams should be the basis for nanotechnological efforts in nCZ and nYZ based systems, and suggest similar efforts are needed in other nano systems to pursue an in depth understanding and optimization of nanomaterials. After working on the theoretical aspects of phase stability, the focus of the research will shift to producing dense samples to measure observable quantities such as oxygen conduction and mechanical hardness. However, producing said samples with the nanocrystalline grain sizes has also been challenging as conventional sintering requires high temperatures which, as a consequence, induces grain growth of the samples limiting the minimum grain size of the samples. Therefore, in this work, we have developed a Pressure Assisted Rapid Sintering Technique (PARS) that uses high currents to Joule heat the samples to moderate temperatures (650-900 °C) for short durations (5-10 min) under large compressive pressures (600-2200 MPa). With this new technique, atomic level grain sizes (sub-10nm) can be easily achieved at high relative densities (>98 %). Using the PARS setup, multiple 3nYZ samples were produced with varied grain sizes down to 9 nm and as large as 5mum. The mechanical hardness of these samples were tested using a Vicker's microhardness indentation apparatus. The hardness of the "bulk" grains was roughly 12.9 GPa while the smallest grain size pellet had a hardness approaching 15 GPa. All of the 3nYZ pellets had a higher hardness with diminishing grain size, thereby extending the Hall-Petch relationship to 9 nm in the 3YZ system. This is an amazing and unprecedented result to date. After producing the extreme nano-grained samples (15nCZ and 17.5nYSZ), they were tested for inter- and intragranular oxygen ion conduction as well. The results showed that the smaller grained samples have increased levels of oxygen ion conduction from both inter- and intragranular diffusion regardless of the operating temperatures. In addition, it was seen that the activation energies for both modes of oxygen ion diffusion were lowered for the nCZ system while a plateaued effect was seen in the nYZ system. A new theoretical formulation was proposed to explain the trends such that there are two modifiable parameters to exploit; activation energy and grain size. With the lowering of the grain size, the number of interconnected grain boundaries would increase dramatically allowing for more efficient travel around and through the grains. The activation energy can be lowered by modifying the chemistry of the grain boundary by specifically choosing larger dopants with a positive enthalpy of segregation such the concentration of the dopants on the grain boundary would increase, spacing the unattached bonds further apart and reducing their number. Therefore, one can use an engineered nanograined SOFC to decrease the operating temperature of the device without altering the output power density; significantly improving safety and economics.
Diao, Junshu; Chen, Zhao; Gong, Chao; Jiang, Xiuping
2015-09-01
This study investigated the survival of Escherichia coli O157:H7 and Salmonella Typhimurium in finished dairy compost with different particle sizes during storage as affected by moisture content and temperature under greenhouse conditions. The mixture of E. coli O157:H7 and S. Typhimurium strains was inoculated into the finished composts with moisture contents of 20, 30, and 40%, separately. The finished compost samples were then sieved into 3 different particle sizes (>1000, 500-1000, and <500 μm) and stored under greenhouse conditions. For compost samples with moisture contents of 20 and 30%, the average Salmonella reductions in compost samples with particle sizes of >1000, 500-1000, and <500 μm were 2.15, 2.27, and 2.47 log colony-forming units (CFU) g(-1) within 5 days of storage in summer, respectively, as compared with 1.60, 2.03, and 2.26 log CFU g(-1) in late fall, respectively, and 2.61, 3.33, and 3.67 log CFU g(-1) in winter, respectively. The average E. coli O157:H7 reductions in compost samples with particle sizes of >1000, 500-1000, and <500 μm were 1.98, 2.30, and 2.54 log CFU g(-1) within 5 days of storage in summer, respectively, as compared with 1.70, 2.56, and 2.90 log CFU g(-1) in winter, respectively. Our results revealed that both Salmonella and E. coli O157:H7 in compost samples with larger particle size survived better than those with smaller particle sizes, and the initial rapid moisture loss in compost may contribute to the fast inactivation of pathogens in the finished compost. For the same season, the pathogens in the compost samples with the same particle size survived much better at the initial moisture content of 20% compared to 40%.
Effect of Pt Nanoparticles on the Optical Gas Sensing Properties of WO3 Thin Films
Qadri, Muhammad U.; Diaz Diaz, Alex Fabian; Cittadini, Michaela; Martucci, Alessandro; Pujol, Maria Cinta; Ferré-Borrull, Josep; Llobet, Eduard; Aguiló, Magdalena; Díaz, Francesc
2014-01-01
Thin films of tungsten trioxide were deposited on quartz substrates by RF magnetron sputtering. Different annealing temperatures in the range from 423 to 973 K were used under ambient atmosphere. The influence of the annealing temperature on the structure and optical properties of the resulting WO3 thin films were studied. The surface morphology of the films is composed of grains with an average size near 70 nm for the films annealed between 773 and 973 K. Some of the WO3 thin films were also coated with Pt nanoparticles of about 45 nm in size. Spectrometric measurements of transmittance were carried out for both types of WO3 samples in the wavelength range from 200–900 nm, to determine the effect of the exposure to two different gases namely H2 and CO. Films showed fast response and recovery times, in the range of few seconds. The addition of Pt nanoparticles enables reducing the operation temperature to room temperature. PMID:24977386
The Influence of Hot-Rolled Temperature on Plasma Nitriding Behavior of Iron-Based Alloys
NASA Astrophysics Data System (ADS)
El-Hossary, F. M.; Khalil, S. M.; Lotfy, Kh.; Kassem, M. A.
2009-07-01
Experiments were performed with an aim of studying the effect of hot-rolled temperature (600 and 900°C) on radio frequency (rf) plasma nitriding of Fe93Ni4Zr3 alloy. Nitriding was carried out for 10 min in a nitrogen atmosphere at a base pressure of 10-2 mbarr. Different continuous plasma processing powers of 300-550 W in steps 50 W or less were applied. Nitrided hot-rolled specimens were characterized by optical microscopy (OM), X-ray diffraction (XRD) and microhardness measurements. The results reveal that the surface of hot-rolled rf plasma nitrided specimens at 600°C is characterized with a fine microstructure as a result of the high nitrogen solubility and diffusivity. Moreover, the hot-rolled treated samples at 600°C exhibit higher microhardness value than the associated values of hot-rolled treated samples at 900°C. The enhancement of microhardness is due to precipitation and predominance of new phases ( γ and ɛ phases). Mainly, this conclusion has been attributed to the high defect densities and small grain sizes of the samples hot-rolled at 600°C. Generally, the refinement of grain size plays a dramatic role in improvement of mechanical properties of tested samples.
Cracks and nanodroplets produced on tungsten surface samples by dense plasma jets
NASA Astrophysics Data System (ADS)
Ticoş, C. M.; Galaţanu, M.; Galaţanu, A.; Luculescu, C.; Scurtu, A.; Udrea, N.; Ticoş, D.; Dumitru, M.
2018-03-01
Small samples of 12.5 mm in diameter made from pure tungsten were exposed to a dense plasma jet produced by a coaxial plasma gun operated at 2 kJ. The surface of the samples was analyzed using a scanning electron microscope (SEM) before and after applying consecutive plasma shots. Cracks and craters were produced in the surface due to surface tensions during plasma heating. Nanodroplets and micron size droplets could be observed on the samples surface. An energy-dispersive spectroscopy (EDS) analysis revealed that the composition of these droplets coincided with that of the gun electrode material. Four types of samples were prepared by spark plasma sintering from powders with the average particle size ranging from 70 nanometers up to 80 μm. The plasma power load to the sample surface was estimated to be ≈4.7 MJ m-2 s-1/2 per shot. The electron temperature and density in the plasma jet had peak values 17 eV and 1.6 × 1022 m-3, respectively.
The Response of Simple Polymer Structures Under Dynamic Loading
NASA Astrophysics Data System (ADS)
Proud, William; Ellison, Kay; Yapp, Su; Cole, Cloe; Galimberti, Stefano; Institute of Shock Physics Team
2017-06-01
The dynamic response of polymeric materials has been widely studied with the effects of degree of crystallinity, strain rate, temperature and sample size being commonly reported. This study uses a simple PMMA structure, a right cylindrical sample, with structural features such as holes. The features are added an varied in a systematic fashion. Samples were dynamically loaded using a Split Hopkinson Pressure Bar up to failure. The resulting stress-strain curves are presented showing the change in sample response. The strain to failure is shown to increase initially with the presence of holes, while failure stress is relatively unaffected. The fracture patterns seen in the failed samples change, with tensile cracks, Hertzian cones, shear effects being dominant for different holes sizes and geometries. The sample were prepared by laser cutting and checked for residual stress before experiment. The data is used to validate predictive model predictions where material, structure and damage are included.. The Institute of Shock Physics acknowledges the support of Imperial College London and the Atomic Weapons Establishment.
NASA Astrophysics Data System (ADS)
Ryan, A. J.; Christensen, P. R.
2016-12-01
Laboratory measurements have been necessary to interpret thermal data of planetary surfaces for decades. We present a novel radiometric laboratory method to determine temperature-dependent thermal conductivity of complex regolith simulants under high vacuum and across a wide range of temperatures. Here, we present our laboratory method, strategy, and initial results. This method relies on radiometric temperature measurements instead of contact measurements, eliminating the need to disturb the sample with thermal probes. We intend to determine the conductivity of grains that are up to 2 cm in diameter and to parameterize the effects of angularity, sorting, layering, composition, and cementation. These results will support the efforts of the OSIRIS-REx team in selecting a site on asteroid Bennu that is safe and meets grain size requirements for sampling. Our system consists of a cryostat vacuum chamber with an internal liquid nitrogen dewar. A granular sample is contained in a cylindrical cup that is 4 cm in diameter and 1 to 6 cm deep. The surface of the sample is exposed to vacuum and is surrounded by a black liquid nitrogen cold shroud. Once the system has equilibrated at 80 K, the base of the sample cup is rapidly heated to 450 K. An infrared camera observes the sample from above to monitor its temperature change over time. We have built a time-dependent finite element model of the experiment in COMSOL Multiphysics. Boundary temperature conditions and all known material properties (including surface emissivities) are included to replicate the experiment as closely as possible. The Optimization module in COMSOL is specifically designed for parameter estimation. Sample thermal conductivity is assumed to be a quadratic or cubic polynomial function of temperature. We thus use gradient-based optimization methods in COMSOL to vary the polynomial coefficients in an effort to reduce the least squares error between the measured and modeled sample surface temperature.
Buoyancy-corrected gravimetric analysis of lightly loaded filters.
Rasmussen, Pat E; Gardner, H David; Niu, Jianjun
2010-09-01
Numerous sources of uncertainty are associated with the gravimetric analysis of lightly loaded air filter samples (< 100 microg). The purpose of the study presented here is to investigate the effectiveness and limitations of air buoyancy corrections over experimentally adjusted conditions of temperature (21-25 degrees C) and relative humidity (RH) (16-60% RH). Conditioning (24 hr) and weighing were performed inside the Archimedes M3 environmentally controlled chamber. The measurements were performed using 20 size-fractionated samples of resuspended house dust loaded onto Teflo (PTFE) filters using a Micro-Orifice Uniform Deposit Impactor representing a wide range of mass loading (7.2-3130 microg) and cut sizes (0.056-9.9 microm). By maintaining tight controls on humidity (within 0.5% RH of control setting) throughout pre- and postweighing at each stepwise increase in RH, it was possible to quantify error due to water absorption: 45% of the total mass change due to water absorption occurred between 16 and 50% RH, and 55% occurred between 50 and 60% RH. The buoyancy corrections ranged from -3.5 to +5.8 microg in magnitude and improved relative standard deviation (RSD) from 21.3% (uncorrected) to 5.6% (corrected) for a 7.2 microg sample. It is recommended that protocols for weighing low-mass particle samples (e.g., nanoparticle samples) should include buoyancy corrections and tight temperature/humidity controls. In some cases, conditioning times longer than 24 hr may be warranted.
Synthesis and characterization of LiFePO4/C cathode materials by sol-gel method.
Liu, Shuxin; Yin, Hengbo; Wang, Haibin; Wang, Hong
2014-09-01
The carbon coated LiFePO4 cathode materials (LiFePO4/C) were successfully synthesized by sol-gel method with glucose, citric acid and PEG-4000 as dispersant and carbon source, respectively. The microstructure and grain size of LiFePO4/C composite were characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy. The results showed that the carbon source and calcination temperature had important effect on the graphitization degree of carbon; the carbon decomposed by citric acid had higher graphitization degree; with calcination temperature rising, the graphitization degree of carbon increased and the particles size increased. The graphitization degree and grain size were very important for improving the electrochemical performance of LiFePO4 cathode materials, according to the experimental results, the sample LFP-700 (LFP-C) which was synthesized with citric acid as dispersant at 700 degree C had lower polarization and larger discharge capacity.
Metastable phase formation in the Au-Si system via ultrafast nanocalorimetry
NASA Astrophysics Data System (ADS)
Zhang, M.; Wen, J. G.; Efremov, M. Y.; Olson, E. A.; Zhang, Z. S.; Hu, L.; de la Rama, L. P.; Kummamuru, R.; Kavanagh, K. L.; Ma, Z.; Allen, L. H.
2012-05-01
We have investigated the stability and solidification of nanometer size Au-Si droplets using an ultrafast heating/cooling nanocalorimetry and in situ growth techniques. The liquid can be supercooled to very low temperatures for both Au-rich (ΔT ˜ 95 K) and Si-rich (ΔT ˜ 220 K) samples. Solidification of a unique metastable phase δ1 is observed with a composition of 74 ± 4 at. % Au and a b-centered orthorhombic structure (a = 0.92, b = 0.72, and c = 1.35 nm; body-center in the a-c plane), which grows heteroepitaxially to Aus. Its melting temperature Tm is 305 ± 5 °C. There is competition during formation between the eutectic and δ1 phases but δ1 is the only metastable alloy observed. For small size droplets, both the δ1 and eutectic phases show considerable depression of the melting point (size-dependent melting).
NASA Astrophysics Data System (ADS)
Pawcenis, Dominika; Smoleń, Mariusz; Aksamit-Koperska, Monika A.; Łojewski, Tomasz; Łojewska, Joanna
2016-06-01
Size exclusion chromatography (SEC), especially coupled with multiple angle laser light scattering detector (MALLS) is a powerful tool in diagnostics of deterioration of historic and art objects to evaluate their condition. In this paper, SEC-UV-MALLS-DRI technique was applied to study degradation of silk fibroin samples ( Bombyx mori) artificially aged under various conditions: in the presence of oxygen, in different amount of water vapour and in volatile organic products (VOCs), all at temperature of 90 °C. Conditions were chosen in such a way that it mimicked real conditions of textiles' storing during exhibitions and in show cases. The influence of temperature, moisture and VOCs content on the state of silk textiles was examined with the use of size exclusion chromatography. Pseudo-zero-order Ekenstam equation was applied to study degradation rates of fibroin with use of the approximated values of DP of fibroin.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Halder, Nilanjan; Misra, Kamakhya Prakash
2016-05-06
Using titanium isopropoxide as the precursor, Titanium dioxide (TiO{sub 2}) powder was synthesized via sol-gel method, a promising low temperature route for preparing nanosized metal oxide semiconductors with good homogeneity at low cost. The as-prepared nano powder was thermally treated in air at 550, 650, 750, 900 and 1100°C for 1hr after drying at room temperature and used for further characterization. X-ray diffraction measurements showed that the annealing treatment has a strong impact on the crystal phase of TiO{sub 2} samples. The crystallite size as calculated from Debye Scherer formula lies in the range 29-69 nm and is found to increasemore » with increase in annealing temperature. Photoluminescence studies exhibit an improvement in the optical efficiency of the samples with post synthesis heat treatment. Annealing at temperature above 900°C results in a degradation of the structural and optical quality of the TiO{sub 2} nano powder samples.« less
NASA Astrophysics Data System (ADS)
Royle, Samuel H.; Montgomery, Wren; Kounaves, Samuel P.; Sephton, Mark A.
2017-12-01
Three Mars missions have analyzed the composition of surface samples using thermal extraction techniques. The temperatures of decomposition have been used as diagnostic information for the materials present. One compound of great current interest is perchlorate, a relatively recently discovered component of Mars' surface geochemistry that leads to deleterious effects on organic matter during thermal extraction. Knowledge of the thermal decomposition behavior of perchlorate salts is essential for mineral identification and possible avoidance of confounding interactions with organic matter. We have performed a series of experiments which reveal that the hydration state of magnesium perchlorate has a significant effect on decomposition temperature, with differing temperature releases of oxygen corresponding to different perchlorate hydration states (peak of O2 release shifts from 500 to 600°C as the proportion of the tetrahydrate form in the sample increases). Changes in crystallinity/crystal size may also have a secondary effect on the temperature of decomposition, and although these surface effects appear to be minor for our samples, further investigation may be warranted. A less than full appreciation of the hydration state of perchlorate salts during thermal extraction analyses could lead to misidentification of the number and the nature of perchlorate phases present.
Iron oxide nanoparticles in NaA zeolite cages
NASA Astrophysics Data System (ADS)
Kulshreshtha, S. K.; Vijayalakshmi, R.; Sudarsan, V.; Salunke, H. G.; Bhargava, S. C.
2013-07-01
Zeolite NaA samples with varying concentration of Fe3+ ions have been prepared by wet chemical method. Based on powder X-ray diffraction, 29Si and 27Al MAS NMR and Fe3+ EPR investigations, the formation of nano-sized ferric oxide particles inside the larger α-cages of zeolite NaA has been established. Both Mössbauer effect and magnetization measurements carried out down to 4.5 K established the superparamagnetic behaviour of these Fe2O3 particles with a blocking temperature of ≈20 K, where the magnetization values showed deviation for the zero field cooled and field cooled samples and the appearance of a very narrow magnetic hysteresis loop below this temperature. For all Fe3+ containing samples the room temperature Mössbauer spectrum is a broad quadrupole doublet with chemical shift, δ ≈ 0.33 mm/s and quadrupole splitting, ΔEq ≈ 0.68 mm/s. Variable temperature 57Fe Mössbauer effect measurements exhibited magnetic features below the blocking temperature and at 4.5 K, the observed spectrum is a broad magnetic sextet characterized by an internal hyperfine field value of ≈504 kOe along with a very weak central superparamagnetic quadrupole doublet.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Upadhyay, Sanjay Kumar; Reddy, V. Raghavendra, E-mail: varimalla@yahoo.com, E-mail: vrreddy@csr.res.in; Bag, Pallab
2014-09-15
Structural, dielectric, ferroelectric (FE), {sup 119}Sn Mössbauer, and specific heat measurements of polycrystalline BaTi{sub 1–x}Sn{sub x}O{sub 3} (x = 0% to 15%) ceramics are reported. Phase purity and homogeneous phase formation with Sn doping is confirmed from x-ray diffraction and {sup 119}Sn Mössbauer measurements. With Sn doping, the microstructure is found to change significantly. Better ferroelectric properties at room temperature, i.e., increased remnant polarization (38% more) and very low field switchability (225% less) are observed for x = 5% sample as compared to other samples and the results are explained in terms of grain size effects. With Sn doping, merging of all the phasemore » transitions into a single one is observed for x ≥ 10% and for x = 5%, the tetragonal to orthorhombic transition temperature is found close to room temperature. As a consequence better electro-caloric effects are observed for x = 5% sample and therefore is expected to satisfy the requirements for non-toxic, low energy (field) and room temperature based applications.« less
Analysis of a MIL-L-27502 lubricant from a gas-turbine engine test by size-exclusion chromatography
NASA Technical Reports Server (NTRS)
Jones, W. R., Jr.; Morales, W.
1983-01-01
Size exclusion chromatography was used to determine the chemical degradation of MIL-L-27502 oil samples from a gas turbine engine test run at a bulk oil temperature of 216 C. Results revealed a progressive loss of primary ester and additive depletion and the formation of higher molecular weight products with time. The high molecular weight products absorbed strongly in the ultraviolet indicating the presence of chromophoric groups.
