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At least 1,261 records · Page 70

High-pressure studies with x-rays using diamond anvil cells

Pressure profoundly alters all states of matter. The symbiotic development of ultrahigh-pressure diamond anvil cells, to compress samples to sustainable multi-megabar pressures; and synchrotron x-ray techniques, to probe materials' properties in situ, has enabled the exploration of rich high-pressure (HP) science. In this article, we first introduce the essential concept of diamond anvil cell technology, together with recent developments and its integration with other extreme environments. We then provide an overview of the latest developments in HP synchrotron techniques, their applications, and current problems, followed by a discussion of HP scientific studies using x-rays in the key multidisciplinary fields. These HP studies include: HP x-ray emission spectroscopy, which provides information on the filled electronic states of HP samples; HP x-ray Raman spectroscopy, which probes the HP chemical bonding changes of light elements; HP electronic inelastic x-ray scattering spectroscopy, which accesses high energy electronic phenomena, including electronic band structure, Fermi surface, excitons, plasmons, and their dispersions; HP resonant inelastic x-ray scattering spectroscopy, which probes shallow core excitations, multiplet structures, and spin-resolved electronic structure; HP nuclear resonant x-ray spectroscopy, which provides phonon densities of state and time-resolved Mössbauer information; HP x-ray imaging, which provides information on hierarchical structures, dynamic processes, and internal strains; HP x-ray diffraction, which determines the fundamental structures and densities of single-crystal, polycrystalline, nanocrystalline, and non-crystalline materials; and HP radial x-ray diffraction, which yields deviatoric, elastic and rheological information. Integrating these tools with hydrostatic or uniaxial pressure media, laser and resistive heating, and cryogenic cooling, has enabled investigations of the structural, vibrational, electronic, and magnetic properties of materials over a wide range of pressure-temperature conditions.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Synthesis of Narrow SnTe Nanowires Using Alloy Nanoparticles

Topological crystalline insulator tin telluride (SnTe) provides a rich playground to examine interactions of correlated electronic states, such as ferroelectricity, topological surface states, and superconductivity. The study of SnTe nanowires may lead to even richer physics owing to the one-dimensional (1D) confinement effect and an increased contribution from the topological surface states. Thus, for transport measurements, SnTe nanowires must be synthesized with reduced diameters and high crystalline quality to ensure 1D confinement and phase coherence of the topological surface electrons. Here, we report a facile growth method to produce narrow SnTe nanowires with a high yield using alloy nanoparticles as growth catalysts. The average diameter of the SnTe nanowires grown using alloy nanoparticles is 85 nm, nearly a factor of three reduction compared to the average diameter of 240 nm when using gold nanoparticles as growth catalysts. Transport measurements reveal the effect of the nanowire diameter on the residual resistance ratio and magnetoresistance. Particularly, the ferroelectric transition temperature for SnTe evolves systematically with the nanowire diameter. In situ cryogenic cooling of narrow SnTe nanowires in a transmission electron microscope directly reveals the cubic to rhombohedral structural transition, which is associated with the ferroelectric transition. Thus, these narrow SnTe nanowires represent a model system to study electronic states arising from 1D confinement, such as 1D topological superconductivity and potential multiband superconductivity.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Towards the construction of the Mu2e electromagnetic calorimeter at Fermilab

Mu2e will search for the Charge Lepton Flavor Violating (CLFV) conversion of a muon into an electron in the field of a nucleus. A clean discovery signature is provided by the mono-energetic conversion electron (E e = 104.96 MeV). If no events are observed, Mu2e will set a limit on the ratio between the conversion and the nuclear capture rate below 3 × 10$^{-17}$ (at 90% C.L.). In order to confirm that the observed candidate is an electron, the calorimeter resolution requirements are to provide E res < 10%, T res < 500 ps for 100 MeV electrons while working in vacuum and in a high radiation environment and high magnetic field. The calorimeter is made of two annular aluminum disks, each one filled with 674 pure CsI crystals read out by SiPMs. A sophisticated mechanics and cooling system has been developed to support the crystals and cool the sensors. Radiation hard analog and fast digital electronics have been developed. In this paper the QC tests performed on the produced components and the construction status are reported, as well as the results obtained on the large size prototype with test beam data and at a cosmic ray test stand.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

Probing the electronic structure and dipole-bound state of the 7-azaindolide anion