NASA Astrophysics Data System (ADS)
Parimita Rath, Pragyan; Parhi, Pankaj Kumar; Ranjan Panda, Sirish; Priyadarshini, Barsharani; Ranjan Sahoo, Tapas
2017-08-01
This article, deals with a microwave-assisted polyol method to demonstrate a low temperature route < 250°C, to prepare a high temperature cubic zirconia phase. Powder XRD pattern shows broad diffraction peaks suggesting nanometric size of the particles. Magnetic behavior of 1-5 at% Ni doped samples show a threshold for substitutional induced room temperature ferromagnetism up to 3 at% of Ni. TGA data reveals that Ni-doped ZrO2 polyol precursors decompose exothermically below 300°C. IR data confirms the reduction of Zr(OH)4 precipitates to ZrO2, in agreement with the conclusions drawn from the TGA analysis.
BLISTERING AND EXPLOSIVE DESORPTION OF IRRADIATED AMMONIA-WATER MIXTURES
DOE Office of Scientific and Technical Information (OSTI.GOV)
Loeffler, M. J.; Baragiola, R. A., E-mail: mark.loeffler@nasa.gov, E-mail: raul@virginia.edu
2012-01-10
We present laboratory studies on the thermal evolution of a solid ammonia-water mixture after it has been irradiated at 20, 70, and 120 K. In samples irradiated at {<=}70 K, we observed fast outbursts that appear to indicate grain ejection and correlate well with the formation of micron-sized scattering centers. The occurrence of this phenomenon at the lower irradiation temperatures indicates that our results may be most relevant for understanding the release of gas and grains by comets and the surfaces of some of the colder icy satellites. We observe outgassing at temperatures below those where ice sublimates, which suggestsmore » that comets containing radiolyzed material may have outbursts farther from the Sun that those that are passive. In addition, the estimated size of the grains ejected from our sample is on the order of the size of E-ring particles, suggesting that our results give a plausible mechanism for how micron-sized grains could be formed from an icy surface. Finally, we propose that the presence of the {approx}4.5 {mu}m N{sub 2}O absorption band on an icy surface in outer space will serve to provide indirect evidence for radiation-processed ices that originally contained ammonia or nitrogen, which could be particularly useful since nitrogen is such a weak absorber in the infrared and ammonia is rapidly decomposed by radiolysis.« less
Vilaplana, Francisco; Martínez-Sanz, Marta; Ribes-Greus, Amparo; Karlsson, Sigbritt
2010-01-15
The emission of low molecular weight compounds from recycled high-impact polystyrene (HIPS) has been investigated using headspace solid-phase microextraction (HS-SPME) and gas chromatography-mass spectrometry (GC-MS). Four released target analytes (styrene, benzaldehyde, acetophenone, and 2-phenylpropanal) were selected for the optimisation of the HS-SPME sampling procedure, by analysing operating parameters such as type of SPME fibre (polarity and operating mechanism), particle size, extraction temperature and time. 26 different compounds were identified to be released at different temperatures from recycled HIPS, including residues of polymerisation, oxidated derivates of styrene, and additives. The type of SPME fibre employed in the sampling procedure affected the detection of emitted components. An adsorptive fibre such as carbowax/polydimethylsiloxane (CAR/PDMS fibre) offered good selectivity for both non-polar and polar volatile compounds at lower temperatures; higher temperatures result in interferences from less-volatile released compounds. An absorptive fibre as polydimethylsiloxane (PDMS) fibre is suitable for the detection of less-volatile non-polar molecules at higher temperatures. The nature and relative amount of the emitted compounds increased with higher exposure temperature and smaller polymeric particle size. HS-SPME proves to be a suitable technique for screening the emission of semi-volatile organic compounds (SVOCs) from polymeric materials; reliable quantification of the content of target analytes in recycled HIPS is however difficult due to the complex mass-transfer processes involved, matrix effects, and the difficulties in equilibrating the analytical system. 2009 Elsevier B.V. All rights reserved.
In-Situ Ultrafast 3D Imaging of Magma Vesiculation at High Temperature
NASA Astrophysics Data System (ADS)
Ulmer, P.; Pistone, M.; Caricchi, L.; Fife, J.; Marone, F.; Benson, P. M.; Almqvist, B.; Reusser, E.; Rust, A.; Burlini, L.
2011-12-01
We present new experimental results on magma vesiculation at high temperature. We investigated the processes of volatile exsolution (nucleation, growth and coalescence of gas bubbles) in magmas by performing in-situ high-temperature and ambient pressure experiments. Samples were heated with a newly-commissioned class 4 laser system and manual control. Simultaneously, the evolving 3D structure was captured by ultrafast synchrotron based X-ray tomographic microscopy (pixel size of 2.9 microns; 1 complete tomographic dataset acquired in 1 s), performed at the TOMCAT beam-line at Swiss Light Source (PSI, Villigen, Switzerland). Hydrous crystal- and bubble-free magmatic glasses liable to vesiculate at high temperature (400-1100 °C) were employed for the experiments. The samples used were cylindrical cores (2 mm in diameter and 2 mm in length), drilled from natural samples of obsidian (from: Lipari Island, Italy; Mayor Island, New Zealand; Tenerife Island, Spain; Little Glass Mountain, USA), containing different amounts of water (less than 1 wt%). These were chosen to represent a range of different physical properties (i.e., viscosity) as function of increasing temperature, due to their specific chemical compositions and, in particular, water content in the starting glass (measured via Karl Fischer titration). We observed the development of four different kinds of 3D microstructures during in-situ high-temperature experiments, depending on the starting material employed: (1) low vesicularity (40 vol%) with a narrow range in size of bubbles, which are generally spherical; (2) high vesicularity (80 vol%), showing a range of bubble sizes, shapes and extent of coalescence; (3) high vesicularity (85 vol%) and a polyhedral cell network (similar to reticulites); (4) a single expanding bubble. No magma fragmentation occurred in any of the experiments performed; we noticed different degrees of vertical thermal expansion, mainly depending on the amount of bubbles generated during heating. The real-time three-dimensional analyses provide new insights into the nucleation and exsolution mechanisms of volatiles that occur during ascent of magmas in volcanic conduits. As the timescale and modality of gas release from magmas are known to exert a key control on eruptive dynamics, we therefore propose a model that links the evolution of viscosity and water content with the modalities of vesiculation, in order to establish a relationship between gas release and eruptive dynamics.
Reaction of sodium calcium borate glasses to form hydroxyapatite.
Han, Xue; Day, Delbert E
2007-09-01
This study investigated the transformation of two sodium calcium borate glasses to hydroxyapatite (HA). The chemical reaction was between either 1CaO . 2Na(2)O . 6B(2)O(3) or 2CaO . 2Na(2)O . 6B(2)O(3) glass and a 0.25 M phosphate (K(2)HPO(4)) solution at 37, 75 and 200 degrees C. Glass samples in the form of irregular particles (125-180 microm) and microspheres (45-90 and 125-180 microm) were used in order to understand the reaction mechanism. The effect of glass composition (calcium content) on the weight loss rate and reaction temperature on crystal size, crystallinity and grain shape of the reaction products were studied. Carbonated HA was made by dissolving an appropriate amount of carbonate (K(2)CO(3)) in the 0.25 M phosphate solution. X-ray diffraction, Fourier transform infrared spectroscopy, and scanning electron microscopy were used to characterize the reaction products. The results show that sodium calcium borate glasses can be transformed to HA by reacting with a phosphate solution. It is essentially a process of dissolution of glass and precipitation of HA. The transformation begins from an amorphous state to calcium-deficient HA without changing the size and shape of the original glass sample. Glass with a lower calcium content (1CaO . 2Na(2)O . 6B(2)O(3)), or reacted at an elevated temperature (75 degrees C), has a higher reaction rate. The HA crystal size increases and grain shape changes from spheroidal to cylindrical as temperature increases from 37 to 200 degrees C. Increase in carbonate concentration can also decrease the crystal size and yield a more needle-like grain shape.
NASA Technical Reports Server (NTRS)
Mohr, Karen I.; Molinari, John; Thorncroft, Chris D,
2010-01-01
The characteristics of convective system populations in West Africa and the western Pacific tropical cyclone basin were analyzed to investigate whether interannual variability in convective activity in tropical continental and oceanic environments is driven by variations in the number of events during the wet season or by favoring large and/or intense convective systems. Convective systems were defined from TRMM data as a cluster of pixels with an 85 GHz polarization-corrected brightness temperature below 255 K and with an area at least 64 km 2. The study database consisted of convective systems in West Africa from May Sep for 1998-2007 and in the western Pacific from May Nov 1998-2007. Annual cumulative frequency distributions for system minimum brightness temperature and system area were constructed for both regions. For both regions, there were no statistically significant differences among the annual curves for system minimum brightness temperature. There were two groups of system area curves, split by the TRMM altitude boost in 2001. Within each set, there was no statistically significant interannual variability. Sub-setting the database revealed some sensitivity in distribution shape to the size of the sampling area, length of sample period, and climate zone. From a regional perspective, the stability of the cumulative frequency distributions implied that the probability that a convective system would attain a particular size or intensity does not change interannually. Variability in the number of convective events appeared to be more important in determining whether a year is wetter or drier than normal.
NASA Astrophysics Data System (ADS)
Das, Harinarayan; Inukai, Akihiro; Debnath, Nipa; Kawaguchi, Takahiko; Sakamoto, Naonori; Hoque, Sheikh Manjura; Aono, Hiromichi; Shinozaki, Kazuo; Suzuki, Hisao; Wakiya, Naoki
2018-01-01
In this paper, we report a detailed study of magnetic properties and AC magnetic heat generation characteristics of La0.77Sr0.23MnO3 (LSMO) nanoparticles to investigate appropriate crystallite size with a view to the proper application of self-controlled magnetic hyperthermia treatments of cancer. A series of nanocrystalline LSMO manganite was synthesized through the chemical route called as "polymerized complex method" and then subsequently annealed at the different temperature from 600 to 1400 °C to obtain various crystallite size. Phase formation and crystal structure of the prepared powder were determined by the powder X-ray diffraction (XRD) using Rietveld analysis. The XRD patterns reveal that all powder samples are a single phase rhombohedral perovskite-like structure with R 3 bar c space group. The mean crystallite size of prepared particles varied from 19 to 243.8 nm with the increase of the annealing temperature starting from 600 to 1400 °C. The field emission scanning electron microscopy (FE-SEM) analysis shows the surface morphology with a strong agglomeration of fine nanoparticles. The Magnetic study reveals that these nanoparticles exhibit ferromagnetic nature with different value of magnetization, coercivity, Curie temperature which is strongly dependent on their crystallite size. The maximum saturation temperature (TS = 66 °C) under AC magnetic field (H = 1.77 kA/m, f = 370 kHz) was found for the crystallite size of 39.5 nm due to its pure single domain phase. Such LSMO nanoparticles, having the higher heating rate, can be used in magnetically induced hyperthermia cancer treatment.
Urban Streams as Transporters or Transformers of Carbon and Nutrients: Does Size Matter?
NASA Astrophysics Data System (ADS)
Wood, K. L.; Kaushal, S.
2017-12-01
Urbanization degrades water quality, channel form/ function, and related ecosystem services. Biological and hydrological responses to urbanization vary between sites potentially due to watershed size, channel size, and geomorphology along the broader urban watershed continuum. We investigated if/when the size of a stream can influence water quality in urban watersheds. We conducted high-frequency sampling of a small polluted headwater stream and a large restored stream in the Anacostia watershed, Washington D.C. metro area. Temperature, pH, conductivity, discharge, dissolved inorganic carbon (DIC), dissolved organic carbon (DOC) and total dissolved nitrogen (TDN) were measured 2-3 times a week at two locations near the University of Maryland campus. DOC showed strong positive linear relationships with discharge at both sites, but TDN showed significant but contrasting linear relationships in the small polluted headwater site vs. the larger restored stream. In the larger restored stream, TDN significantly decreased with increasing water temperatures, which potentially suggested biological uptake. In the headwater stream, TDN concentrations significantly increased with increasing temperature, which suggests a possible seasonal input from terrestrial or in-stream sources. Interestingly, there were significant relationships between DIC and DOC in the larger restored stream, which suggested that there may have been a biological coupling of carbon forms due to stream ecosystem metabolism. Differences in relationships between TDN, DIC, and DOC and discharge, pH, and water temperatures may indicate the effects of stream size and floodplain restoration on water chemistry responses to human inputs. Larger streams may show greater potential for biogeochemical transformations, and stream size may need to be better evaluated in efforts to prioritize restoration strategies.
NASA Astrophysics Data System (ADS)
Sumangala, T. P.; Mahender, C.; Barnabe, A.; Venkataramani, N.; Prasad, Shiva
2016-11-01
Stoichiometric nano sized copper ferrite particles were synthesized by sol gel combustion technique. They were then calcined at various temperatures ranging from 300-800 °C and were either furnace cooled or quenched in liquid nitrogen. A high magnetisation value of 48.2 emu/g signifying the cubic phase of copper ferrite, was obtained for sample quenched to liquid nitrogen temperature from 800 °C. The ethanol sensing response of the samples was studied and a maximum of 86% response was obtained for 500 ppm ethanol in the case of a furnace cooled sample calcined at 800 °C. The chemical sensing is seen to be correlated with the c/a ratio and is best in the case of tetragonal copper ferrite.
Solution and Aging of MAR-M246 Nickel-Based Superalloy
NASA Astrophysics Data System (ADS)
Baldan, Renato; da Silva, Antonio Augusto Araújo Pinto; Nunes, Carlos Angelo; Couto, Antonio Augusto; Gabriel, Sinara Borborema; Alkmin, Luciano Braga
2017-02-01
Solution and aging heat-treatments play a key role for the application of the superalloys. The aim of this work is to evaluate the microstructure of the MAR-M246 nickel-based superalloy solutioned at 1200 and 1250 °C for 330 min and aged at 780, 880 and 980 °C for 5, 20 and 80 h. The γ' solvus, solidus and liquidus temperatures were calculated with the aid of the JMatPro software (Ni database). The as-cast and heat-treated samples were characterized by SEM/EDS and SEM-FEG. The γ' size precipitated in the aged samples was measured and compared with JMatPro simulations. The results have shown that the sample solutioned at 1250 °C for 330 min showed a very homogeneous γ matrix with carbides and cubic γ' precipitates uniformly distributed. The mean γ' size of aged samples at 780 and 880 °C for 5, 20 and 80 h did not present significant differences when compared to the solutioned sample. However, a significant increasing in the γ' particles was observed at 980 °C, evidenced by the large mean size of these particles after 80 h of aging heat-treatment.
NASA Astrophysics Data System (ADS)
Sharifzadegan, L.; Sedghi, H.
2018-07-01
In this work, samples of a nominal composition Y1 Ba2 - x Smx Cu3O7 - δ With Sm substitution (X = 0.00, 0.01, 0.03, 0.05) were prepared by the solid state reaction method. And the effect of substituting Sm instead of Ba was investigated on the structural and superconducting properties of the samples. Measurement of electrical resistance and critical temperature was done using 4-Probe connection method. Results indicate that Sm substitution affects the YBSCO superconducting samples, decrease the transition temperature of the superconductor and increases the special electrical resistance and the transition width. Also, XRD studies show that in all samples of the Y-123 phase, the formation and structure is orthorhombic. SEM images showed that the porosity in the samples increased with increasing Sm due to disruption in grain growth and instead, increase Sm in the samples cause decreasing the size of the grain.
How Students Cope with a Procedureless Lab Exercise.
ERIC Educational Resources Information Center
Pickering, Miles; Crabtree, Robert H.
1979-01-01
Reports a study conducted to determine how students cope with a procedureless laboratory situation in physical chemistry. Students are expected to use ingenuity, determine choice of sample size, conditions, and temperature extrapolation in an experiment on measuring heat of solution of an unknown salt. (Author/SA)
Synthesis and characterization of silicon nanorod on n-type porous silicon.
Behzad, Kasra; Mat Yunus, Wan Mahmood; Bahrami, Afarin; Kharazmi, Alireza; Soltani, Nayereh
2016-03-20
This work reports a new method for growing semiconductor nanorods on a porous silicon substrate. After preparation of n-type porous silicon samples, a thin layer of gold was deposited on them. Gold deposited samples were annealed at different temperatures. The structural, thermal, and optical properties of the samples were studied using a field emission scanning electron microscope (FESEM), photoacoustic spectroscopy, and photoluminescence spectroscopy, respectively. FESEM analysis revealed that silicon nanorods of different sizes grew on the annealed samples. Thermal behavior of the samples was studied using photoacoustic spectroscopy. Photoluminescence spectroscopy showed that the emission peaks were degraded by gold deposition and attenuated for all samples by annealing.
NASA Astrophysics Data System (ADS)
Ha, Jeong Won; Seong, Baek Seok; Jeong, Hi Won; Choi, Yoon Suk; Kang, Namhyun
2015-02-01
Inconel X-750 is a Ni-based precipitation-hardened superalloy typically used in springs designed for high-temperature applications such as the hold-down springs in nuclear power plants. γ‧ is a major precipitate in X-750 alloys which affects the strength, creep resistance, and stress relaxation properties of the spring. In this study, a solution-treated X-750 wire coiled into a spring was used that was aged at various temperatures and submitted to stress relaxation tests with and without loading. Small angle neutron scattering was employed to quantify the size and volume fraction of γ‧ phase in the springs as a function of the aging temperature and the application of a load during stress relaxation. The volume fraction of γ‧ precipitates increased in the specimen aged at 732 °C following stress relaxation at 500 °C for 300 h. However, the mean size of the precipitates in the samples was not affected by stress relaxation. The specimen aged at the lower temperature (620 °C) contained a smaller γ‧ volume fraction and gained a smaller fraction of γ‧ during stress relaxation compared with the sample aged at the higher temperature (732 °C). The smaller increase in the γ‧ volume fraction for the sample aged at 620 °C was associated with a larger increase in the M23C6 secondary carbide content during relaxation. The Cr depletion zone around the secondary carbides raises the solubility of γ‧ thereby decreasing the volume fraction of γ‧ precipitates in Inconel X-750. In terms of stress relaxation, a larger increase in the γ‧ volume fraction was measured with loading rather than without. This is probably associated with the dislocation accumulation generated under loading that facilitate the nucleation and growth of heterogeneous γ‧ phase due to enhanced diffusion.
NASA Astrophysics Data System (ADS)
Miura, H.; Kobayashi, T.; Kobayashi, M.
2014-08-01
Cu-18.2Zn-1.5Si-0.25Fe (mass%) alloy was heavily cold rolled. Ultrafine grained (UFGed) structure, containing a mixture of lamellar and mechanical twins, was easily and homogeneously formed. The average grain size was approximately 100 nm. The as-rolled sample showed quite high ultimate tensile strength (UTS) over 1 GPa. The UTS was higher than those obtained by multi directional forging. When the samples were annealed at relatively low temperatures between 553 K and 653 K, they showed slight hardening followed by large softening due to occurrence of static recrystallization (SRX). Annealing of UFGed structure at relatively low temperature of around 0.4 Tm caused extensive SRX that, in turn, induces ultrafine RXed grained structure. The grain size of the RXed sample was as fine as 200 nm. Although the annealing induced recovery of ductility while UTS gradually reduces, UTS over 1 GPa with ductility of 15 % were attained. The RXed grains mainly contained ultrafine annealing twins. Therefore, UFGed structure and superior mechanical properties could be achieved by a simple process of cold rolling, i.e., without severe plastic deformation.
Xu, Jiageng; Chen, Yu; Tan, Zhi; Nie, Rui; Wang, Qingyuan; Zhu, Jianguo
2018-01-01
A sort of tungsten/chromium(W/Cr) co-doped bismuth titanate (BIT) ceramics (Bi4Ti2.95W0.05O12.05 + 0.2 wt % Cr2O3, abbreviate to BTWC) are ordinarily sintered between 1050 and 1150 °C, and the indentation behavior and mechanical properties of ceramics sintered at different temperatures have been investigated by both nanoindentation and microindentation technology. Firstly, more or less Bi2Ti2O7 grains as the second phase were found in BTWC ceramics, and the grain size of ceramics increased with increase of sintering temperatures. A nanoindentation test for BTWC ceramics reveals that the testing hardness of ceramics decreased with increase of sintering temperatures, which could be explained by the Hall–Petch equation, and the true hardness could be calculated according to the pressure-state-response (PSR) model considering the indentation size effect, where the value of hardness depends on the magnitude of load. While, under the application of microsized Vickers, the sample sintered at a lower temperature (1050 °C) gained four linearly propagating cracks, however, they were observed to shorten in the sample sintered at a higher temperature (1125 °C). Moreover, both the crack deflection and the crack branching existed in the latter. The hardness and the fracture toughness of BTWC ceramics presented a contrary variational tendency with increase of sintering temperatures. A high sintering tends to get a lower hardness and a higher fracture toughness, which could be attributed to the easier plastic deformation and the stronger crack inhibition of coarse grains, respectively, as well as the toughening effect coming from the second phase. PMID:29584677
A Powder Delivery System (PoDS) for Mars in situ Science
NASA Astrophysics Data System (ADS)
Bryson, C.; Blake, D.; Saha, C.; Sarrazin, P.
2004-12-01
Many instruments proposed for in situ Mars science investigations work best with fine-grained samples of rocks or soils. Such instruments include the mineral analyzer CheMin [1] and any instrument that requires samples having high surface areas (e.g., mass spectrometers, organic analyzers, etc). The Powder Delivery System (PoDS) is designed to deliver powders of selected grain sizes from a sample acquisition device such as an arm-deployed robotic driller or corer to an instrument suite located on the body of a rover/lander. PoDS is capable of size-selective sampling of crushed rocks, soil or drill powder for delivery to instruments that require specific grain sizes (e.g. 5-50 mg of less than150 micron powder for CheMin). Sample material is transported as an aerosol of particles and gas by vacuum advection. In the laboratory a venturi pump driven by compressed air provides the impulse. On Mars, the ambient atmosphere is a source of CO2 that can be captured and compressed by adsorption pumping during diurnal temperature cycling [2]. The lower atmospheric pressure on the surface of Mars (7 torr) will affect fundamental parameters of gas-particle interaction such as Reynolds, Stocks and Knudsen numbers [3]. However, calculations show that the PoDS will operate under both Martian and terrestrial atmospheric conditions. Cyclone separators with appropriate particle size selection ranges remove particles from the aerosol stream. The vortex flow inside the cyclone causes grains larger than a specific size to be collected, while smaller grains remain entrained in the gas. Cyclones are very efficient inertial and centrifugal particle separators with cut sizes (d50) as low as 4 microns. Depending on the particle size ranges desired, a series of cyclones with descending cut sizes may be used, the simplest case being a single cyclone for particle deposition without mass separation. Transmission / membrane filters of appropriate pore sizes may also be used to collect powder from the aerosol stream. Results of a number of tests of the prototype PoDS will be presented. [1] Blake D. F., Sarrazin P., Bish D. L., Feldman S., Chipera S. J, Vaniman D.T., and Collins S., 2004, Definitive Mineralogical Analysis of Mars Analog Rocks Using the CheMin XRD/XRF Instrument, LPSC XXXV abstr. #1794 (CD-ROM). [2] Finn J. E., McKay C. P. and Sridhar R. K., 1999, Martian Atmosphere Utilization by Temperature-Swing Adsorption, University of Arizona, Publication No.961597, http://stl.ame.arizona.edu/publications/961597.pdf [3] Hinds W. C., 1999, Aerosol Technology - Properties, Behavior, and Measurement of Airborne Particles, Second edition, John Wiley & Sons, Inc., pp 15-67, 111-136.
NASA Astrophysics Data System (ADS)
Shabestari, S. G.; Divandari, M.; Ghoncheh, M. H.; Jamali, V.
2017-10-01
The aim of this research was evaluation of the solidification parameters of A356 alloy, e.g., dendrite arm spacing (DAS), correlation between cooling rate (CR) and DAS, hot tearing, and microstructural analysis at different coating thicknesses and strip sizes during the lost foam casting process (LFC). To achieve this goal, the DAS was measured at six coating thicknesses and six different strip sizes. In addition, thermal characteristics, such as the CR, temperatures of start and finish points of solidification, recalescence undercooling, and hot tearing susceptibility (HCSC), at five coating thicknesses were recognized from the cooling curves and their first derivative and the solid fraction curves, which have been plotted through the thermal analysis technique. The pouring temperature and strip size were fixed at 1063 K (790 °C) and 12 mm, respectively. Besides, to derive a numerical equation to predict the CR by measuring the DAS in this alloy, a microstructural evaluation was carried out on samples cast through 12-mm strip size. The results showed that both coating thickness and strip size had similar influences on the DAS, in which, by retaining one parameter at a constant value and simultaneous enhancement in the other parameter, the DAS increased significantly. Furthermore, at thinner coating layer, the higher amount of the CR was observed, which caused reduction in the temperatures of both the start and finish points of solidification. Also, increasing the CR caused a nonlinear increase in both the recalescence undercooling and the HCSC.
NASA Astrophysics Data System (ADS)
Kelson, Julia R.; Huntington, Katharine W.; Schauer, Andrew J.; Saenger, Casey; Lechler, Alex R.
2017-01-01
Carbonate clumped isotope (Δ47) thermometry has been applied to a wide range of problems in earth, ocean and biological sciences over the last decade, but is still plagued by discrepancies among empirical calibrations that show a range of Δ47-temperature sensitivities. The most commonly suggested causes of these discrepancies are the method of mineral precipitation and analytical differences, including the temperature of phosphoric acid used to digest carbonates. However, these mechanisms have yet to be tested in a consistent analytical setting, which makes it difficult to isolate the cause(s) of discrepancies and to evaluate which synthetic calibration is most appropriate for natural samples. Here, we systematically explore the impact of synthetic carbonate precipitation by replicating precipitation experiments of previous workers under a constant analytical setting. We (1) precipitate 56 synthetic carbonates at temperatures of 4-85 °C using different procedures to degas CO2, with and without the use of the enzyme carbonic anhydrase (CA) to promote rapid dissolved inorganic carbon (DIC) equilibration; (2) digest samples in phosphoric acid at both 90 °C and 25 °C; and (3) hold constant all analytical methods including acid preparation, CO2 purification, and mass spectrometry; and (4) reduce our data with 17O corrections that are appropriate for our samples. We find that the CO2 degassing method does not influence Δ47 values of these synthetic carbonates, and therefore probably only influences natural samples with very rapid degassing rates, like speleothems that precipitate out of drip solution with high pCO2. CA in solution does not influence Δ47 values in this work, suggesting that disequilibrium in the DIC pool is negligible. We also find the Δ47 values of samples reacted in 25 and 90 °C acid are within error of each other (once corrected with a constant acid fractionation factor). Taken together, our results show that the Δ47-temperature relationship does not measurably change with either the precipitation methods used in this study or acid digestion temperature. This leaves phosphoric acid preparation, CO2 gas purification, and/or data reduction methods as the possible sources of the discrepancy among published calibrations. In particular, the use of appropriate 17O corrections has the potential to reduce disagreement among calibrations. Our study nearly doubles the available synthetic carbonate calibration data for Δ47 thermometry (adding 56 samples to the 74 previously published samples). This large population size creates a robust calibration that enables us to examine the potential for calibration slope aliasing due to small sample size. The similarity of Δ47 values among carbonates precipitated under such diverse conditions suggests that many natural samples grown at 4-85 °C in moderate pH conditions (6-10) may also be described by our Δ47-temperature relationship.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Ahmad, Imran, E-mail: imraan77@yahoo.com; Abbas, Tahir; Ziya, A.B.
2014-04-01
Highlights: • Well-crystalline Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} nanoparticles with small grain size were obtained. • The approach is sol–gel auto-combustion technique for obtained nanoparticles. • The prepared Co{sub 0.7}Mg{sub 0.3}AlFeO{sub 4} ferrites are decent soft materials with low coercivity. • The minor decrease in lattice parameter with increase of temperature was observed. - Abstract: Single phased nanocrystalline Co{sub 0.7}Mg{sub 0.3}FeAlO{sub 4} ferrites having low coercivity were synthesized by the sol–gel auto-combustion route. The subsequent powder materials were sintered in a temperature range of 800–1200 °C for 2 h. The effects of sintering temperatures on the structure, morphology and magnetic propertiesmore » of the prepared soft magnetic material were studied. X-ray diffractometer (XRD), scanning electron microscope (SEM), transmission electron microscope (TEM), and magnetic property measurement system (MPMS) were used to characterize the samples. X-ray diffraction analysis confirmed a single-phase cubic spinel structure and ruled out the presence of impurities like hematite. The higher sintering temperatures have caused in enhanced mark of crystallinity and bigger average grain size of the nanocrystals. A slight decrease in lattice parameters was noticed with a rise of grain size. Magnetic measurements revealed that grain size increase led to a decrease in the coercivity and, in difference, an increase in the saturation magnetization.« less
Distinctive features of transport in topological insulators
NASA Astrophysics Data System (ADS)
Sacksteder, Vincent; Wu, Quansheng; Arnardottir, Kristin; Shelykh, Ivan; Kettemann, Stefan
2015-03-01
The surface states of a topological insulator in a fine-tuned magnetic field are ideal candidates for realizing a topological metal which is protected against disorder. Its signatures are (1) a conductance plateau in long wires and (2) a conductivity which always increases with sample size. We numerically show that the bulk substantially accelerates the conductance plateaus's decay in a magnetic field. It also reduces the effects of surface disorder and causes the magnitude of the surface conductivity and the magnetoconductivity to depend systematically on sample details such as doping and disorder strength. In addition, we predict a new signature of the topological state: at low temperatures the magnetoresistance will deviate strongly from the Hikami-Larkin-Nagaoka (HLN) formula. In this regime the magnetoresistance is dominated by scattering processes which wrap around the TI sample. The HLN formula's shoulder is replaced by a feature with a larger critical field magnetic strength that is caused by wrapping. Inside the wrapping regime the magnetoconductance will lose its dependence on temperature. This new topological signature should be visible in the same samples and temperatures where the Altshuler-Aronov-Spivak (AAS) effect has already been observed.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Machida, Emi; Research Fellowships of the Japan Society for the Promotion of Science, Japan Society for the Promotion of Science, 1-8 Chiyoda, Tokyo 102-8472; Horita, Masahiro
2012-12-17
We propose a low-temperature laser annealing method of a underwater laser annealing (WLA) for polycrystalline silicon (poly-Si) films. We performed crystallization to poly-Si films by laser irradiation in flowing deionized-water where KrF excimer laser was used for annealing. We demonstrated that the maximum value of maximum grain size of WLA samples was 1.5 {mu}m, and that of the average grain size was 2.8 times larger than that of conventional laser annealing in air (LA) samples. Moreover, WLA forms poly-Si films which show lower conductivity and larger carrier life time attributed to fewer electrical defects as compared to LA poly-Si films.
Ionic Impurity in a Bose-Einstein Condensate at Submicrokelvin Temperatures
NASA Astrophysics Data System (ADS)
Kleinbach, K. S.; Engel, F.; Dieterle, T.; Löw, R.; Pfau, T.; Meinert, F.
2018-05-01
Rydberg atoms immersed in a Bose-Einstein condensate interact with the quantum gas via electron-atom and ion-atom interaction. To suppress the typically dominant electron-neutral interaction, Rydberg states with a principal quantum number up to n =190 are excited from a dense and tightly trapped micron-sized condensate. This allows us to explore a regime where the Rydberg orbit exceeds the size of the atomic sample by far. In this case, a detailed line shape analysis of the Rydberg excitation spectrum provides clear evidence for ion-atom interaction at temperatures well below a microkelvin. Our results may open up ways to enter the quantum regime of ion-atom scattering for the exploration of charged quantum impurities and associated polaron physics.
NASA Astrophysics Data System (ADS)
Herrero-Bervera, E.; Acton, G.
2005-12-01
We investigate the magnetic mineralogy and absolute paleointensity of oceanic basalt samples from Hole 1256D, cored during Ocean Drilling Program (ODP) Leg 206. Hole 1256D is located on the Cocos Plate about 5 km east of the transition zone between marine magnetic anomalies 5Bn.2n and 5Br (~15 Ma). During Leg 206, the hole penetrated 502 m into basalts of the upper oceanic crust that was generated by superfast seafloor spreading (>200 mm/yr) along the East Pacific Rise. Rock magnetic investigations included continuous low field (k-T) thermomagnetic analyses, alternating field (AF) and thermal demagnetization, optical microscopy, saturation isothermal remanent magnetization (SIRM), and magnetic grain size analyses. Following the removal of a drilling overprint, AF and thermal demagnetization paths for most samples decay linearly to the origin on orthogonal vector end point diagrams, suggesting that a stable characteristic remanent magnetization component can be resolved. Optical microscopy and k-T (Curie points) identified titanomagnetites and titanomaghemites as the main magnetic carriers and grain size studies indicate that the carriers are either single domain (SD) and/or pseudosingle domain (PSD) in nature. Using the modified Thellier-Coe double heating method, we determined absolute paleointensity determinations for 51 specimens sampled from different ``stratigraphic'' levels of the core. pTRM checks were performed systematically one temperature step down the last pTRM acquisition in order to document magnetomineralogical changes during heating. The temperature was incremented by steps of 50°C between room temperature and 500°C and every 25-30°C for higher temperatures. The paleointensity determinations were obtained from the slope of the Arai diagrams. Special care was taken to interpret the Arai diagrams within the same range of temperatures lower than 300°C unless a clear and unique slope was present over a higher range of temperatures. Only about 10 percent of the samples yielded acceptable results. The paleofield estimated from these samples ranges between 28 to 16 micro Teslas (i.e., VADM of 6 to 4 x 1022 A/m2), which is concordant with the average paleofield intensity for the period between 0-160 Myr (4 ± 2 x1022 A/m2) and half of the strength of the present field (~8x1022 A/m2).
Baixench, M T; Al-Sheikh, M; Paugam, A
2005-01-01
The study included 37 urine samples which have been artificially infected with low levels (10(3) CFU/mL) of various fungi strains. We compared the effects of sample storage, up to 48 hours, at room temperature, in a urine evacuated tube containing specific additives with storage at + 4 degrees C, for the same length of time, in a urine evacuated tube without any additives. There have been no differences of results (speed of growth and colony size) between the 2 modes of storage. However, the experience has shown that samples needed a careful mixing before seeding to avoid underdetection of the strains. Based on the study results, the BD Vacutainer C&S tubes are suitable for delayed testing for the diagnosis of urine fungal infection.
NASA Astrophysics Data System (ADS)
Hiranuma, N.; Augustin-Bauditz, S.; Bingemer, H.; Budke, C.; Curtius, J.; Danielczok, A.; Diehl, K.; Dreischmeier, K.; Ebert, M.; Frank, F.; Hoffmann, N.; Kandler, K.; Kiselev, A.; Koop, T.; Leisner, T.; Möhler, O.; Nillius, B.; Peckhaus, A.; Rose, D.; Weinbruch, S.; Wex, H.; Boose, Y.; DeMott, P. J.; Hader, J. D.; Hill, T. C. J.; Kanji, Z. A.; Kulkarni, G.; Levin, E. J. T.; McCluskey, C. S.; Murakami, M.; Murray, B. J.; Niedermeier, D.; Petters, M. D.; O'Sullivan, D.; Saito, A.; Schill, G. P.; Tajiri, T.; Tolbert, M. A.; Welti, A.; Whale, T. F.; Wright, T. P.; Yamashita, K.
2015-03-01
Immersion freezing is the most relevant heterogeneous ice nucleation mechanism through which ice crystals are formed in mixed-phase clouds. In recent years, an increasing number of laboratory experiments utilizing a variety of instruments have examined immersion freezing activity of atmospherically relevant ice-nucleating particles. However, an intercomparison of these laboratory results is a difficult task because investigators have used different ice nucleation (IN) measurement methods to produce these results. A remaining challenge is to explore the sensitivity and accuracy of these techniques and to understand how the IN results are potentially influenced or biased by experimental parameters associated with these techniques. Within the framework of INUIT (Ice Nuclei Research Unit), we distributed an illite-rich sample (illite NX) as a representative surrogate for atmospheric mineral dust particles to investigators to perform immersion freezing experiments using different IN measurement methods and to obtain IN data as a function of particle concentration, temperature (T), cooling rate and nucleation time. A total of 17 measurement methods were involved in the data intercomparison. Experiments with seven instruments started with the test sample pre-suspended in water before cooling, while 10 other instruments employed water vapor condensation onto dry-dispersed particles followed by immersion freezing. The resulting comprehensive immersion freezing data set was evaluated using the ice nucleation active surface-site density, ns, to develop a representative ns(T) spectrum that spans a wide temperature range (-37 °C < T < -11 °C) and covers 9 orders of magnitude in ns. In general, the 17 immersion freezing measurement techniques deviate, within a range of about 8 °C in terms of temperature, by 3 orders of magnitude with respect to ns. In addition, we show evidence that the immersion freezing efficiency expressed in ns of illite NX particles is relatively independent of droplet size, particle mass in suspension, particle size and cooling rate during freezing. A strong temperature dependence and weak time and size dependence of the immersion freezing efficiency of illite-rich clay mineral particles enabled the ns parameterization solely as a function of temperature. We also characterized the ns(T) spectra and identified a section with a steep slope between -20 and -27 °C, where a large fraction of active sites of our test dust may trigger immersion freezing. This slope was followed by a region with a gentler slope at temperatures below -27 °C. While the agreement between different instruments was reasonable below ~ -27 °C, there seemed to be a different trend in the temperature-dependent ice nucleation activity from the suspension and dry-dispersed particle measurements for this mineral dust, in particular at higher temperatures. For instance, the ice nucleation activity expressed in ns was smaller for the average of the wet suspended samples and higher for the average of the dry-dispersed aerosol samples between about -27 and -18 °C. Only instruments making measurements with wet suspended samples were able to measure ice nucleation above -18 °C. A possible explanation for the deviation between -27 and -18 °C is discussed. Multiple exponential distribution fits in both linear and log space for both specific surface area-based ns(T) and geometric surface area-based ns(T) are provided. These new fits, constrained by using identical reference samples, will help to compare IN measurement methods that are not included in the present study and IN data from future IN instruments.
Deforestation and stream warming affect body size of Amazonian fishes.
Ilha, Paulo; Schiesari, Luis; Yanagawa, Fernando I; Jankowski, KathiJo; Navas, Carlos A
2018-01-01
Declining body size has been suggested to be a universal response of organisms to rising temperatures, manifesting at all levels of organization and in a broad range of taxa. However, no study to date evaluated whether deforestation-driven warming could trigger a similar response. We studied changes in fish body size, from individuals to assemblages, in streams in Southeastern Amazonia. We first conducted sampling surveys to validate the assumption that deforestation promoted stream warming, and to test the hypothesis that warmer deforested streams had reduced fish body sizes relative to cooler forest streams. As predicted, deforested streams were up to 6 °C warmer and had fish 36% smaller than forest streams on average. This body size reduction could be largely explained by the responses of the four most common species, which were 43-55% smaller in deforested streams. We then conducted a laboratory experiment to test the hypothesis that stream warming as measured in the field was sufficient to cause a growth reduction in the dominant fish species in the region. Fish reared at forest stream temperatures gained mass, whereas those reared at deforested stream temperatures lost mass. Our results suggest that deforestation-driven stream warming is likely to be a relevant factor promoting observed body size reductions, although other changes in stream conditions, like reductions in organic matter inputs, can also be important. A broad scale reduction in fish body size due to warming may be occurring in streams throughout the Amazonian Arc of Deforestation, with potential implications for the conservation of Amazonian fish biodiversity and food supply for people around the Basin.
Deforestation and stream warming affect body size of Amazonian fishes
Yanagawa, Fernando I.; Jankowski, KathiJo; Navas, Carlos A.