We report an investigation of the electronic structure and dipole-bound state (DBS) of the cryogenically-cooled 7-azaindolide anion (7-AI − ) using high-resolution photoelectron imaging, photodetachment spectroscopy, and resonant photoelectron spectroscopy. The electron affinity of the 7-AI radical is measured to be 2.6967(8) eV (21 751 ± 6 cm −1 ). Two excited electronic states of the neutral radical are observed at 0.8 eV and 1.4 eV above the ground state. Two minor isomers of 7-AI − due to deprotonation from the α- and β-carbon on the pyrrole ring are also detected with lower adiabatic detachment energies. A DBS is observed for the 7-AI − anion at 156 cm −1 below the detachment threshold, along with 16 vibrational Feshbach resonances. Resonant two-photon photoelectron imaging reveals that the DBS is relatively long-lived. Resonant photoelectron spectroscopy via the vibrational Feshbach resonances of the DBS gives rise to rich vibrational features for the 7-AI radical not accessible in conventional photoelectron spectroscopy. Fundamental vibrational frequencies for 16 vibrational modes of the 7-AI neutral radical are measured experimentally, including 7 bending modes. The current work provides extensive experimental electronic and vibrational information for the 7-AI − anion and the 7-AI radical.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Effect of Cooling Rate on Microsegregation During Solidification of Superalloy INCONEL 718 Under Slow-Cooled Conditions

The solidification sequence, microstructural evolution, solid-liquid interface variation, interdendritic segregation, and elemental distribution of as-cast IN718 alloy at three slow-cooling rates (5, 10, and 20 °C/min) were investigated by differential scanning calorimetry (DSC), confocal laser scanning microscopy (CLSM), optical microscopy (OM), field-emission scanning electron microscopy (FESEM), and electron-probe microanalysis (EPMA) techniques. The results indicate that as the cooling rate decreases, the constitutional supercooling at the solidification front affects the solid-liquid interface more significantly, and the size and quantity of the Laves phase increase. However, the composition of the Laves phase is insensitive to the cooling rate in the range of conditions studied here. In dendrite core, the contents of Ni, Cr, Fe, and Al follow a slight downward trend with an increasing cooling rate, whereas the Nb, Mo, and Ti contents show an upward trend. Additionally, Mo shows a stronger propensity to segregate under slow-cooling conditions because its effective partition coefficient almost linearly decreased with decreasing cooling rate, which is same as Nb. Using the parameters experimentally determined in this study and the Clyne–Kurz equation, we achieved reasonable agreement between the calculated and measured liquid composition change during the solidification process at different cooling rates. All experimental and theoretical programs in this research were undertaken with the aim of gaining further understanding of the microsegregation behaviors in large-scale IN718 ingots, whose cooling rates are within a lower range.

36 MATERIALS SCIENCE↗

Microstructural development of electron beam processed Al-3Ti-1Sc alloy under different electron beam scanning speeds

A systematic study has been made of the microstructural development in as-cast 30 mm thick Al-3Ti-1Sc (wt%) plate samples that were processed by electron beam (EB) melting at different scanning speeds of 3, 5, 8, 12, 15 and 20 mm/s. The composition of the alloy is designed to capitalize on the potential for significantly extended solubility values of both Sc and Ti in Al when cooled at high cooling rates. The resulting microstructures are characterised using transmission electron microscopy (TEM) and other analytical means, assisted with Thermo-Calc predictions and Vicker's microhardness measurements. EB scanning speed plays a key role in determining the phase formation and microstructural development in the Al-3Ti-1Sc alloy when the beam is applied an accelerating voltage of 50 kV and a current of 30 μA. The major microstructural features in the re-solidified zone include (i) the formation of the primary tetragonal Al{sub 3}(Ti,Sc) phases and their retention or subsequent transformation to stable cubic Al{sub 3}(Ti,Sc) phases; (ii) the complete suppression of the primary tetragonal Al{sub 3}(Ti,Sc) phases at the scanning speed of 20 mm/s; and (iii) the formation of cubic Al{sub 3}(Ti,Sc) precipitates in the α(Al) matrix supersaturated with both Sc and Ti. These experimental findings are informative for both EB processing of Al-Ti-Sc alloys and the design of new Al alloys for additive manufacturing processes.