2018-01-01
Declining body size has been suggested to be a universal response of organisms to rising temperatures, manifesting at all levels of organization and in a broad range of taxa. However, no study to date evaluated whether deforestation-driven warming could trigger a similar response. We studied changes in fish body size, from individuals to assemblages, in streams in Southeastern Amazonia. We first conducted sampling surveys to validate the assumption that deforestation promoted stream warming, and to test the hypothesis that warmer deforested streams had reduced fish body sizes relative to cooler forest streams. As predicted, deforested streams were up to 6 °C warmer and had fish 36% smaller than forest streams on average. This body size reduction could be largely explained by the responses of the four most common species, which were 43–55% smaller in deforested streams. We then conducted a laboratory experiment to test the hypothesis that stream warming as measured in the field was sufficient to cause a growth reduction in the dominant fish species in the region. Fish reared at forest stream temperatures gained mass, whereas those reared at deforested stream temperatures lost mass. Our results suggest that deforestation-driven stream warming is likely to be a relevant factor promoting observed body size reductions, although other changes in stream conditions, like reductions in organic matter inputs, can also be important. A broad scale reduction in fish body size due to warming may be occurring in streams throughout the Amazonian Arc of Deforestation, with potential implications for the conservation of Amazonian fish biodiversity and food supply for people around the Basin. PMID:29718960
NASA Astrophysics Data System (ADS)
Zhao, Huayong; Williams, Ben; Stone, Richard
2014-01-01
A new low-cost optical diagnostic technique, called Cone Beam Tomographic Three Colour Spectrometry (CBT-TCS), has been developed to measure the planar distributions of temperature, soot particle size, and soot volume fraction in a co-flow axi-symmetric laminar diffusion flame. The image of a flame is recorded by a colour camera, and then by using colour interpolation and applying a cone beam tomography algorithm, a colour map can be reconstructed that corresponds to a diametral plane. Look-up tables calculated using Planck's law and different scattering models are then employed to deduce the temperature, approximate average soot particle size and soot volume fraction in each voxel (volumetric pixel). A sensitivity analysis of the look-up tables shows that the results have a high temperature resolution but a relatively low soot particle size resolution. The assumptions underlying the technique are discussed in detail. Sample data from an ethylene laminar diffusion flame are compared with data in the literature for similar flames. The comparison shows very consistent temperature and soot volume fraction profiles. Further analysis indicates that the difference seen in comparison with published results are within the measurement uncertainties. This methodology is ready to be applied to measure 3D data by capturing multiple flame images from different angles for non-axisymmetric flame.
In situ neutron scattering study of nanoscale phase evolution in PbTe-PbS thermoelectric material
Ren, Fei; Schmidt, Robert; Keum, Jong K.; ...
2016-08-24
Introducing nanostructural second phases has been proved to be an effective approach to reduce the lattice thermal conductivity and thus enhance the figure of merit for many thermoelectric materials. Furthermore studies of the formation and evolution of these second phases are central to understanding temperature dependent material behavior, improving thermal stabilities, as well as designing new materials. We examined powder samples of PbTe-PbS thermoelectric material using in situ neutron diffraction and small angle neutron scattering (SANS) techniques from room temperature to elevated temperature up to 663 K, to explore quantitative information on the structure, weight fraction, and size of themore » second phase. Neutron diffraction data showed the as-milled powder was primarily solid solution before heat treatment. During heating, PbS second phase precipitated out of the PbTe matrix around 480 K, while re-dissolution started around 570 K. The second phase remained separated from the matrix upon cooling. Furthermore, SANS data indicated there are two populations of nanostructures. The size of the smaller nanostructure increased from initially 5 nm to approximately 25 nm after annealing at 650 K, while the size of the larger nanostructure remained unchanged. Our study demonstrated that in situ neutron techniques are effective means to obtain quantitative information to study temperature dependent nanostructural behavior of thermoelectrics and likely other high-temperature materials.« less
Effect of phase transformation on optical and dielectric properties of zirconium oxide nanoparticles
NASA Astrophysics Data System (ADS)
Chintaparty, Rajababu; Palagiri, Bhavani; Reddy Nagireddy, Ramamanohar; subbha Reddy Imma Reddy, Venkata
2015-09-01
Zirconium oxide nanoparticle (ZrO2) is synthesized by the hydrothermal method at different calcination temperatures. The structural analysis is carried out by X-ray diffraction and Raman spectra. The sample prepared at 400 °C and 1100 °C showed the cubic and monoclinic phase, respectively, and the sample calcined at 600 °C and 800 °C showed the mixed phase with co-existence of cubic and monoclinic phases. Furthermore, the morphology and particle size of these samples were investigated by scanning electron microscope (SEM) and transmission electron microscope (TEM) analysis. The band gap estimated from UV-Vis spectra of ZrO2 (zirconia) nanocrystalline materials calcined at different temperatures from 400 °C to 1100 °C was in the range of 2.6-4.2 eV. The frequency dependence of dielectric constant and dielectric loss was investigated at room temperature. The low frequency region of dielectric constant is attributed to space charge effects.
NASA Astrophysics Data System (ADS)
Sun, Li; Zhang, Ru; Wang, Zhenduo; Ju, Lin; Cao, Ensi; Zhang, Yongjia
2017-01-01
Nickelferrite (NiFe2O4)powders were synthesized via sol-gel auto-combustion method and the corresponding temperature dependence of microstructure, dielectric and magnetic properties have been investigated. Results of XRD and SEM indicate that the NiFe2O4 samples exhibit a typical single phase spinel structure and a uniform particle distribution. The dielectric constant and dielectric loss measurements show strong frequency dependence of all the samples. The peak observed in frequency dependence of dielectric loss measurements shifts to higher frequency with the increasing sintering temperature, indicating a Debye-like dielectric relaxation. The remanent magnetization increases with the increasing grain size while the coercivity is just the opposite. The saturation magnetization can achieve 50 emu/g when the sintering temperature is more than 1000 °C, and the lowest coercivity (159.49 Oe) was observed in the NFO sample sintered at 1300 °C for 2 h.
Effect of temperature on the electrical properties of Zn0.95M0.05O (M = Zn, Fe, Ni)
NASA Astrophysics Data System (ADS)
Sedky, A.; Mohamed, S. B.
2014-01-01
We report here the structural and electrical properties of Zn0.95M0.05O ceramic varistors, M = Zn, Ni and Fe. The samples were tested for phase purity and structural morphology by using X-Ray diffraction XRD and scanning electron microscope SEM techniques. The current-voltage characteristics J-E were obtained by dc electrical measurements in the temperature range of 300-500 K. Addition of doping did not influence the hexagonal wurtzite structure of ZnO ceramics. Furthermore, the lattice parameters ratio c/a for hexagonal distortion and the length of the bond parallel to the c axis, u were nearly unaffected. The average grain size was decreased from 1.57 μm for ZnO to 1.19 μm for Ni sample and to 1.22 μm for Fe sample. The breakdown field EB was decreased as the temperature increased, in the following order: Fe > Zn > Ni. The nonlinear region was clearly observed for all samples as the temperature increased up to 400 K and completely disappeared with further increase of temperature up to 500 K. The values of nonlinear coefficient, a were between 1.16 and 42 for all samples, in the following order: Fe > Zn > Ni. Moreover, the electrical conductivity s was gradually increased as the temperature increased up to 500 K, in the following order: Ni > Zn > Fe. On the other hand, the activation energies were 0.194 eV, 0.136 and 0.223 eV for all samples, in the following order: Fe, Zn and Ni. These results have been discussed in terms of valence states, magnetic moment and thermo-ionic emission, which were produced by the doping, and controlling the potential barrier of ZnO.
Development of test methodology for dynamic mechanical analysis instrumentation
NASA Technical Reports Server (NTRS)
Allen, V. R.
1982-01-01
Dynamic mechanical analysis instrumentation was used for the development of specific test methodology in the determination of engineering parameters of selected materials, esp. plastics and elastomers, over a broad range of temperature with selected environment. The methodology for routine procedures was established with specific attention given to sample geometry, sample size, and mounting techniques. The basic software of the duPont 1090 thermal analyzer was used for data reduction which simplify the theoretical interpretation. Clamps were developed which allowed 'relative' damping during the cure cycle to be measured for the fiber-glass supported resin. The correlation of fracture energy 'toughness' (or impact strength) with the low temperature (glassy) relaxation responses for a 'rubber-modified' epoxy system was negative in result because the low-temperature dispersion mode (-80 C) of the modifier coincided with that of the epoxy matrix, making quantitative comparison unrealistic.
Temperature, grain size, and CO2-clathrate hydrates maps of Enceladus and Dione
NASA Astrophysics Data System (ADS)
Taffin, C.; Combe, J.; Grasset, O.; Le Menn, E.; McCord, T. B.; Bollengier, O.; Oancea, A.; Giraud, M.; Tobie, G.
2011-12-01
Reflectance spectra of water ice have absorption bands at 1.30 and 1.50 μm that depend on temperature and grain size. Band shape measurements can be used to characterize the surface properties of icy celestial bodies1,2,3. Moreover, CO2-clathrates have a diagnostic and unique absorption band at 2.7 μm. Mapping of these properties and components of the surface can be used to better constrain the internal activity and surface tectonics. We present an analysis of the 1.30 and 1.50 μm water ice absorption bands and the 2.7-μm CO2-clathrates absorption band in reflectance spectra from VIMS on Cassini in order to understand the geological history of the South Pole of Enceladus and an equatorial area of Dione. We have synthesized samples of pure ice Ih grains and acquired reflectance spectra between 1 and 5 μm with a Nicolet Fourier Transform spectrometer to investigate the characteristics of near-IR spectra using temperature and pressure ranges relevant for the icy satellites of Saturn. Forty-seven spectra of crystalline water ice have been acquired. We have derived two empirical laws to calculate temperature and grain size from pure crystalline water ice spectrum4. We have also synthesized samples of CO2-clathrates and acquired reflectance spectra for the band. These two spectra have been used as end-member. A linear sum is computed using the end-member spectra: [CRF×(clathrate)+(1-CRF)×(pure water ice)], where CRF is the to-be-determined clathrate ratio factor, 'clathrate' and 'pure water ice' are the reference spectra (end-member). Figure 1 shows results on one equatorial area where craters and ridges can be observed. Temperature appears to be higher besides the ridges (Figure 1f), but this may indicate that water ice is amorphous, which results in overestimating the temperature. Along the ridge, grain size is larger (Figure 1e), and CO2-clathrates have higher concentration near the ridges (Figure 1d). All these clues indicate a recent activity that we are planning to interpret in more details. 1)Fink and Larson, Icarus, 1975. 2)Leto et al. Mem. S.A.It. Suppl. 2005. 3)Grundy, Icarus, 1999. 4)Taffin et al., PSS, 2011
Comparative study of carbon free and carbon containing Li4Ti5O12 electrodes
NASA Astrophysics Data System (ADS)
Pohjalainen, Elina; Kallioinen, Jani; Kallio, Tanja
2015-04-01
Traditionally electrodes for lithium ion batteries are manufactured using carbon additives to increase the conductivity. However, in case of lithium titanate, Li4Ti5O12 (LTO), carbon free electrodes have gathered some interest lately. Therefore two LTO materials synthesized using the same synthesis but different end milling process resulting in materials with different particle size and surface area are compared here using electrodes manufactured with and without carbon additives. Both LTO samples (LTO-SP with small primary particle size and high surface area, and LTO-LP with larger primary particle size and small surface area) produce similar capacities and voltages with or without carbon additives at low C-rates at the room temperature. However, at high C-rates and/or sub-zero temperatures electrodes with carbon additives produce higher capacities and smaller ohmic losses and this behavior is more pronounced for the LTO electrodes with smaller primary particle size and larger surface area. These results show that the feasibility of carbon free LTO electrodes depends on the properties of LTO affecting the morphology of the electrode and consequently, the transport properties. This is most pronounced under conditions where electron and Li+ ion transfer become limiting (high C-rates and low temperature).
DOE Office of Scientific and Technical Information (OSTI.GOV)
Saw, C K
To date a global kinetic rate law has not been written to accurately describe solid-solid phase transformations of HMX and TATB where contributions from grain size effects, binder contents, and impurity levels are explicitly defined. Our recent work presented at the 2001 SCCM topical APS meeting, Atlanta, GA, demonstrated one can not confidently use the second harmonic generation (SHG) diagnostic to study energetic material phase transitions where non-uniform grain size distributions are present. For example, in HMX, the early arrival of SHG before the XRD in the SHG/XRD simultaneous high temperature experiment clearly indicates the partial molecular conversion from centrosymmetricmore » to non-centrosymmetric without any structural changes as exhibit by the XRD pattern. This conversion is attributed to the changes of the surface molecules due to the differences in potential between the surface and the bulk. The present paper reports on accurate XRD measurements following changes of {beta}-HMX to {delta}-HMX at elevated temperature. The results are compared for sample with 2 different grain sizes for HMX. We report accurate temperature dependent lattice parameters and hence volume and linear thermal expansion coefficients along each crystallographic axis. We have also conducted kinetic studies of the behavior of 2 grain-sizes of HMX and concluded that their kinetics, are drastically different.« less
DOE Office of Scientific and Technical Information (OSTI.GOV)
Willa, K.; Diao, Z.; Campanini, D.
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 ofmore » 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.« less
NASA Astrophysics Data System (ADS)
Das, Sananda; Sahoo, R. C.; Bera, K. P.; Nath, T. K.
2018-04-01
Doping at the post-transition metal site by trivalent rare-earth ions and 3d transition metal site by transition metal ions in perovskite lattice has observed a variety of magnetic and electronic orders with spatially correlated charge, spin and orbital degrees of freedom. Here, we report large ferromagnetism and enhanced dielectric constant (at ∼100 Hz) in chemically synthesized single phase multiferroic Bi1-xNdxFe1-yCoyO3 (x = 0, 0.10; y = 0, 0.10) nanoparticles (average particles size ∼45 nm). We have also examined the ferroelectric nature of our chemically synthesized samples. The Rietveld refinement of the XRD data reveals the structural symmetry breaking from distorted rhombohedral R3c structure of BiFeO3 to the triclinic P1 structure in Bi0.9Nd0.1Fe0.9Co0.1O3 (BNFCO) without having any iron rich impurity phase. The magnetization in these nanoceramics most likely originates from the coexistence of mixed valence states of Fe ion (Fe2+ and Fe3+). A high room temperature dielectric constant (∼1050) has been observed at 100 Hz of BNFCO sample. The frequency dependent anomalies near Neel temperature of antiferromagnet in temperature variation of dielectric study have been observed for all the doped and co-doped samples exhibiting typical characteristic of relaxor ferroelectrics. A spectacular enhancement of remanent magnetization MR (∼7.2 emu/gm) and noticeably large coercivity HC (∼17.4 kOe) at 5 K have been observed in this BNFCO sample. Such emergence of ferromagnetic ordering indicates the canting of the surface spins at the surface boundaries because of the reduction of particle size in nanodimension. We have also observed P-E hysteresis loops with a remanent polarization of 26 μC/cm2 and coercive field of 5.6 kV/cm of this sample at room temperature. From impedance spectroscopy study the estimated activation energy of 0.41 eV suggests the semiconducting nature of our nanoceramic BNCFO sample.
Planetesimal Formation in the Warm, Inner Disk: Experiments with Tempered Dust
NASA Astrophysics Data System (ADS)
de Beule, Caroline; Landers, Joachim; Salamon, Soma; Wende, Heiko; Wurm, Gerhard
2017-03-01
It is an open question how elevated temperatures in the inner parts of protoplanetary disks influence the formation of planetesimals. We approach this problem here by studying the tensile strength of granular beds with dust samples tempered at different temperatures. We find via laboratory experiments that tempering at increasing temperatures is correlated with an increase in cohesive forces. We studied dust samples of palagonite (JSC Mars-1a) which were tempered for up to 200 hr at temperatures between 600 and 1200 K, and measured the relative tensile strengths of highly porous dust layers once the samples cooled to room temperature. Tempering increases the tensile strength from 800 K upwards. This change is accompanied by mineral transformations, the formation of iron oxide crystallites as analyzed by Mössbauer spectroscopy, changes in the number size distribution, and the morphology of the surface visible as cracks in larger grains. These results suggest a difference in the collisional evolution toward larger bodies with increasing temperature as collisional growth is fundamentally based on cohesion. While high temperatures might also increase sticking (not studied here), compositional evolution will already enhance the cohesion and the possibility of growing larger aggregates on the way toward planetesimals. This might lead to a preferred in situ formation of inner planets and explain the observed presence of dense inner planetary systems.
Planetesimal Formation in the Warm, Inner Disk: Experiments with Tempered Dust
DOE Office of Scientific and Technical Information (OSTI.GOV)
De Beule, Caroline; Landers, Joachim; Salamon, Soma
2017-03-01
It is an open question how elevated temperatures in the inner parts of protoplanetary disks influence the formation of planetesimals. We approach this problem here by studying the tensile strength of granular beds with dust samples tempered at different temperatures. We find via laboratory experiments that tempering at increasing temperatures is correlated with an increase in cohesive forces. We studied dust samples of palagonite (JSC Mars-1a) which were tempered for up to 200 hr at temperatures between 600 and 1200 K, and measured the relative tensile strengths of highly porous dust layers once the samples cooled to room temperature. Temperingmore » increases the tensile strength from 800 K upwards. This change is accompanied by mineral transformations, the formation of iron oxide crystallites as analyzed by Mössbauer spectroscopy, changes in the number size distribution, and the morphology of the surface visible as cracks in larger grains. These results suggest a difference in the collisional evolution toward larger bodies with increasing temperature as collisional growth is fundamentally based on cohesion. While high temperatures might also increase sticking (not studied here), compositional evolution will already enhance the cohesion and the possibility of growing larger aggregates on the way toward planetesimals. This might lead to a preferred in situ formation of inner planets and explain the observed presence of dense inner planetary systems.« less
NASA Astrophysics Data System (ADS)
Wongpratat, Unchista; Maensiri, Santi; Swatsitang, Ekaphan
2016-09-01
Effect of cations distribution upon EXAFS analysis on magnetic properties of Co1-xNixFe2O4 (x = 0, 0.25, 0.50, 0.75 and 1.0) nanoparticles prepared by the hydrothermal method in aloe vera extract solution were studied. XRD analysis confirmed a pure phase of cubic spinel ferrite of all samples. Changes in lattice parameter and particle size depended on the Ni content with partial substitution and site distributions of Co2+, Ni2+ ions of different ionic radii at both tetrahedral and octahedral sites in the crystal structure. Particle sizes of samples estimated by TEM images were found to be in the range of 10.87-62.50 nm. The VSM results at room temperature indicated the ferrimagnetic behavior of all samples. Superparamagnetic behavior was observed in NiFe2O4 sample. The coercivity (Hc) and remanance (Mr) values were related to the particle sizes of samples. The saturation magnetization (Ms) was increased by a factor of 1.4 to a value of 57.57 emu/g, whereas the coercivity (Hc) was decreased by a factor of 20 to a value of 63.15 Oe for a sample with x = 0.75. In addition to the cations distribution, the increase of aspect ratio (surface to volume ratio) due to the decrease of particle size could significantly affect the magnetic properties of the materials.
Freeze-cast alumina pore networks: Effects of freezing conditions and dispersion medium
DOE Office of Scientific and Technical Information (OSTI.GOV)
Miller, S. M.; Xiao, X.; Faber, K. T.
Alumina ceramics were freeze-cast from water- and camphene-based slurries under varying freezing conditions and examined using X-ray computed tomography (XCT). Pore network characteristics, i.e., porosity, pore size, geometric surface area, and tortuosity, were measured from XCT reconstructions and the data were used to develop a model to predict feature size from processing conditions. Classical solidification theory was used to examine relationships between pore size, temperature gradients, and freezing front velocity. Freezing front velocity was subsequently predicted from casting conditions via the two-phase Stefan problem. Resulting models for water-based samples agreed with solidification-based theories predicting lamellar spacing of binary eutectic alloys,more » and models for camphene-based samples concurred with those for dendritic growth. Relationships between freezing conditions and geometric surface area were also modeled by considering the inverse relationship between pore size and surface area. Tortuosity was determined to be dependent primarily on the type of dispersion medium. (C) 2015 Elsevier Ltd. All rights reserved.« less
Particle Morphology and Size Results from the Smoke Aerosol Measurement Experiment-2
NASA Technical Reports Server (NTRS)
Urban, David L.; Ruff, Gary A.; Greenberg, Paul S.; Fischer, David; Meyer, Marit; Mulholland, George; Yuan, Zeng-Guang; Bryg, Victoria; Cleary, Thomas; Yang, Jiann
2012-01-01
Results are presented from the Reflight of the Smoke Aerosol Measurement Experiment (SAME-2) which was conducted during Expedition 24 (July-September 2010). The reflight experiment built upon the results of the original flight during Expedition 15 by adding diagnostic measurements and expanding the test matrix. Five different materials representative of those found in spacecraft (Teflon, Kapton, cotton, silicone rubber and Pyrell) were heated to temperatures below the ignition point with conditions controlled to provide repeatable sample surface temperatures and air flow. The air flow past the sample during the heating period ranged from quiescent to 8 cm/s. The smoke was initially collected in an aging chamber to simulate the transport time from the smoke source to the detector. This effective transport time was varied by holding the smoke in the aging chamber for times ranging from 11 to 1800 s. Smoke particle samples were collected on Transmission Electron Microscope (TEM) grids for post-flight analysis. The TEM grids were analyzed to observe the particle morphology and size parameters. The diagnostics included a prototype two-moment smoke detector and three different measures of moments of the particle size distribution. These moment diagnostics were used to determine the particle number concentration (zeroth moment), the diameter concentration (first moment), and the mass concentration (third moment). These statistics were combined to determine the diameter of average mass and the count mean diameter and, by assuming a log-normal distribution, the geometric mean diameter and the geometric standard deviations can also be calculated. Overall the majority of the average smoke particle sizes were found to be in the 200 nm to 400 nm range with the quiescent cases producing some cases with substantially larger particles.
Evaluation of Low-Gravity Smoke Particulate for Spacecraft Fire Detection
NASA Technical Reports Server (NTRS)
Urban, David; Ruff, Gary A.; Mulholland George; Meyer, Marit; Yuan, Zeng guang; Cleary, Thomas; Yang, Jiann; Greenberg, Paul; Bryg, Victoria
2013-01-01
Tests were conducted on the International Space Station to evaluate the smoke particulate size from materials and conditions that are typical of those expected in spacecraft fires. Five different materials representative of those found in spacecraft (Teflon, Kapton, cotton, silicone rubber and Pyrell) were heated to temperatures below the ignition point with conditions controlled to provide repeatable sample surface temperatures and air flow. The air flow past the sample during the heating period ranged from quiescent to 8 cm/s. The effective transport time to the measurement instruments was varied from 11 to 800 seconds to simulate different smoke transport conditions in spacecraft. The resultant aerosol was evaluated by three instruments which measured different moments of the particle size distribution. These moment diagnostics were used to determine the particle number concentration (zeroth moment), the diameter concentration (first moment), and the mass concentration (third moment). These statistics were combined to determine the diameter of average mass and the count mean diameter and by assuming a log-normal distribution, the geometric mean diameter and the geometric standard deviations were also calculated. Smoke particle samples were collected on TEM grids using a thermal precipitator for post flight analysis. The TEM grids were analyzed to determine the particle morphology and shape parameters. The different materials produced particles with significantly different morphologies. Overall the majority of the average smoke particle sizes were found to be in the 200 to 400 nanometer range with the quiescent cases and the cases with increased transport time typically producing with substantially larger particles. The results varied between materials but the smoke particles produced in low gravity were typically twice the size of particles produced in normal gravity. These results can be used to establish design requirements for future spacecraft smoke detectors.
NASA Astrophysics Data System (ADS)
Smits, K. M.; Sakaki, T.; Limsuwat, A.; Illangasekare, T. H.
2009-05-01
It is widely recognized that liquid water, water vapor and temperature movement in the subsurface near the land/atmosphere interface are strongly coupled, influencing many agricultural, biological and engineering applications such as irrigation practices, the assessment of contaminant transport and the detection of buried landmines. In these systems, a clear understanding of how variations in water content, soil drainage/wetting history, porosity conditions and grain size affect the soil's thermal behavior is needed, however, the consideration of all factors is rare as very few experimental data showing the effects of these variations are available. In this study, the effect of soil moisture, drainage/wetting history, and porosity on the thermal conductivity of sandy soils with different grain sizes was investigated. For this experimental investigation, several recent sensor based technologies were compiled into a Tempe cell modified to have a network of sampling ports, continuously monitoring water saturation, capillary pressure, temperature, and soil thermal properties. The water table was established at mid elevation of the cell and then lowered slowly. The initially saturated soil sample was subjected to slow drainage, wetting, and secondary drainage cycles. After liquid water drainage ceased, evaporation was induced at the surface to remove soil moisture from the sample to obtain thermal conductivity data below the residual saturation. For the test soils studied, thermal conductivity increased with increasing moisture content, soil density and grain size while thermal conductivity values were similar for soil drying/wetting behavior. Thermal properties measured in this study were then compared with independent estimates made using empirical models from literature. These soils will be used in a proposed set of experiments in intermediate scale test tanks to obtain data to validate methods and modeling tools used for landmine detection.
Obadia, Laetitia; Rouillon, Thierry; Bujoli, Bruno; Daculsi, Guy; Bouler, Jean Michel
2007-01-01
In this work, calcium-deficient apatites (CDA) were synthesized by ammonia hydrolysis reaction of dicalcium phosphate dihydrate (DCPD; CaHPO4 x 2 H2O) to obtain biphasic calcium phosphates (BCP) without any extraionic substitution. The influence of three parameters was studied: temperature of the reaction (70 and 100 degrees C), time of the reaction (4 and 18 h), and the pressure (open and closed system). Experiments were made according to a factorial design method (FDM) allowing optimization of the number of samples as well as statistical analysis of results. Moreover, the influence of temperature (until 200 degrees C) was investigated. The crystal size of CDA was determined according to the Scherrer's formula and from Rietveld refinements taking the CDA anisotropy into account. The last method seems to be a reliable method to determine crystallite sizes of CDA, since crystallite sizes of CDA along <00l> and
NASA Astrophysics Data System (ADS)
Firrao, D.; Begley, J. A.; Silva, G.; Roberti, R.; de Benedetti, B.
1982-06-01
Charpy-V type samples either step-quenched from 1200 °C or directly quenched from the usual 870 °C temperature, fractured by a slow bend test procedure, have been fractographically examined. Their notch root radius, ρ, ranged from almost zero (fatigue precrack) up to 2.0 mm. The fracture initiation process at the notch differs according to root radius and heat treatment. Conventionally austenitized samples with ρ values larger than 0.07 mm approximately ( ρ eff) always display a continuous shear lip formation along the notch surface, whereas specimens with smaller notches do not exhibit a similar feature. Moreover, shear lip width in specimens with ρ > ρ eff is linearly related to the applied J-integral at fracture. In high temperature austenitized samples similar shear lips are almost nonexistent. The above findings, as well as overall fractographic features, are combined to explain why blunt notch AISI 4340 steel specimens display a better fracture resistance if they are conventionally heat treated, whereas fatigue precracked samples show a superior fracture toughness when they are step-quenched from 1200 °C. Variations of fracture morphologies with the notch root radius and heat treating procedures are associated with a shift toward higher Charpy transition temperatures under the combined influence of decreasing root radii and coarsening of the prior austenitic grain size at high austenitizing temperatures.
Structural and magnetic properties of Ga-substituted Co 2 ‑W hexaferrites
NASA Astrophysics Data System (ADS)
Mahmood, Sami H.; Al Sheyab, Qusai; Bsoul, Ibrahim; Mohsen, Osama; Awadallah, Ahmad
2018-05-01
Precursor powders of BaMg2-xCoxFe16O27 with (x = 0.0, 1.0, and 2.0) were prepared using high-energy ball milling, and the effects of chemical composition and sintering temperature on the structural and magnetic properties were investigated using x-ray diffractometer (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry (VSM). XRD patterns of the prepared samples indicated that crystallization of pure BaW hexaferrite phase was achieved at sintering temperature of 1300{\\deg} C, while BaM and cubic spinel phase intermediate phases were obtained at lower sintering temperatures of 1100{\\deg} C and 1200{\\deg} C. SEM images revealed improvement of the crystallization of the structural phases, and growth of the particle size with increasing the sintering temperature. The magnetic data of the samples sintered at 1300{\\deg} C revealed an increase of the saturation magnetization from 59.44 emu/g to 72.56 emu/g with increasing Co concentration (x) from 0.0 to 2.0. The coercive field Hc decreased from 0.07 kOe at x = 0.0, to 0.03 kOe at x = 1.0, and then increases to 0.09 kOe at x = 2.0. The thermomagnetic curves of the samples sintered at 1300{\\deg} C confirmed the existence of the W-type phase, and revealed spin reorientation transitions above room temperature.
NASA Astrophysics Data System (ADS)
Shabrawy, S. El; Bocker, C.; Miglierini, M.; Schaaf, P.; Tzankov, D.; Georgieva, M.; Harizanova, R.; Rüssel, C.
2017-01-01
An iron containing magnesium borate glass with the mol% composition 51.7 B2O3/9.3 K2O /1 P2O5/27.6MgO/10.4Fe2O3was prepared by the conventional melts quenching method followed by a thermal treatment process at temperatures in the range from 530 to 604 °C.The thermally treated samples were characterized by X-ray diffraction, scanning and transmission electron microscopy. It was shown that superparamagnetic MgFe2O4 nanoparticles were formed during thermal treatment. The size of the spinel type crystals was in the range from 6 to 15 nm. Mössbauer spectra of the powdered glass ceramic samples and the extracted nanoparticles after dissolving the glass matrix in diluted acid were recorded at room temperature. The deconvolution of the spectra revealed the crystallization of two spinel phases MgFe2O4 (as a dominant phase) and superparamagnetic maghemite, γ-Fe2O3 (as a secondary phase). Room temperature magnetic measurements showed that, increasing the crystallization temperature changed the superparamagnetic behavior of the samples to ferrimagnetic behavior. The Curie temperatures of the samples were measured and showed a higher value than that of the pure bulk MgFe2O4.
Rheology of ice I at low stress and elevated confining pressure
Durham, W.B.; Stern, L.A.; Kirby, S.H.
2001-01-01
Triaxial compression testing of pure, polycrystalline water ice I at conditions relevant to planetary interiors and near-surface environments (differential stresses 0.45 to 10 MPa, temperatures 200 to 250 K, confining pressure 50 MPa) reveals that a complex variety of rheologies and grain structures may exist for ice and that rheology of ice appears to depend strongly on the grain structures. The creep of polycrystalline ice I with average grain size of 0.25 mm and larger is consistent with previously published dislocation creep laws, which are now extended to strain rates as low as 2 ?? 10-8s-1. When ice I is reduced to very fine and uniform grain size by rapid pressure release from the ice II stability field, the rheology changes dramatically. At 200 and 220 K the rheology matches the grain-size-sensitive rheology measured by Goldsby and Kohlstedt [1997, this issue] at 1 atm. This finding dispels concerns that the Goldsby and Kohlstedt results were influenced by mechanisms such as microfracturing and cavitation, processes not expected to operate at elevated pressures in planetary interiors. At 233 K and above, grain growth causes the fine-grained ice to become more creep resistant. Scanning electron microscopy investigation of some of these deformed samples shows that grains have markedly coarsened and the strain hardening can be modeled by normal grain growth and the Goldsby and Kohlstedt rheology. Several samples also displayed very heterogeneous grain sizes and high aspect ratio grain shapes. Grain-size-sensitive creep and dislocation creep coincidentally contribute roughly equal amounts of strain rate at conditions of stress, temperature, and grain size that are typical of terrestrial and planetary settings, so modeling ice dynamics in these settings must include both mechanisms. Copyright 2001 by the American Geophysical Union.
Little effect of climate change on body size of herbivorous beetles.
Baar, Yuval; Friedman, Ariel Leib Leonid; Meiri, Shai; Scharf, Inon
2018-04-01
Ongoing climate change affects various aspects of an animal's life, with important effects on distribution range and phenology. The relationship between global warming and body size changes in mammals and birds has been widely studied, with most findings indicating a decline in body size over time. Nevertheless, little data exist on similar size change patterns of invertebrates in general and insects in particular, and it is unclear whether insects should decrease in size or not with climate warming. We measured over 4000 beetle specimens, belonging to 29 beetle species in 8 families, collected in Israel during the last 100 years. The sampled species are all herbivorous. We examined whether beetle body size had changed over the years, while also investigating the relationships between body size and annual temperature, precipitation, net primary productivity (NPP) at the collection site and collection month. None of the environmental variables, including the collection year, was correlated with the size of most of the studied beetle species, while there were strong interactions of all variables with species. Our results, though mostly negative, suggest that the effect of climate change on insect body size is species-specific and by no means a general macro-ecological rule. They also suggest that the intrapopulation variance in body size of insects collected as adults in the field is large enough to conceal intersite environmental effects on body size, such as the effect of temperature and NPP. © 2016 Institute of Zoology, Chinese Academy of Sciences.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Huie, Matthew M.; Marschilok, Amy C.; Takeuchi, Esther S.
Here, this report describes a synthetic approach to control the crystallite size of silver vanadium phosphorous oxide, Ag 0.50VOPO 4·1.9H 2O, and the impact on electrochemistry in lithium based batteries. Ag 0.50VOPO 4·1.9H 2O was synthesized using a stirred hydrothermal method over a range of temperatures. X-ray diffraction (XRD) was used to confirm the crystalline phase and the crystallite size sizes of 11, 22, 38, 40, 49, and 120 nm. Particle shape was plate-like with edges <1 micron to >10 microns. Under galvanostatic reduction the samples with 22 nm crystallites and 880 nm particles produced the highest capacity, ~25% moremore » capacity than the 120 nm sample. Notably, the 11 nm sample resulted in reduced delivered capacity and higher resistance consistent with increased grain boundaries contributing to resistance. Under intermittent pulsing ohmic resistance decreased with increasing crystallite size from 11 nm to 120 nm implying that electrical conduction within a crystal is more facile than between crystallites and across grain boundaries. Finally, this systematic study of material dimension shows that crystallite size impacts deliverable capacity as well as cell resistance where both interparticle and intraparticle transport are important.« less
Huie, Matthew M.; Marschilok, Amy C.; Takeuchi, Esther S.; ...
2017-04-12
Here, this report describes a synthetic approach to control the crystallite size of silver vanadium phosphorous oxide, Ag 0.50VOPO 4·1.9H 2O, and the impact on electrochemistry in lithium based batteries. Ag 0.50VOPO 4·1.9H 2O was synthesized using a stirred hydrothermal method over a range of temperatures. X-ray diffraction (XRD) was used to confirm the crystalline phase and the crystallite size sizes of 11, 22, 38, 40, 49, and 120 nm. Particle shape was plate-like with edges <1 micron to >10 microns. Under galvanostatic reduction the samples with 22 nm crystallites and 880 nm particles produced the highest capacity, ~25% moremore » capacity than the 120 nm sample. Notably, the 11 nm sample resulted in reduced delivered capacity and higher resistance consistent with increased grain boundaries contributing to resistance. Under intermittent pulsing ohmic resistance decreased with increasing crystallite size from 11 nm to 120 nm implying that electrical conduction within a crystal is more facile than between crystallites and across grain boundaries. Finally, this systematic study of material dimension shows that crystallite size impacts deliverable capacity as well as cell resistance where both interparticle and intraparticle transport are important.« less
Structural and Magnetic Characterization of BaFe12O19 Nanoparticles
NASA Astrophysics Data System (ADS)
Dhage, Vinod N.; Mane, M. L.; Shirsath, Sagar E.; Jadhav, S. P.; Gunjal, R. P.; Jadhav, K. M.
2011-07-01
Barium hexaferrite nanoparticles have been synthesized successfully by using sol-gel auto-combustion technique. In this process dextrose and citric acid both used as a fuel separately. The ratio of cation to both the fuel was maintained at 1:3 whereas the pH of the sample was kept constant at 8. The particle size for dextrose and citric acid sample is 34 nm and 45 nm respectively. The room temperature hysteresis curve gives maximum magnetization (48.46 emu/g) and coercivity (1.350 kOe) values for dextrose used sample. The dextrose used sample gives better results than that of citric acid used sample.
NASA Astrophysics Data System (ADS)
Sadiq, Muhammad; Pesci, Raphaël; Cherkaoui, Mohammed
2013-03-01
An extensive study is made to analyze the impact of pure lanthanum on the microstructure and mechanical properties of Sn-Ag-Cu (SAC) alloys at high temperatures. Different compositions are tested; the temperature applied for the isothermal aging is 150°C, and aging times of 10 h, 25 h, 50 h, 100 h, and 200 h are studied. Optical microscopy with cross-polarized light is used to follow the grain size, which is refined from 8 mm to 1 mm for as-cast samples and is maintained during thermal aging. Intermetallic compounds (IMCs) present inside the bulk Sn matrix affect the mechanical properties of the SAC alloys. Due to high-temperature exposure, these IMCs grow and hence their impact on mechanical properties becomes more significant. This growth is followed by scanning electron microscopy, and energy-dispersive spectroscopy is used for elemental mapping of each phase. A significant refinement in the average size of IMCs of up to 40% is identified for the as-cast samples, and the coarsening rate of these IMCs is slowed by up to 70% with no change in the interparticle spacing. Yield stress and tensile strength are determined through tensile testing at 20°C for as-cast samples and after thermal aging at 150°C for 100 h and 200 h. Both yield stress and tensile strength are increased by up to 20% by minute lanthanum doping.
NASA Astrophysics Data System (ADS)
Qiu, Ren-Zheng; Li, Chi-Chen; Fang, Te-Hua
2017-08-01
This study investigated the mechanical properties and crack propagation behavior of polycrystalline copper using a molecular dynamics simulation. The effects of temperature, grain size, and crack length were evaluated in terms of atomic trajectories, slip vectors, common neighbor analysis, the material’s stress-strain diagram and Young’s modulus. The simulation results show that the grain boundary of the material is more easily damaged at high temperatures and that grain boundaries will combine at the crack tip. From the stress-strain diagram, it was observed that the maximum stress increased as the temperature decreased. In contrast, the maximum stress was reduced by increasing the temperature. With regard to the effect of the grain size, when the grain size was too small, the structure of the sample deformed due to the effect of atomic interactions, which caused the grain boundary structure to be disordered in general. However, when the grain size was larger, dislocations appeared and began to move from the tip of the crack, which led to a new dislocation phenomenon. With regards to the effect of the crack length, the tip of the crack did not affect the sample’s material when the crack length was less than 5 nm. However, when the crack length was above 7.5 nm, the grain boundary was damaged, and twinning structures and dislocations appeared on both sides of the crack tip. This is because the tip of the crack was blunt at first before sharpening due to the dislocation effect.
EPR investigation of UV light effect on calcium carbonate powders with different grain sizes.
Kabacińska, Zuzanna; Krzyminiewski, Ryszard; Dobosz, Bernadeta
2014-06-01
This study is based on investigation of calcium carbonate powders with different grain sizes exposed to UV light. Calcium carbonate is widely used in many branches of industry, e.g. as a filler for polymer materials; therefore, knowing its properties, among them also its reaction to UV light, is essential. Samples of powdered calcium carbonate with average grain sizes of 69 and 300 nm and 2.1, 6, 16, 25 µm were used in this investigation. Measurements were performed at room temperature using EPR X-band spectrometer, and they have shown the additional signals induced by the light from Hg lamp. The effect of annealing of the micro-grain samples was also studied. The spectra of four micro-grain samples after irradiation are similar, but there are differences between them and the other two powders, which could be related to the different sizes of their grains. Further studies based on these preliminary results may prove useful in research of photodegradation of CaCO3-filled materials, as well as helpful in increasing the accuracy of dating of archaeological and geological objects. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.