36 MATERIALS SCIENCE↗

Toward the Development of Molten Salt Reactor Diagnostics based on Resonantly Enhanced Laser Spectroscopy

One emerging concern within the safeguards community is how to best ensure compliance with nuclear security regulations within molten salt reactor (MSR) facilities. This problem is nontrivial as molten salts used for fuel or coolant are highly corrosive, chemically complex, and inherently require high operational temperatures. Laser spectroscopy methods such as laser-induced breakdown spectroscopy (LIBS) and laser-induced fluorescence (LIF) have previously been suggested for molten salt diagnostics due to their compatibility with liquid phase samples and potential for in-situ measurements [1]. In the former, the laser is used to ionize the sample, allowing for the characteristic light from electronic de-excitation as the resultant plasma cools to be used for material characterization. In the latter, a tunable light source is set be resonant with a specific transition, resulting in element specific excitation and the emission of fluorescence light. In our previous work [2], we demonstrated that LIF could be used for the detection of fission fragments such as Nd in solution through the separation of laser scatter and fluorescence within the time domain. Here, we present progress towards two alternate measurement schemes: LIF measurements based on spectroscopic discrimination of fluorescence emissions and resonant LIBS measurements that induce plasma using a light source set to the resonant frequency of a specific electronic transition. Both methods aim to exploit resonant excitation methods to enhance the emitted signal. The studies may provide routes for element-specific detection of constituents within complicated matrices and a means to better understand the chemical behavior of lanthanides and actinides relevant to MSRs.

98 - NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL↗

Effect of Heat Treatment on Microstructure and Mechanical Property of 316L Stainless Steel Produced by Laser Powder Bed Fusion

The advanced non-light water reactor designs (Gen IV reactors), including molten salt/ very high temperature/ sodium-cooled and lead-cooled fast reactors, typically operate at higher temperatures and more extreme radiation conditions than light water reactors. An intrinsic part of the deployment and progress of Gen IV reactor designs is selecting the most suitable structural material for a specific application. Additive manufacturing (AM), a fairly new process of making physical, three-dimensional objects from a computer design file, is going to completely change the way of design, build and certify nuclear systems. It offers a range of opportunities to produce complex geometries from existing materials, offers new routes for processing of previously difficult to process materials, allows for design of new high-performance materials, and finally facilitates hybridization of dissimilar materials. This emerging technology has successfully produced cars, wind turbine blade molds and even live cells. It could also open up big opportunities for the nuclear industry to quickly deploy technologies at a fraction of the cost. So far, AM techniques have been preliminarily applied in the field of nuclear reactors, including the classical parts such as the pressure vessel of a small reactor with 508-III steel, the bottom nozzle of a fuel assembly with 304L steel, the fuel cladding with zirconium alloy and the integrated impeller of a pump and the multi-channel valve body with 316L steel [6,7]. The AM applications for operating nuclear reactors started in auxiliary plant components and have slowly migrated to metallic reactors and core components, but many of these are not safety critical components. Although many parts used for nuclear reactors have been fabricated by AM techniques, practical applications in engineering are still a long way off due to the uncertainty factors focused on the processing, material properties, analysis methods and application standards, which feeds the safety and life-cycle of the nuclear reactor. Due to rapid, repeated heating and cooling during production, a high dislocation density was present in the AM material. This microstructure feature is unstable at elevated temperature while high temperature is one of the typical operation environments for nuclear reactors. Thus, it is important to understand the thermal effect on the microstructure of AM material. The objectives of this study are to investigate the effect of heat treatment on the microstructure and mechanical properties of 316L stainless steel produced by laser powder bed fusion additive manufacturing, and to determine an appropriate heat treatment practice that will be applied to the lightweight AM lattice-structured material with the same chemistry. The heat treatment study consisted of annealing the samples at a temperature range of 800 to 1200 oC with a 50 oC increment for different times (1-24 hours), followed by vacuum or air cooling. Microstructural characterization was carried out by Scanning Electron Microscope (SEM). Grain size and crystallographic orientation were investigated by Electron Backscatter Diffraction (EBSD). Vickers hardness tests with a 0.5 kg load were employed to determine the hardness of samples after different heat treatments. After heat treatment, the random crystallographic orientation was preserved, and the volume fraction of high-angle grain boundaries (grain boundary misorientation =15 oC) remained the same. The dislocation density decreased with annealing temperature due to recovery. The fine subgrain structures in the as-printed specimen were quite stable up to 1200 oC. Minimal recrystallization was observed up to 1200 oC. Recrystallization initiated only after 8.5 hours at 1200 oC. The SEM images did not show obvious dependence of microstructure on cooling rate. The hardness of the specimens decreased with increasing annealing temperature as a result of the decrease in dislocation density. It is interesting to note that the AM material showed very similar hardness to the wrought material when annealing at similar temperature, although the microstructures are very different. Annealing at 1050 oC for 1 hour followed by air cooling was selected as the heat treatment procedure for the lattice designed lightweight AM 316L material.