Crystalline silicon growth in nickel/a-silicon bilayer
NASA Astrophysics Data System (ADS)
Mohiddon, Md Ahamad; Naidu, K. Lakshun; Dalba, G.; Rocca, F.; Krishna, M. Ghanashyam
2013-02-01
The effect of substrate temperature on amorphous Silicon crystallization, mediated by metal impurity is reported. Bilayers of Ni(200nm)/Si(400nm) are deposited on fused silica substrate by electron beam evaporator at 200 and 500 °C. Raman mapping shows that, 2 to 5 micron size crystalline silicon clusters are distributed over the entire surface of the sample. X-ray diffraction and X-ray absorption spectroscopy studies demonstrate silicon crystallizes over the metal silicide seeds and grow with the annealing temperature.
About the optical properties of oxidized black silicon structures
NASA Astrophysics Data System (ADS)
Pincik, E.; Brunner, R.; Kobayashi, H.; Mikula, M.; Kučera, M.; Švec, P.; Greguš, J.; Vojtek, P.; Zábudlá, Z.; Imamura, K.; Zahoran, M.
2017-02-01
The paper deals with the optical and morphological properties of thermally oxidized black silicon (OBSi) nano-crystalline specimens produced by the surface structure chemical transfer method (SSCT). This method can produce a nano-crystalline Si black color layer on c-Si with a range of thickness of ∼50 nm to ∼300 nm by the contact of c-Si immersed in chemical solutions HF + H2O2 with a catalytic mesh. We present and discuss mainly the photoluminescence properties of both polished c-Si and OBSi structures, respectively. The similar photoluminescence (PL) behaviors recorded at liquid helium (6 K) and room temperatures on both polished crystalline Si and OBSi samples, respectively, indicate the similar origin of recorded luminescence light. As the positions of PL maxima of OBSi structures are mainly related to the size of Si nanocrystallites and SiO(x), we therefore suppose that the size of the dominant parts of the luminated OBSi nanostructure is pre-determined by the used polishing Si procedure, and/or the distribution function of the number of formed crystallites on their size is very similar. The blue shift of both PL spectra reaching almost value of 0.40 eV observed after the decrease of the sample temperature to 6 K we relate also with the change of the semiconductor band gap width.
NASA Astrophysics Data System (ADS)
Chen, D. G.; Tang, X. G.; Wu, J. B.; Zhang, W.; Liu, Q. X.; Jiang, Y. P.
2011-06-01
Ni 0.5Zn 0.5Fe 2O 4 (NZFO) spinel-type nanoparticles were directly fabricated by the chemical co-precipitation process using metal nitrate and acetate as precursors since nitrogen and carbon would be taken away in the forms of oxynitride and oxycarbide, respectively, after the precursors were annealed and then investigated in detail by employing X-ray diffraction (XRD), magnetic measurement and Raman spectroscopy. XRD analysis indicates that the as-prepared nanocrystals are all of a pure cubic spinel structure with their sizes ranging from 20.8 to 53.3 nm, as well as peaks of some samples shifting to lower angles due to lattice expansion. Calculations from the derived XRD data indicate that the activation energy is 30.83 kJ/mol. The magnetic measurements show that these samples are superparamagnetic. The saturation magnetization increases with annealing temperature, which may be explained by super-exchange interactions of Fe ions occurring at A- and B-sites. The variation of coercivity with particle size is interpreted on the basis of domain structure and crystal anisotropy. Furthermore, these nanoparticles exhibit a redshift phenomenon at lower temperatures seen in the Raman spectra, which could be related to ionic substitution.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Allen, T. R.; Tsai, H.; Cole, J. I.
2002-09-17
To assess the effects of long-term, low-dose-rate neutron exposure on mechanical strength and ductility, tensile properties were measured on 12% and 20% cold-worked Type 316 stainless steel. Samples were prepared from reactor core components retrieved from the EBR-II reactor following final shutdown. Sample locations were chosen to cover a dose range of 1-56 dpa at temperatures from 371-440 C and dose rates from 0.5-5.8 x10{sup -7} dpa/s. These dose rates are approximately an order of magnitude lower than those of typical EBR-II test sample locations. The tensile tests for the 12% CW material were performed at 380 C and 430more » C while those for the 20% CW samples were performed at 370 C. In each case, the tensile test temperature approximately matched the irradiation temperature. To help understand the tensile properties, microstructural samples with similar irradiation history were also examined. The strength and loss of work hardening increase the fastest as a function of irradiation dose for the 12% CW material irradiated at lower temperature. The decrease in ductility with increasing dose occurs more rapidly for the 12% CW material irradiated at lower temperature and the 20% cold-worked material. Post-tensile test fractography indicates that at higher dose, the 20% CW samples begin a shift in fracture mode from purely ductile to mainly small facets and slip bands, suggesting a transition toward channel fracture. The fracture for all of the 12% cold-worked samples was ductile. For both the 12% and 20% CW materials, the yield strength increases correlate with changes in void and loop density and size.« less
NASA Technical Reports Server (NTRS)
Okoro, Chika L.
2004-01-01
GRCop-84 was developed to meet the mechanical and thermal property requirements for advanced regeneratively cooled rocket engine main combustion chamber liners. It is a ternary Cu- Cr-Nb alloy having approximately 8 at% Cr and 4 at% Nb. The chromium and niobium constituents combine to form 14 vol% Cr2Nb, the strengthening phase. The alloy is made by producing GRCop-84 powder through gas atomization and consolidating the powder using extrusion, hot isostatic pressing (HIP) or vacuum plasma spraying (VPS). GRCop-84 has been selected by Rocketdyne, Ratt & Wlutney and Aerojet for use in their next generation of rocket engines. GRCop-84 demonstrates favorable mechanical and thermal properties at elevated temperatures. Compared to NARloy-Z, the currently used inaterial in the Space Shuttle, GRCop-84 has approximately twice the yield strength, 10-1000 times the creep life, and 1.5-2.5 times the low cycle fatigue life. The thermal expansion of GRCop-84 is 7515% less than NARloy-Z which minimizes thermally induced stresses. The thermal conductivity of the two alloys is comparable at low temperature but NARloy-Z has a 20-50 W/mK thermal conductivity advantage at typical rocket engine hot wall temperatures. GRCop-84 is also much more microstructurally stable than NARloy-Z which translates into better long term stability of mechanical properties. Previous research into metal alloys fabricated by means of powder metallurgy (PM), has demonstrated that initial powder size can affect the microstructural development and mechanical properties of such materials. Grain size, strength, ductility, size of second phases, etc., have all been shown to vary with starting powder size in PM-alloys. This work focuses on characterizing the effect of varying starting powder size on the microstructural evolution and mechanical properties of as- extruded GRCop-84. Tensile tests and constant load creep tests were performed on extrusions of four powder meshes: +140 mesh (great3er than l05 micron powder size), -140 mesh (less than or equal to 105 microns), -140 plus or minus 270 (53 - 105 microns), and - 270 mesh (less than or equal to 53 microns). Samples were tested in tension at room temperature and at 500 C (932 F). Creep tests were performed under vacuum at 500 C using a stress of 111 MPa (16.1 ksi). The fracture surfaces of selected samples from both tests were studied using a Scanning Electron Microscope (SEM). The as-extruded materials were also studied, using both optical microscopy and SEM analysis, to characterize changes within the microstructure.
NASA Astrophysics Data System (ADS)
Bolon, Bruce T.; Haugen, M. A.; Abin-Fuentes, A.; Deneen, J.; Carter, C. B.; Leighton, C.
2007-02-01
We have used ferromagnet/antiferromagnet/ferromagnet trilayers and ferromagnet/antiferromagnet multilayers to probe the grain size dependence of exchange bias in polycrystalline Co/Fe 50Mn 50. X-ray diffraction and transmission electron microscopy show that the Fe 50Mn 50 (FeMn) grain size increases with increasing FeMn thickness in the Co (30 Å)/FeMn system. Hence, in Co(30 Å)/FeMn( tAF Å)/Co(30 Å) trilayers the two Co layers sample different FeMn grain sizes at the two antiferromagnet/ferromagnet interfaces. For FeMn thicknesses above 100 Å, where simple bilayers have a thickness-independent exchange bias, we are therefore able to deduce the influence of FeMn grain size on the exchange bias and coercivity (and their temperature dependence) simply by measuring trilayer and multilayer samples with varying FeMn thicknesses. This can be done while maintaining the (1 1 1) orientation, and with little variation in interface roughness. Increasing the average grain size from 90 to 135 Å results in a fourfold decrease in exchange bias, following an inverse grain size dependence. We interpret the results as being due to a decrease in uncompensated spin density with increasing antiferromagnet grain size, further evidence for the importance of defect-generated uncompensated spins.
NASA Astrophysics Data System (ADS)
Marselin, M. Abila; Jaya, N. Victor
2016-04-01
In this paper, pure NiO and Cu-doped NiO nanoparticles are prepared by co-precipitation method. The electrical resistivity measurements by applying high pressure on pure NiO and Cu-doped NiO nanoparticles were reported. The Bridgman anvil set up is used to measure high pressures up to 8 GPa. These measurements show that there is no phase transformation in the samples till the high pressure is reached. The samples show a rapid decrease in electrical resistivity up to 5 GPa and it remains constant beyond 5 GPa. The electrical resistivity and the transport activation energy of the samples under high pressure up to 8 GPa have been studied in the temperature range of 273-433 K using diamond anvil cell. The temperature versus electrical resistivity studies reveal that the samples behave like a semiconductor. The activation energies of the charge carriers depend on the size of the samples.
NASA Technical Reports Server (NTRS)
Walker, D.; Kirkpatrick, R. J.; Longhi, J.; Hays, J. F.
1976-01-01
Experimental crystallization of a lunar picrite composition (sample 12002) at controlled linear cooling rates produces systematic changes in the temperature at which crystalline phases appear, in the texture, and in crystal morphology as a function of cooling rate. Phases crystallize in the order olivine, chromium spinel, pyroxene, plagioclase, and ilmenite during equilibrium crystallization, but ilmenite and plagioclase reverse their order of appearance and silica crystallizes in the groundmass during controlled cooling experiments. The partition of iron and magnesium between olivine and liquid is independent of cooling rate, temperature, and pressure. Comparison of the olivine nucleation densities in the lunar sample and in the experiments indicates that the sample began cooling at about 1 deg C/hr. Pyroxene size, chemistry, and growth instability spacings, as well as groundmass coarseness, all suggest that the cooling rate subsequently decreased by as much as a factor of 10 or more. The porphyritic texture of this sample, then, is produced at a decreasing, rather than a discontinuously increasing, cooling rate.
Armelao, Lidia; Barreca, Davide; Bottaro, Gregorio; Maragno, Cinzia; Tondello, Eugenio; Caneschi, Andrea; Sangregorio, Claudio; Gialanella, Stefano
2006-04-01
Pure and Ca-doped LaCoO3 nanopowders were prepared by a non-alkoxidic sol-gel route using cobalt(II) acetate, lanthanum(III) nitrate and calcium(II) acetate as oxide precursors. The structural evolution and magnetic properties of the samples were studied as a function of thermal treatments in air up to 1273 K. In particular, the microstructure and composition of the systems were analyzed by X-ray Diffraction (XRD), Transmission Electron Microscopy (TEM), and X-ray Photoelectron Spectroscopy (XPS). Both pure and calcium-doped samples annealing at 973 K resulted in the formation of cubic LaCoO3 (average crystallite size <30 nm). This phase was fully retained in the calcium-doped materials even after annealing at higher temperatures, whereas a transition to the rhomboedral polymorph was detected in the pure samples at 1073 K. The magnetic behavior of the nanopowders was investigated as a function of temperature and applied field using both dynamic and static susceptibility measurements. Pure lanthanum cobaltite samples underwent a transition to an ordered state at 88 K, and their magnetic properties changed as a function of thermal treatments. As concerns calcium-doped samples, they ordered ferromagnetically at 171 and 185 K depending on the annealing temperature and displayed open hysteresis loops with coercive fields as large as 1.75 T at low temperatures.
Microstructure and Mechanical Behavior of Porous Ti–6Al–4V Processed by Spherical Powder Sintering
Reig, Lucía; Tojal, Concepción; Busquets, David J.; Amigó, Vicente
2013-01-01
Reducing the stiffness of titanium is an important issue to improve the behavior of this material when working together with bone, which can be achieved by generating a porous structure. The aim of this research was to analyze the porosity and mechanical behavior of Ti–6Al–4V porous samples developed by spherical powder sintering. Four different microsphere sizes were sintered at temperatures ranging from 1300 to 1400 °C for 2, 4 and 8 h. An open, interconnected porosity was obtained, with mean pore sizes ranging from 54.6 to 140 µm. The stiffness of the samples diminished by as much as 40% when compared to that of solid material and the mechanical properties were affected mainly by powder particles size. Bending strengths ranging from 48 to 320 MPa and compressive strengths from 51 to 255 MPa were obtained. PMID:28788365
Microstructure and Mechanical Behavior of Porous Ti-6Al-4V Processed by Spherical Powder Sintering.
Reig, Lucía; Tojal, Concepción; Busquets, David J; Amigó, Vicente
2013-10-23
Reducing the stiffness of titanium is an important issue to improve the behavior of this material when working together with bone, which can be achieved by generating a porous structure. The aim of this research was to analyze the porosity and mechanical behavior of Ti-6Al-4V porous samples developed by spherical powder sintering. Four different microsphere sizes were sintered at temperatures ranging from 1300 to 1400 °C for 2, 4 and 8 h. An open, interconnected porosity was obtained, with mean pore sizes ranging from 54.6 to 140 µm. The stiffness of the samples diminished by as much as 40% when compared to that of solid material and the mechanical properties were affected mainly by powder particles size. Bending strengths ranging from 48 to 320 MPa and compressive strengths from 51 to 255 MPa were obtained.
Modeling and Simulation of A Microchannel Cooling System for Vitrification of Cells and Tissues.
Wang, Y; Zhou, X M; Jiang, C J; Yu, Y T
The microchannel heat exchange system has several advantages and can be used to enhance heat transfer for vitrification. To evaluate the microchannel cooling method and to analyze the effects of key parameters such as channel structure, flow rate and sample size. A computational flow dynamics model is applied to study the two-phase flow in microchannels and its related heat transfer process. The fluid-solid coupling problem is solved with a whole field solution method (i.e., flow profile in channels and temperature distribution in the system being simulated simultaneously). Simulation indicates that a cooling rate >10 4 C/min is easily achievable using the microchannel method with the high flow rate for a board range of sample sizes. Channel size and material used have significant impact on cooling performance. Computational flow dynamics is useful for optimizing the design and operation of the microchannel system.
NASA Astrophysics Data System (ADS)
Riapanitra, Anung; Asakura, Yusuke; Cao, Wenbin; Noda, Yasuto; Yin, Shu
2018-06-01
Fluorine-doped VO2(M) nanoparticles have been successfully synthesized using the hydrothermal method at a supercritical temperature of 490 °C. The pristine VO2(M) has the critical phase transformation temperature of 64 °C. The morphology and homogeneity of the monoclinic structure VO2(M) were adopted by the fluorine-doped system. The obtained particle size of the samples is smaller at the higher concentration of anion doping. The best reduction of critical temperature was achieved by fluorine doping of 0.13% up to 48 °C. The thin films of the fluorine-doped VO2(M) showed pronounced thermochromic property and therefore are suitable for smart window applications.
A THERMODYNAMIC ANALYSIS OF MITOTIC SPINDLE EQUILIBRIUM AT ACTIVE METAPHASE
Stephens, R. E.
1973-01-01
The mitotic apparatus of first-division metaphase eggs of the sea urchin Strongylocentrotus drobachiensis was observed by means of polarization microscopy under controlled temperature conditions. Eggs were fertilized and grown at two temperature extremes in order to produce two different sizes of available spindle pool. Slow division time allowed successive samples of such cells to be observed at the same point in metaphase but at different equilibrium temperatures, yielding curves of metaphase equilibrium birefringence vs. observational temperature. Using the plateau value of birefringence at higher temperatures as a measure of total available spindle pool and the observed birefringence at lower temperatures as a measure of polymerized material at equilibrium, the spindle protein association was evaluated according to the method of Inoué. Both pool conditions produced linear van't Hoff functions. Analysis of these functions yielded enthalpy and entropy changes of +55–65 kcal/mol and +197–233 entropy units (eu), respectively. These values for active mitotic metaphase are quite comparable to those obtained by Inoué and co-workers for arrested meiotic metaphase cells. When other equilibrium treatments were considered, the best fit to the experimental data was still that of Inoué, a treatment which theoretically involves first-order polymerization and dissociation kinetics. Treatment of metaphase cells with D2O by direct immersion drove the equilibrium to completion regardless of temperature, attaining or exceeding a birefringence value equal to the cell's characteristic pool size; perfusion with D2O appeared to erase the original temperature-determined pool size differences for the two growth conditions, attaining a maximum value characteristic of the larger pool condition. These data confirm Inoué's earlier contention that D2O treatment can modify the available spindle pool. PMID:4734864
Molecular mobility of nematic E7 confined to molecular sieves with a low filling degree.
Brás, A R; Frunza, S; Guerreiro, L; Fonseca, I M; Corma, A; Frunza, L; Dionísio, M; Schönhals, A
2010-06-14
The nematic liquid crystalline mixture E7 was confined with similar filling degrees to molecular sieves with constant composition but different pore diameters (from 2.8 to 6.8 nm). Fourier transform infrared analysis proved that the E7 molecules interact via the cyanogroup with the pore walls of the molecular sieves. The molecular dynamics of the system was investigated by broadband dielectric spectroscopy (10(-2)-10(9) Hz) covering a wide temperature range of approximately 200 K from temperatures well above the isotropic-nematic transition down to the glass transition of bulk E7. A variety of relaxation processes is observed including two modes that are located close to the bulk behavior in its temperature dependence. For all confined samples, two relaxation processes, at frequencies lower than the processes observed for the bulk, were detected. At lower temperatures, their relaxation rates have different temperature dependencies whereas at higher temperatures, they seem to collapse into one chart. The temperature dependence of the slowest process (S-process) obeys the Vogel-Fulcher-Tammann law indicating a glassy dynamics of the E7 molecules anchored to the pore surface. The pore size dependence of both the Vogel temperature and fragility revealed a steplike transition around 4 nm pore size, which indicates a transition from a strong to a fragile behavior. The process with a relaxation rate in between the bulklike and the S-process (I-process) shows no dependence on the pore size. The agreement of the I-process with the behavior of a 5CB surface layer adsorbed on nonporous silica leads to the assignment of E7 molecules anchored at the outer surface of the microcrystals of the molecular sieves.
Characterization of ingot material for SRF cavity production
DOE Office of Scientific and Technical Information (OSTI.GOV)
Mondal, Jayanta; Ciovati, Gianluigi; Kneisel, Peter K.
In recent years, large-grain/single-crystal niobium has become a viable alternative to the standard fine grain (ASTM grain size>6), high purity (RRR ) niobium for the fabrication of high-performance SRF cavities for particle accelerators. In this contribution we present the results of a systematic study of the superconducting properties of samples obtained from four Niobium ingots (from CBMM, Brazil) of different purity. Measurements of bulk magnetization, surface pinning, critical temperature and thermal conductivity have been carried out on the samples subjected to different surface treatments such as buffered chemical polishing (BCP), 6000C heat treatment, and low temperature baking (LTB). A correlationmore » has been established between the LTB and the ratio . In addition, the phonon peak in the thermal conductivity data is suppressed by the presence of trapped magnetic vortices in the samples.« less
Ferromagnetism in sphalerite and wurtzite CdS nanostructures
2013-01-01
Room-temperature ferromagnetism is observed in undoped sphalerite and wurtzite CdS nanostructures which are synthesized by hydrothermal methods. Scanning electron microscopy and transmission electron microscopy results indicate that the sphalerite CdS samples show a spherical-like shape and the wurtzite CdS ones show a flower-like shape, both of which are aggregated by lots of smaller particles. The impurity of the samples has been ruled out by the results of X-ray diffraction, selected-area electron diffraction, and X-ray photoelectron spectroscopy. Magnetization measurements indicate that all the samples exhibit room-temperature ferromagnetism and the saturation magnetization decreases with the increased crystal sizes, revealing that the observed ferromagnetism is defect-related, which is also confirmed by the post-annealing processes. This finding in CdS should be the focus of future electronic and spintronic devices. PMID:23294671
NASA Astrophysics Data System (ADS)
Sharma, Ravi Kant; Ghose, Ranjana
2015-04-01
Porous nanocrystalline NiO has been synthesized by a simple homogeneous precipitation method in short time at low calcination temperature without using any surfactant, chelating or gelating agents. The porous nanocrystalline NiO with a hexagonal sheet-like morphology were obtained by calcination of Ni(OH)2 nanoflakes at 500 °C. The calcination temperature strongly influences the morphology, crystallite size, specific surface area, pore volume and optical band gap of the samples. The samples were characterized using powder X-ray diffraction, thermal gravimetric analysis, FT-IR spectroscopy, UV-Visible diffuse reflectance spectroscopy, surface area measurements, field emission scanning electron microscopy coupled with energy dispersive X-ray analysis and transmission electron microscopy. The chemical activity of the samples was tested by catalytic reduction of 4-nitrophenol with NaBH4.
Magnetic studies of nickel hydride nanoparticles embedded in chitosan matrix
NASA Astrophysics Data System (ADS)
Araújo-Barbosa, S.; Morales, M. A.
2017-11-01
In this work we present a method to produce NiH (β-NiH phase) nanoparticles from Ni-Cu solid solution. The reduction of Ni2+ and Cu2+ occurred at high temperatures and in presence of glutaraldehyde, citric acid and chitosan biopolymer. The samples are mainly composed of Ni and NiH phases with particles sizes ranging from 9 to 27 nm. DC magnetization studies reveal the presence of hydrogen-poor nickel hydride phase (α-NiH phase) which enhances the saturation magnetization at temperatures below 50 K. Stability of samples stored in air after 8 months was verified, and thermal treatment at 350 oC in presence of air transformed the samples to Ni and Cu oxides. Furthermore, we present a discussion regarding the mechanism of Ni2+ and Cu2+ chemical reduction.
A ubiquitous ice size bias in simulations of tropical deep convection
NASA Astrophysics Data System (ADS)
Stanford, McKenna W.; Varble, Adam; Zipser, Ed; Strapp, J. Walter; Leroy, Delphine; Schwarzenboeck, Alfons; Potts, Rodney; Protat, Alain
2017-08-01
The High Altitude Ice Crystals - High Ice Water Content (HAIC-HIWC) joint field campaign produced aircraft retrievals of total condensed water content (TWC), hydrometeor particle size distributions (PSDs), and vertical velocity (w) in high ice water content regions of mature and decaying tropical mesoscale convective systems (MCSs). The resulting dataset is used here to explore causes of the commonly documented high bias in radar reflectivity within cloud-resolving simulations of deep convection. This bias has been linked to overly strong simulated convective updrafts lofting excessive condensate mass but is also modulated by parameterizations of hydrometeor size distributions, single particle properties, species separation, and microphysical processes. Observations are compared with three Weather Research and Forecasting model simulations of an observed MCS using different microphysics parameterizations while controlling for w, TWC, and temperature. Two popular bulk microphysics schemes (Thompson and Morrison) and one bin microphysics scheme (fast spectral bin microphysics) are compared. For temperatures between -10 and -40 °C and TWC > 1 g m-3, all microphysics schemes produce median mass diameters (MMDs) that are generally larger than observed, and the precipitating ice species that controls this size bias varies by scheme, temperature, and w. Despite a much greater number of samples, all simulations fail to reproduce observed high-TWC conditions ( > 2 g m-3) between -20 and -40 °C in which only a small fraction of condensate mass is found in relatively large particle sizes greater than 1 mm in diameter. Although more mass is distributed to large particle sizes relative to those observed across all schemes when controlling for temperature, w, and TWC, differences with observations are significantly variable between the schemes tested. As a result, this bias is hypothesized to partly result from errors in parameterized hydrometeor PSD and single particle properties, but because it is present in all schemes, it may also partly result from errors in parameterized microphysical processes present in all schemes. Because of these ubiquitous ice size biases, the frequently used microphysical parameterizations evaluated in this study inherently produce a high bias in convective reflectivity for a wide range of temperatures, vertical velocities, and TWCs.
NASA Astrophysics Data System (ADS)
Pan, Bing; Wu, Dafang; Xia, Yong
2010-09-01
To determine the full-field high-temperature thermal deformation of the structural materials used in high-speed aerospace flight vehicles, a novel non-contact high-temperature deformation measurement system is established by combining transient aerodynamic heating simulation device with the reliability-guided digital image correlation (RG-DIC). The test planar sample with size varying from several mm 2 to several hundreds mm 2 can be heated from room temperature to 1100 °C rapidly and accurately using the infrared radiator of the transient aerodynamic heating simulation system. The digital images of the test sample surface at various temperatures are recorded using an ordinary optical imaging system. To cope with the possible local decorrelated regions caused by black-body radiation within the deformed images at the temperatures over 450 °C, the RG-DIC technique is used to extract full-field in-plane thermal deformation from the recorded images. In validation test, the thermal deformation fields and the values of coefficient of thermal expansion (CTEs) of a chromiumnickel austenite stainless steel sample from room temperature to 550 °C is measured and compared with the well-established handbook value, confirming the effectiveness and accuracy of the proposed technique. The experimental results reveal that the present system using an ordinary optical imaging system, is able to accurately measure full-field thermal deformation of metals and alloys at temperatures not exceeding 600 °C.
NASA Astrophysics Data System (ADS)
Dunne, Conor F.; Roche, Kevin; Ruddy, Mark; Doherty, Kevin A. J.; Twomey, Barry; O'Donoghue, John; Hodgson, Darel; Stanton, Kenneth T.
2018-06-01
This work investigates the deposition of hydroxyapatite (HA) onto superelastic nickel-titanium (NiTi) using an ambient temperature coating process known as CoBlast. The process utilises a stream of abrasive alumina (Al2O3) and a coating medium (HA) sprayed simultaneously at the surface of the substrate. The use of traditional coatings methods, such as plasma spray, is unsuitable due to the high temperatures of the process. This can result in changes to both the crystallinity of the HA and properties of the thermally sensitive NiTi. HA is a biocompatible, biodegradable and osteoconductive ceramic, which when used as a coating can promote bone growth and prevent the release of nickel from NiTi in vivo. Samples were coated using different blast pressures and abrasive particle sizes and were examined using a variety of techniques. The coated samples had a thin adherent coating, which increased in surface roughness and coating thickness with increasing abrasive particle size. X-ray diffraction analysis revealed that the process gave rise to a stress-induced martensite phase in the NiTi which may enhance mechanical properties. The study indicates that the CoBlast process can be used to deposit thin adherent coatings of HA onto the surface of superelastic NiTi.
Kellner, Elliott; Hubbart, Jason A
2017-11-15
Given the importance of suspended sediment to biogeochemical functioning of aquatic ecosystems, and the increasing concern of mixed-land-use effects on pollutant loading, there is an urgent need for research that quantitatively characterizes spatiotemporal variation of suspended sediment dynamics in contemporary watersheds. A study was conducted in a representative watershed of the central United States utilizing a nested-scale experimental watershed design, including five gauging sites (n=5) partitioning the catchment into five sub-watersheds. Hydroclimate stations at gauging sites were used to monitor air temperature, precipitation, and stream stage at 30-min intervals during the study (Oct. 2009-Feb. 2014). Streamwater grab samples were collected four times per week, at each site, for the duration of the study (Oct. 2009-Feb. 2014). Water samples were analyzed for suspended sediment using laser particle diffraction. Results showed significant differences (p<0.05) between monitoring sites for total suspended sediment concentration, mean particle size, and silt volume. Total concentration and silt volume showed a decreasing trend from the primarily agricultural upper watershed to the urban mid-watershed, and a subsequent increasing trend to the more suburban lower watershed. Conversely, mean particle size showed an opposite spatial trend. Results are explained by a combination of land use (e.g. urban stormwater dilution) and surficial geology (e.g. supply-controlled spatial variation of particle size). Correlation analyses indicated weak relationships with both hydroclimate and land use, indicating non-linear sediment dynamics. Suspended sediment parameters displayed consistent seasonality during the study, with total concentration decreasing through the growing season and mean particle size inversely tracking air temperature. Likely explanations include vegetation influences and climate-driven weathering cycles. Results reflect unique observations of spatiotemporal variation of suspended sediment particle size class. Such information is crucial for land and water resource managers working to mitigate aquatic ecosystem degradation and improve water resource sustainability in mixed-land-use watersheds globally. Copyright © 2017 Elsevier B.V. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
DeMartini, Jaclyn D.; Foston, Marcus; Meng, Xianzhi
We report that woody biomass is highly recalcitrant to enzymatic sugar release and often requires significant size reduction and severe pretreatments to achieve economically viable sugar yields in biological production of sustainable fuels and chemicals. However, because mechanical size reduction of woody biomass can consume significant amounts of energy, it is desirable to minimize size reduction and instead pretreat larger wood chips prior to biological conversion. To date, however, most laboratory research has been performed on materials that are significantly smaller than applicable in a commercial setting. As a result, there is a limited understanding of the effects that largermore » biomass particle size has on the effectiveness of steam explosion pretreatment and subsequent enzymatic hydrolysis of wood chips. To address these concerns, novel downscaled analysis and high throughput pretreatment and hydrolysis (HTPH) were applied to examine whether differences exist in the composition and digestibility within a single pretreated wood chip due to heterogeneous pretreatment across its thickness. Heat transfer modeling, Simons’ stain testing, magnetic resonance imaging (MRI), and scanning electron microscopy (SEM) were applied to probe the effects of pretreatment within and between pretreated wood samples to shed light on potential causes of variation, pointing to enzyme accessibility (i.e., pore size) distribution being a key factor dictating enzyme digestibility in these samples. Application of these techniques demonstrated that the effectiveness of pretreatment of Populus tremuloides can vary substantially over the chip thickness at short pretreatment times, resulting in spatial digestibility effects and overall lower sugar yields in subsequent enzymatic hydrolysis. Finally, these results indicate that rapid decompression pretreatments (e.g., steam explosion) that specifically alter accessibility at lower temperature conditions are well suited for larger wood chips due to the non-uniformity in temperature and digestibility profiles that can result from high temperature and short pretreatment times. Furthermore, this study also demonstrated that wood chips were hydrated primarily through the natural pore structure during pretreatment, suggesting that preserving the natural grain and transport systems in wood during storage and chipping processes could likely promote pretreatment efficacy and uniformity.« less
DeMartini, Jaclyn D.; Foston, Marcus; Meng, Xianzhi; ...
2015-12-09
We report that woody biomass is highly recalcitrant to enzymatic sugar release and often requires significant size reduction and severe pretreatments to achieve economically viable sugar yields in biological production of sustainable fuels and chemicals. However, because mechanical size reduction of woody biomass can consume significant amounts of energy, it is desirable to minimize size reduction and instead pretreat larger wood chips prior to biological conversion. To date, however, most laboratory research has been performed on materials that are significantly smaller than applicable in a commercial setting. As a result, there is a limited understanding of the effects that largermore » biomass particle size has on the effectiveness of steam explosion pretreatment and subsequent enzymatic hydrolysis of wood chips. To address these concerns, novel downscaled analysis and high throughput pretreatment and hydrolysis (HTPH) were applied to examine whether differences exist in the composition and digestibility within a single pretreated wood chip due to heterogeneous pretreatment across its thickness. Heat transfer modeling, Simons’ stain testing, magnetic resonance imaging (MRI), and scanning electron microscopy (SEM) were applied to probe the effects of pretreatment within and between pretreated wood samples to shed light on potential causes of variation, pointing to enzyme accessibility (i.e., pore size) distribution being a key factor dictating enzyme digestibility in these samples. Application of these techniques demonstrated that the effectiveness of pretreatment of Populus tremuloides can vary substantially over the chip thickness at short pretreatment times, resulting in spatial digestibility effects and overall lower sugar yields in subsequent enzymatic hydrolysis. Finally, these results indicate that rapid decompression pretreatments (e.g., steam explosion) that specifically alter accessibility at lower temperature conditions are well suited for larger wood chips due to the non-uniformity in temperature and digestibility profiles that can result from high temperature and short pretreatment times. Furthermore, this study also demonstrated that wood chips were hydrated primarily through the natural pore structure during pretreatment, suggesting that preserving the natural grain and transport systems in wood during storage and chipping processes could likely promote pretreatment efficacy and uniformity.« less
Cheng, S L; Wong, S L; Lu, S W; Chen, H
2008-09-01
We report here the successful fabrication of large-area size-tunable periodic arrays of cobalt and Co-silicide nanodots on silicon substrates by employing the colloidal nanosphere lithography (NSL) technique and heat treatments. The growth of low-resistivity epitaxial CoSi(2) was found to be more favorable for the samples with smaller Co nanodot sizes. The sizes of the epitaxial CoSi(2) nanodots can be tuned from 50 to 100 nm by varying the diameter of the colloidal spheres and annealing temperatures. The epitaxial CoSi(2) nanodots were found to grow with an epitaxial orientation with respect to the (001)Si substrates: [001]CoSi(2)//[001]Si and (200)CoSi(2)//(400)Si. From the results of planview HRTEM, XTEM, and SAED analysis, the epitaxial CoSi(2) nanodots were identified to be inverse pyramids in shape, and the average sizes of the faceted silicide nanodots were measured to decrease with annealing temperature. The observed results present the exciting prospect that with appropriate controls, the colloidal NSL technique promises to facilitate the growth of a variety of well-ordered silicide nanodots with selected shape, size, and periodicity.
Effect of wheat flour characteristics on sponge cake quality.
Moiraghi, Malena; de la Hera, Esther; Pérez, Gabriela T; Gómez, Manuel
2013-02-01
To select the flour parameters that relate strongly to cake-making performance, in this study the relationship between sponge cake quality, solvent retention capacity (SRC) profile and flour physicochemical characteristics was investigated using 38 soft wheat samples of different origins. Particle size average, protein, damaged starch, water-soluble pentosans, total pentosans, SRC and pasting properties were analysed. Sponge cake volume and crumb texture were measured to evaluate cake quality. Cluster analysis was applied to assess differences in flour quality parameters among wheat lines based on the SRC profile. Cluster 1 showed significantly higher sponge cake volume and crumb softness, finer particle size and lower SRC sucrose, SRC carbonate, SRC water, damaged starch and protein content. Particle size, damaged starch, protein, thickening capacity and SRC parameters correlated negatively with sponge cake volume, while total pentosans and pasting temperature showed the opposite effect. The negative correlations between cake volume and SRC parameters along with the cluster analysis results indicated that flours with smaller particle size, lower absorption capacity and higher pasting temperature had better cake-making performance. Some simple analyses, such as SRC, particle size distribution and pasting properties, may help to choose flours suitable for cake making. Copyright © 2012 Society of Chemical Industry.
Self-healing coatings containing microcapsule
NASA Astrophysics Data System (ADS)
Zhao, Yang; Zhang, Wei; Liao, Le-ping; Wang, Si-jie; Li, Wu-jun
2012-01-01
Effectiveness of epoxy resin filled microcapsules was investigated for healing of cracks generated in coatings. Microcapsules were prepared by in situ polymerization of urea-formaldehyde resin to form shell over epoxy resin droplets. Characteristics of these capsules were studied by 3D measuring laser microscope, particle size analyzer, Fourier-transform infrared spectroscopy (FTIR) and differential scanning calorimeter (DSC) to investigate their surface morphology, size distribution, chemical structure and thermal stability, respectively. The results indicate that microcapsules containing epoxy resins can be synthesized successfully. The size is around 100 μm. The rough outer surface of microcapsule is composed of agglomerated urea-formaldehyde nanoparticles. The size and surface morphology of microcapsule can be controlled by selecting different processing parameters. The microcapsules basically exhibit good storage stability at room temperature, and they are chemically stable before the heating temperature is up to approximately 200 °C. The model system of self-healing coating consists of epoxy resin matrix, 10 wt% microencapsulated healing agent, 2 wt% catalyst solution. The self-healing function of this coating system is evaluated through self-healing testing of damaged and healed coated steel samples.
NASA Astrophysics Data System (ADS)
Srinivasa Rao, K.; Ranga Nayakulu, S. V.; Chaitanya Varma, M.; Choudary, G. S. V. R. K.; Rao, K. H.
2018-04-01
The present investigation describes the development of cobalt ferrite nanoparticles having size less than 10 nm, by a sol-gel method using polyvinyl alcohol as chelating agent. X-ray results show all the samples, annealed above 700 °C have spinel structure. The information about phase evolution with reaction temperatures was obtained by subjecting the as-prepared powder for DSC/TGA study. High saturation magnetization of 84.63 emu/g has been observed for a particle size of 8.1 nm, a rare event reported till date. The dM/dH versus H curves suggest that the transition from single domain state to multi-domain state occurs with increasing annealing temperature and the critical size for the single domain nature of CoFe2O4 is around 6.5 nm. The estimated critical diameter for single domain particle (6.7 nm) is in good agreement with that (6.5 nm) obtained from Transmission Electron Micrographs. The highest coercivity (1645 Oe) has been found for a particle of size 6.5 nm.
Expansion and melting of Xe nanocrystals in Si
NASA Astrophysics Data System (ADS)
Faraci, Giuseppe; Pennisi, Agata R.; Zontone, Federico; Li, Boquan; Petrov, Ivan
2006-12-01
Xe agglomerates confined in a Si matrix by ion implantation were synthesized with different size depending on the implantation process and/or the thermal treatment. At low temperature Xe nanocrystals are formed, whose expansion and melting were studied in the range 15- 300K . Previous high resolution x-ray diffraction spectra were corroborated with complementary techniques such as two-dimensional imaging plate patterns and transmission electron microscopy. We detected fcc Xe nanocrystals whose properties were size dependent. The experiments showed that in annealed samples epitaxial condensation of small Xe clusters, on the cavities of the Si matrix, gave in fact expanded and oriented Xe, suggesting a possible preferential growth of Xe(311) planes oriented orthogonally to the Si[02-2] direction. On the contrary, small Xe clusters in an amorphous Si matrix have a fcc lattice contracted as a consequence of surface tension. Furthermore, a solid-to-liquid phase transition size dependent was found. Expansion of fcc Xe lattice was accurately determined as a function of the temperature. Overpressurized nanocrystals and/or binary size distributions were disproved.
Konz, Ioana; Fernández, Beatriz; Fernández, M Luisa; Pereiro, Rosario; Sanz-Medel, Alfredo
2014-01-27
A new custom-built Peltier-cooled laser ablation cell is described. The proposed cryogenic cell combines a small internal volume (20 cm(3)) with a unique and reliable on-sample temperature control. The use of a flexible temperature sensor, directly located on the sample surface, ensures a rigorous sample temperature control throughout the entire analysis time and allows instant response to any possible fluctuation. In this way sample integrity and, therefore, reproducibility can be guaranteed during the ablation. The refrigeration of the proposed cryogenic cell combines an internal refrigeration system, controlled by a sensitive thermocouple, with an external refrigeration system. Cooling of the sample is directly carried out by 8 small (1 cm×1 cm) Peltier elements placed in a circular arrangement in the base of the cell. These Peltier elements are located below a copper plate where the sample is placed. Due to the small size of the cooling electronics and their circular allocation it was possible to maintain a peephole under the sample for illumination allowing a much better visualization of the sample, a factor especially important when working with structurally complex tissue sections. The analytical performance of the cryogenic cell was studied using a glass reference material (SRM NIST 612) at room temperature and at -20°C. The proposed cell design shows a reasonable signal washout (signal decay within less than 10 s to background level), high sensitivity and good signal stability (in the range 6.6-11.7%). Furthermore, high precision (0.4-2.6%) and accuracy (0.3-3.9%) in the isotope ratio measurements were also observed operating the cell both at room temperature and at -20°C. Finally, experimental results obtained for the cell application to qualitative elemental imaging of structurally complex tissue samples (e.g. eye sections from a native frozen porcine eye and fresh flower leaves) demonstrate that working in cryogenic conditions is critical in such type of direct sample analysis. Copyright © 2013 Elsevier B.V. All rights reserved.