36 MATERIALS SCIENCE↗

Jet Impingement Cooling of Electric Machines with Driveline Fluids

In the presentation thermal management of electric traction drives is discussed and capabilities of NREL's Advanced Power Electronics and Electric Machines group is reviewed. Emphasis is made on jet impingement cooling technique of electric machines with driveline fluids and experimental measurements of associated heat transfer coefficients.

47 OTHER INSTRUMENTATION↗

Influence of cooling rate on the development of multiple generations of {gamma}' precipitates in a commercial nickel base superalloy

The compositional and microstructural evolution of different generations of {gamma}' precipitates during the continuous cooling of a commercial nickel base superalloy, Rene88DT, has been characterized by three dimensional atom probe tomography coupled with energy-filtered transmission electron microscopy studies. After solutionizing in the single {gamma} phase field, continuous cooling at a very high rate results in a monomodal size distribution of {gamma}' precipitates with a high nucleation density and non-equilibrium compositions. In contrast, a relatively slower cooling rate ({approx} 24 deg. C/min) results in a multi-modal size distribution of {gamma}' precipitates with the larger first generation primary precipitates exhibiting close to equilibrium composition, along with the smaller scale secondary {gamma}' precipitates, exhibiting non-equilibrium composition (excess of Co and Cr, depleted in Al and Ti). The composition of the {gamma} matrix near these precipitates also exhibits similar trends with the composition being closer to equilibrium near the primary precipitates as compared to the secondary precipitates. - Highlights: {yields} Effect of cooling rate on the precipitation of {gamma}' particles in commercial nickel base superalloy. {yields} Couples EFTEM and 3DAP studies to determine the composition and morphology of {gamma}' precipitates. {yields} Determination of near and far field compositional variations within the gamma matrix leading to subsequent precipitation.

36 MATERIALS SCIENCE↗

Resistivity, I–V characteristics and Hall effect in Dy{sub 0.5}(Sr{sub 1-x}Ca{sub x}){sub 0.5}MnO{sub 3} manganites

Highlights: • The resistivity of Dy{sub 0.5}(Sr{sub 1-x}Ca{sub x}){sub 0.5}MnO{sub 3} (x = 0 and x = 0.3) systems showed that these samples exhibited an insulating behavior. • I–V characteristics of both samples deviate from the Ohmic behavior. • Magnetoresistance and electroresistance provided negative values. • Hall resistivity ρxy of the Dy{sub 0.5}Sr{sub 0.5}MnO{sub 3} sample presents electron-like type of the charge carriers. • The temperature coefficient of resistance (TCR) shows that both systems can be good candidates for bolometer applications. - Abstract: Dy{sub 0.5}(Sr{sub 1-x}Ca{sub x}){sub 0.5}MnO{sub 3} (x = 0 and x = 0.3) manganites were synthesized using sol-gel method. Both samples exhibited an insulating behavior in the whole temperature range. Even the application of 5 T magnetic fields does not change this state. Conduction mechanisms were also investigated. The I–V characteristics of both samples present Ohmic behavior at minor voltages. Magnetoresistance and electroresistance were also studied. The thermal variation of Hall resistivity of Dy{sub 0.5}Sr{sub 0.5}MnO{sub 3} was determined in cooling down and warming up processes revealing electron-like type of charge carriers. Temperature coefficient of resistance shows significant values for both systems making them good candidates for bolometer applications.

36 MATERIALS SCIENCE↗

Heating and cooling of ligand-coated colloidal nanocrystals in solid films and solvent matrices

Ligand-to-nanocrystal heating and subsequent cooling to the environmental medium is investigated with infrared pump, electronic probe (IPEP) spectroscopy. Compared to solid films, solvated nanocrystals show faster ligand-to-nanocrystal heat equilibration (c. 11 ps versus c. 17 ps). Solvated nanocrystals also display more cooling of the hot ligand–nanocrystal complex on the experimentally measured time-scale, emphasizing the thermally insulating nature of semiconductor nanocrystal solids. Although heating transfer rates among solvents are all between 150 ps and 330 ps, cooling of the nanocrystal–ligand complex is slower, on average, in chlorinated solvents (c. 315 ps) compared to deuterated hydrocarbon solvents (c. 215 ps). Differences between chlorinated and hydrocarbon solvents show the importance of matching the vibrational energies of the solvent and the ligands for increasing the rate of heat transfer. Increases in the cooling time for poorer hydrocarbon solvents, in which nanocrystals aggregated, such as toluene, compared to better solvents, like methylcyclohexane, indicate that penetration of solvent into the ligand layer facilitates improved heat transfer to the matrix.