A diamond-based scanning probe spin sensor operating at low temperature in ultra-high vacuum
DOE Office of Scientific and Technical Information (OSTI.GOV)
Schaefer-Nolte, E.; Wrachtrup, J.; 3rd Institute of Physics and Research Center SCoPE, University Stuttgart, 70569 Stuttgart
2014-01-15
We present the design and performance of an ultra-high vacuum (UHV) low temperature scanning probe microscope employing the nitrogen-vacancy color center in diamond as an ultrasensitive magnetic field sensor. Using this center as an atomic-size scanning probe has enabled imaging of nanoscale magnetic fields and single spins under ambient conditions. In this article we describe an experimental setup to operate this sensor in a cryogenic UHV environment. This will extend the applicability to a variety of molecular systems due to the enhanced target spin lifetimes at low temperature and the controlled sample preparation under UHV conditions. The instrument combines amore » tuning-fork based atomic force microscope (AFM) with a high numeric aperture confocal microscope and the facilities for application of radio-frequency (RF) fields for spin manipulation. We verify a sample temperature of <50 K even for strong laser and RF excitation and demonstrate magnetic resonance imaging with a magnetic AFM tip.« less
The Leaching of Aluminium In Spanish Clays, Coal Mining Wastes and Coal Fly Ashes by Sulphuric Acid.
NASA Astrophysics Data System (ADS)
Fernández, A. M.; Ibáñez, J. L.; Llavona, M. A.; Zapico, R.
The acid leaching of aluminium from several non traditional ores, bayerite, kaolinite, different clays, coal mining wastes and coal fly ashes, and the kinetic of their dissolution are described. The effects of time, temperature, acid concentration, sample calcination, particle size were examined. The leaching of aluminium is dependent on acid concentration and strongly on temperature. Generally, the time to reach a fixed percentage of dissolution decreases with increasing acid concentration in the range 6% to 40% acid by weight. On clays and coal mining wastes a good relation between Al removal and ratio kaolinite/illite was also observed at all temperatures and acid concentration tested. Coal fly ashes are particles that were heated at very high temperatures in the power station and Al compounds were transformed into mullite and so Al recovery was minor. Several rate equations describing the kinetics of the leach reaction were discussed and Kinetic parameters and activation energy values of samples are presented.
Cosmology with EMSS Clusters of Galaxies
NASA Technical Reports Server (NTRS)
Donahue, Megan; Voit, G. Mark
1999-01-01
We use ASCA observations of the Extended Medium Sensitivity Survey sample of clusters of galaxies to construct the first z = 0.5 - 0.8 cluster temperature function. This distant cluster temperature function, when compared to local z approximately 0 and to a similar moderate redshift (z = 0.3 - 0.4) temperature function strongly constrains the matter density of the universe. Best fits to the distributions of temperatures and redshifts of these cluster samples results in Omega(sub M) = 0.45 +/- 0.1 if Lambda = 0 and Omega = 0.27 +/- 0.1 if Lambda + Omega(sub M) = 1. The uncertainties are 1sigma statistical. We examine the systematics of our approach and find that systematics, stemming mainly from model assumptions and not measurement errors, are about the same size as the statistical uncertainty +/- 0.1. In this poster proceedings, we clarify the issue of a8 as reported in our paper Donahue & Voit (1999), since this was a matter of discussion at the meeting.
Temperature alters food web body-size structure.
Gibert, Jean P; DeLong, John P
2014-08-01
The increased temperature associated with climate change may have important effects on body size and predator-prey interactions. The consequences of these effects for food web structure are unclear because the relationships between temperature and aspects of food web structure such as predator-prey body-size relationships are unknown. Here, we use the largest reported dataset for marine predator-prey interactions to assess how temperature affects predator-prey body-size relationships among different habitats ranging from the tropics to the poles. We found that prey size selection depends on predator body size, temperature and the interaction between the two. Our results indicate that (i) predator-prey body-size ratios decrease with predator size at below-average temperatures and increase with predator size at above-average temperatures, and (ii) that the effect of temperature on predator-prey body-size structure will be stronger at small and large body sizes and relatively weak at intermediate sizes. This systematic interaction may help to simplify forecasting the potentially complex consequences of warming on interaction strengths and food web stability. © 2014 The Author(s) Published by the Royal Society. All rights reserved.
DOE Office of Scientific and Technical Information (OSTI.GOV)
Rather, Sami ullah, E-mail: rathersami@gmail.com
2014-12-15
Graphical abstract: X-ray diffraction (XRD) pattern of magnesium nanoparticles synthesized by solution reduction method with and without TOPO. - Highlights: • Simple and convenient method of preparing Mg nanoparticles. • Characterized by XRD, SEM, FESEM and TEM. • Trioctylphosphine oxide offers a greater control over the size of the particles. • Hydrogen uptake of samples at different temperatures and pressure of 4.5 MPa. - Abstract: Facile and simple, surfactant-mediated solution reduction method was used to synthesize monodisperse magnesium nanoparticles. Little amount of magnesium oxide nanoparticles were also formed due to the presence of TOPO and easy oxidation of magnesium, eventhough,more » all precautions were taken to avoid oxidation of the sample. Precise size control of particles was achieved by carefully varying the concentration ratio of two different types of surfactants, – trioctylphosphine oxide and hexadecylamine. Recrystallized magnesium nanoparticle samples with and without TOPO were analyzed by X-ray diffraction, scanning electron microscope, field emission scanning electron microscope, and transmission electron microscope. The peak diameters of particles were estimated from size distribution analysis of the morphological data. The particles synthesized in the presence and absence of TOPO found to have diameters 46.5 and 34.8 nm, respectively. This observed dependence of particle size on the presence of TOPO offers a convenient method to control the particle size by simply using appropriate surfactant concentrations. Exceptional enhancement in hydrogen uptake and kinetics in synthesized magnesium nanoparticles as compared to commercial magnesium sample was due to the smaller particle size and improved morphology. Overall hydrogen uptake not affected by the little variation in particle size with and without TOPO.« less
Microstructure modification and oxygen mobility of CeZrO2 nanocrystal doped with Y and Fe metals
NASA Astrophysics Data System (ADS)
Hadi, A.; Shah, M. N. A.; Ismail, K. N.; Roslan, A. B.
2017-09-01
CeZrO2-nanocrystals doped with Y3+ and Fe2+ have been successfully synthesized using the microemulsion method. In this study, the synergetic effect of the synthesis parameters on the formation of structure and catalytic property were reported. XRD analysis found that both doped samples reveal the symmetrical cubic phase and mix in a homogeneous solid solution. The crystallite size of both samples was in nanoscale, which were 11 and 15 nm for CZF and CZY, respectively. This finding was consistent with the physical size investigated by TEM, which was approximately 10 nm for both samples. Meanwhile, isotherm profiles for both samples appeared as the type IV group in the IUPAC classification which was the mesoporous materials. CZY crystal had higher BET surface area than CZF crystal, which was 141.30 and 135.5 m2/g, respectively. Oxygen mobility study found that CZF crystal promotes to active at lower temperature, which is 274.2˚C, than CZY at 302.7˚C. CZF crystal also revealed the higher oxygen removal, which was 286.35 mmol/g, than CZY was 250.49 mmol/g. The doping of transition metal, Fe into CeZrO2 tended to reduce the oxygen mobility's activation temperature, while the addition of rare earth metal, Y into CeZrO2 leaded to remarkable increase of surface area.
Advanced Experimental Methods for Low-temperature Magnetotransport Measurement of Novel Materials
Hagmann, Joseph A.; Le, Son T.; Richter, Curt A.; Seiler, David G.
2016-01-01
Novel electronic materials are often produced for the first time by synthesis processes that yield bulk crystals (in contrast to single crystal thin film synthesis) for the purpose of exploratory materials research. Certain materials pose a challenge wherein the traditional bulk Hall bar device fabrication method is insufficient to produce a measureable device for sample transport measurement, principally because the single crystal size is too small to attach wire leads to the sample in a Hall bar configuration. This can be, for example, because the first batch of a new material synthesized yields very small single crystals or because flakes of samples of one to very few monolayers are desired. In order to enable rapid characterization of materials that may be carried out in parallel with improvements to their growth methodology, a method of device fabrication for very small samples has been devised to permit the characterization of novel materials as soon as a preliminary batch has been produced. A slight variation of this methodology is applicable to producing devices using exfoliated samples of two-dimensional materials such as graphene, hexagonal boron nitride (hBN), and transition metal dichalcogenides (TMDs), as well as multilayer heterostructures of such materials. Here we present detailed protocols for the experimental device fabrication of fragments and flakes of novel materials with micron-sized dimensions onto substrate and subsequent measurement in a commercial superconducting magnet, dry helium close-cycle cryostat magnetotransport system at temperatures down to 0.300 K and magnetic fields up to 12 T. PMID:26863449
NASA Astrophysics Data System (ADS)
Yang, Kun Vanna; Lim, Chao Voon Samuel; Zhang, Kai; Sun, Jifeng; Yang, Xiaoguang; Huang, Aijun; Wu, Xinhua; Davies, Christopher H.
2015-12-01
Heat-treated Ti-6Al-4V forged bar with colony microstructure was machined into double-cone-shaped samples for a series of isothermal uniaxial compression test at 1223 K (950 °C) with varying constant crosshead speeds of 12.5, 1.25, and 0.125 mms-1 to a height reduction of 70 pct. Another set of samples deformed under the same conditions were heat treated at 1173 K (900 °C) for an hour followed by water quench. Finite element modeling was used to provide the strains, strain rates, and temperature profiles of the hot compression samples, and the microstructure and texture evolution was examined at four positions on each sample, representative of different strain ranges. Lamellae fragmentation and kinking are the dominant microstructural features at lower strain range up to a maximum of 2.0, whereas globularization dominates at strains above 2.0 for the as-deformed samples. The globularization fraction generally increases with strain, or by post-deformation heat treatment, but fluctuates at lower strain. The grain size of the globular α is almost constant with strain and maximizes for samples with the lowest crosshead speed due to the longer deformation time. The globular α grain also coarsens because of post-deformation heat treatment, with its size increasing with strain level. With respect to texture evolution, a basal transverse ring and another component 30 deg from ND is determined for samples deformed at 12.5 mms-1, which is consistent with the temperature increase to close to β-transus from simulation results. The texture type remains unchanged with its intensity increased and spreads with increasing strain.
Puls, Robert W.; Eychaner, James H.; Powell, Robert M.
1996-01-01
Investigations at Pinal Creek, Arizona, evaluated routine sampling procedures for determination of aqueous inorganic geochemistry and assessment of contaminant transport by colloidal mobility. Sampling variables included pump type and flow rate, collection under air or nitrogen, and filter pore diameter. During well purging and sample collection, suspended particle size and number as well as dissolved oxygen, temperature, specific conductance, pH, and redox potential were monitored. Laboratory analyses of both unfiltered samples and the filtrates were performed by inductively coupled argon plasma, atomic absorption with graphite furnace, and ion chromatography. Scanning electron microscopy with Energy Dispersive X-ray was also used for analysis of filter particulates. Suspended particle counts consistently required approximately twice as long as the other field-monitored indicators to stabilize. High-flow-rate pumps entrained normally nonmobile particles. Difference in elemental concentrations using different filter-pore sizes were generally not large with only two wells having differences greater than 10 percent in most wells. Similar differences (>10%) were observed for some wells when samples were collected under nitrogen rather than in air. Fe2+/Fe3+ ratios for air-collected samples were smaller than for samples collected under a nitrogen atmosphere, reflecting sampling-induced oxidation.
NASA Astrophysics Data System (ADS)
Bazhan, Z.; Ghodsi, F. E.; Mazloom, J.
2016-10-01
The sol-gel spin-coated nickel ferrite (NF), NiFe2O4, thin films were synthesised and the effect of annealing temperature and compositional ratio on different properties of samples were investigated. Electrochemical performance of the films was measured in the presence of KOH and LiClO4/PC electrolyte. Generally, addition of nickel increases the current density. The NF thin films with molar ratio of 0.5 and annealed at 400 °C have the highest charge density value and the highest capacitance in both electrolytes. Annealing temperature had significant effect on electrochemical properties of NF thin films and the diffusion coefficient enhanced by increasing the annealing temperature. X-ray diffraction patterns of prepared samples showed the rhombohedral structure, hematite phase (α-Fe2O3), of iron oxide sample and the presence of inverse spinel structure confirms the formation of NF. Field emission scanning electron microscopy images revealed that the morphology of films changes from larvae shape to granular structure by nickel incorporation and the grain size increased by raising the annealing temperature. The absorption edge of the hematite shift to higher wavelength by annealing and nickel incorporation and band gap narrowing has been occurred.
NASA Astrophysics Data System (ADS)
Omaraa, Ehsan; Saman, Wasim; Bruno, Frank; Liu, Ming
2017-06-01
Latent heat storage using phase change materials (PCMs) can be used to store large amounts of energy in a narrow temperature difference during phase transition. The thermophysical properties of PCMs such as latent heat, specific heat and melting and solidification temperature need to be defined at high precision for the design and estimating the cost of latent heat storage systems. The existing laboratory standard methods, such as differential thermal analysis (DTA) and differential scanning calorimetry (DSC), use a small sample size (1-10 mg) to measure thermophysical properties, which makes these methods suitable for homogeneous elements. In addition, this small amount of sample has different thermophysical properties when compared with the bulk sample and may have limitations for evaluating the properties of mixtures. To avoid the drawbacks in existing methods, the temperature - history (T-history) method can be used with bulk quantities of PCM salt mixtures to characterize PCMs. This paper presents a modified T-history setup, which was designed and built at the University of South Australia to measure the melting point, heat of fusion, specific heat, degree of supercooling and phase separation of salt mixtures for a temperature range between 200 °C and 400 °C. Sodium Nitrate (NaNO3) was used to verify the accuracy of the new setup.
NASA Astrophysics Data System (ADS)
Fattah-alhosseini, Arash; Ansari, Ali Reza; Mazaheri, Yousef; Karimi, Mohsen
2017-02-01
In this study, the electrochemical behavior of commercial pure titanium with both coarse-grained (annealed sample with the average grain size of about 45 µm) and nano-grained microstructure was compared by potentiodynamic polarization, electrochemical impedance spectroscopy (EIS), and Mott-Schottky analysis. Nano-grained Ti, which typically has a grain size of about 90 nm, is successfully made by six-cycle accumulative roll-bonding process at room temperature. Potentiodynamic polarization plots and impedance measurements revealed that as a result of grain refinement, the passive behavior of the nano-grained sample was improved compared to that of annealed pure Ti in H2SO4 solutions. Mott-Schottky analysis indicated that the passive films behaved as n-type semiconductors in H2SO4 solutions and grain refinement did not change the semiconductor type of passive films. Also, Mott-Schottky analysis showed that the donor densities decreased as the grain size of the samples reduced. Finally, all electrochemical tests showed that the electrochemical behavior of the nano-grained sample was improved compared to that of annealed pure Ti, mainly due to the formation of thicker and less defective oxide film.
Automated sample exchange and tracking system for neutron research at cryogenic temperatures
NASA Astrophysics Data System (ADS)
Rix, J. E.; Weber, J. K. R.; Santodonato, L. J.; Hill, B.; Walker, L. M.; McPherson, R.; Wenzel, J.; Hammons, S. E.; Hodges, J.; Rennich, M.; Volin, K. J.
2007-01-01
An automated system for sample exchange and tracking in a cryogenic environment and under remote computer control was developed. Up to 24 sample "cans" per cycle can be inserted and retrieved in a programed sequence. A video camera acquires a unique identification marked on the sample can to provide a record of the sequence. All operations are coordinated via a LABVIEW™ program that can be operated locally or over a network. The samples are contained in vanadium cans of 6-10mm in diameter and equipped with a hermetically sealed lid that interfaces with the sample handler. The system uses a closed-cycle refrigerator (CCR) for cooling. The sample was delivered to a precooling location that was at a temperature of ˜25K, after several minutes, it was moved onto a "landing pad" at ˜10K that locates the sample in the probe beam. After the sample was released onto the landing pad, the sample handler was retracted. Reading the sample identification and the exchange operation takes approximately 2min. The time to cool the sample from ambient temperature to ˜10K was approximately 7min including precooling time. The cooling time increases to approximately 12min if precooling is not used. Small differences in cooling rate were observed between sample materials and for different sample can sizes. Filling the sample well and the sample can with low pressure helium is essential to provide heat transfer and to achieve useful cooling rates. A resistive heating coil can be used to offset the refrigeration so that temperatures up to ˜350K can be accessed and controlled using a proportional-integral-derivative control loop. The time for the landing pad to cool to ˜10K after it has been heated to ˜240K was approximately 20min.
Ultrasonic Spot Welding of a Rare-Earth Containing ZEK100 Magnesium Alloy: Effect of Welding Energy
NASA Astrophysics Data System (ADS)
Macwan, A.; Chen, D. L.
2016-04-01
Ultrasonic spot welding was used to join a low rare-earth containing ZEK100 Mg alloy at different levels of welding energy, and tensile lap shear tests were conducted to evaluate the failure strength in relation to the microstructural changes. It was observed that dynamic recrystallization occurred in the nugget zone; the grain size increased and microhardness decreased with increasing welding energy arising from the increasing interface temperature and strain rate. The weld interface experienced severe plastic deformation at a high strain rate from ~500 to ~2100 s-1 with increasing welding energy from 500 to 2000 J. A relationship between grain size and Zener-Hollomon parameter, and a Hall-Petch-type relationship between microhardness and grain size were established. The tensile lap shear strength and failure energy were observed to first increase with increasing welding energy, reach the maximum values at 1500 J, and then decrease with a further increase in the welding energy. The samples welded at a welding energy ≤1500 J exhibited an interfacial failure mode, while nugget pull-out occurred in the samples welded at a welding energy above 1500 J. The fracture surfaces showed typical shear failure. Low-temperature tests at 233 K (-40 °C) showed no significant effect on the strength and failure mode of joints welded at the optimal welding energy of 1500 J. Elevated temperature tests at 453 K (180 °C) revealed a lower failure load but a higher failure energy due to the increased deformability, and showed a mixed mode of partial interfacial failure and partial nugget pull-out.
NASA Technical Reports Server (NTRS)
Mohr, Karen I.; Molinari, John; Thorncroft, Chris
2009-01-01
The characteristics of convective system populations in West Africa and the western Pacific tropical cyclone basin were analyzed to investigate whether interannual variability in convective activity in tropical continental and oceanic environments is driven by variations in the number of events during the wet season or by favoring large and/or intense convective systems. Convective systems were defined from Tropical Rainfall Measuring Mission (TRMM) data as a cluster of pixels with an 85-GHz polarization-corrected brightness temperature below 255 K and with an area of at least 64 square kilometers. The study database consisted of convective systems in West Africa from May to September 1998-2007, and in the western Pacific from May to November 1998-2007. Annual cumulative frequency distributions for system minimum brightness temperature and system area were constructed for both regions. For both regions, there were no statistically significant differences between the annual curves for system minimum brightness temperature. There were two groups of system area curves, split by the TRMM altitude boost in 2001. Within each set, there was no statistically significant interannual variability. Subsetting the database revealed some sensitivity in distribution shape to the size of the sampling area, the length of the sample period, and the climate zone. From a regional perspective, the stability of the cumulative frequency distributions implied that the probability that a convective system would attain a particular size or intensity does not change interannually. Variability in the number of convective events appeared to be more important in determining whether a year is either wetter or drier than normal.