36 MATERIALS SCIENCE↗

High efficiency klystron for the SPS application

The enhancement of klystron efficiency through the use of collector depression, that is by recovering energy from the spent electron beam after microwave amplification, was investigated. Design considerations included noise, harmonics, cooling, and service life. The mod anode, to be employed for beam control, and the depressed collector, used in spent electron beam energy recovery, are described.

Larue, A. D.↗

Energetics of RHESSI X-Class Flares

The thermal and nonthermal energies of several X-class flares seen with the Reuven Ramaty High Energy Solar Spectroscopic Imager (RHESSI) will be presented. The same techniques described by Emslie et al. (JGR, 109, A10104, 2004) are used to take the RHESSI imaging spectroscopic observations and compute the energies in the thermal plasma and in the nonthermal electrons as a function of time throughout the flares. Radiative and conductive cooling rates are estimated and total thermal and nonthermal energies are computed for each flare. Typically, the energy in nonthermal electrons integrated up to the time of peak soft X-ray emission is equal to or exceeds the energy in the thermal plasma at that time. This suggests that energy must have been converted into a form not visible with RHESSI and that the total energy released by the flares may be significantly greater than the sum of energies calculated from the RHESSI observations alone. This conclusion is supported by the high radiative energy seen with SORCE during the impulsive phase of the 28 October 2003 flare. The peak increase in total solar irradiance of 270 mW per square meters measured with SORCE was over two orders of magnitude higher than the peak soft X-ray flux seen with GOES or RHESSI. The implications of this new observation as compared to the energetics derived from the X-ray observations of that flare will be discussed along with the energetics analysis of most of the other X- class flares in October/November 2003.

Dennis, Brian R.↗

Electron temperature and density relationships in coronal mass ejections

We examine 10 coronal mass ejections from the in-ecliptic portion of the Ulysses mission. Five of these CMEs are magnetic clouds. In each case we observe an inverse relationship between electron temperature and density. For protons this relationship is less clear. Earlier work has shown a similar inverse relationship for electrons inside magnetic clouds and interpreted it to mean that the polytropic index governing the expansion of electrons is less than unity. This requires electrons to be heated as the CME expands. We offer an alternative view that the inverse relationship between electron temperature and density is caused by more rapid cooling of the denser plasma through collisions. More rapid cooling of denser plasma has been shown for 1 AU measurements in the solar wind. As evidence for this hypothesis we show that the denser plasma inside the CMEs tends to be more isotropic indicating a different history of collisions for the dense plasma. Thus, although the electron temperature inside CMEs consistently shows an inverse correlation with the density, this is not an indication of the polytropic index of the plasma but instead supports the idea of collisional modification of the electrons during their transit from the sun.

Hammond, C. M.↗

Power Electronics Thermal Management R&D; NREL (National Renewable Energy Laboratory)

Presentation containing an update for the Power Electronics Thermal Management project in the Electric Drive Train task funded by the Vehicle Technology Office of DOE. This presentation outlines the purpose, plan, and results of research thus far for cooling and material selection strategies to manage heat in power electronic assemblies such as inverters, converters, and chargers.

30 DIRECT ENERGY CONVERSION↗

Ion temperature evolution in an ultracold neutral plasma

We study the long-time evolution of the ion temperature in an expanding ultracold neutral plasma using spatially resolved, laser-induced-fluorescence spectroscopy. Adiabatic cooling reduces the ion temperature by an order of magnitude during the plasma expansion, to temperatures as low as 0.2 K. Cooling is limited by heat exchange between ions and the much hotter electrons. We also present evidence for an additional heating mechanism and discuss possible sources. Data are described by a model of the plasma evolution, including the effects of ion-electron heat exchange. We show that for appropriate initial conditions, the degree of Coulomb coupling of ions in the plasma increases during expansion.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